JP3545784B2 - Method for producing coated quasi-fine particles - Google Patents
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- JP3545784B2 JP3545784B2 JP21926993A JP21926993A JP3545784B2 JP 3545784 B2 JP3545784 B2 JP 3545784B2 JP 21926993 A JP21926993 A JP 21926993A JP 21926993 A JP21926993 A JP 21926993A JP 3545784 B2 JP3545784 B2 JP 3545784B2
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Description
【０００１】
【産業上の利用分野】
本発明は、被覆準微粒子の製造方法とそのための装置に関する。より詳細には、準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子に、被覆形成物質を被覆する被覆準微粒子の製造方法とそのための装置に関する。
【０００２】
【従来の技術】
気相法により、粉体粒子表面に無機材料や金属材料等の被覆形成物質を、膜を始めとする種々の形態で被覆する方法は、原理的に、（１）雰囲気の制御が容易である、（２）基本的に被覆形成物質の選択に制限がなく、活性金属を始めとする金属単体物質、合金、窒化物、炭化物、硼化物、酸化物などの種々の種類の物質を粉体粒子表面に被覆できる、（３）高純度の物質を被覆できる、（４）被覆形成物質の被覆量を任意に制御できるなど、他の被覆法では成し得ない大きな特徴がある。
【０００３】
そしてこの気相法による、例えば１０μｍを越える粒子径の準微粒子の芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子への、高度に制御された均一な被覆、即ち個々の粒子の表面の、大きな領域にわたって未被覆部分が残らない均一な被覆で、且つこの均一な被覆が全ての粒子に漏れがなく成される被覆が要求されている。しかも、この高度に制御された均一な被覆は、その粒子径が大きいものについては、より一層未被覆部分が少ない均一な被覆が求められている。
【０００４】
しかし、公知の技術として提案されている種々の被覆装置や被覆方法では前記高度に制御された均一な被覆はいまだ達成されていない。
【０００５】
例えば、特開昭５８−３１０７６号公報に開示されている装置・方法によれば、ＰＶＤ装置内に設置された容器の中に芯粒子粉体の粒子を入れ、容器を電磁気的な方法により振動させ、前記容器内の芯粒子を転動させながらＰＶＤ法により被覆される。また、特開昭６１−３０６６３号公報に開示されている装置によれば、ＰＶＤ装置内に設置された容器の中に芯粒子粉体の粒子を入れ、容器を機械的な方法により振動させ、前記容器内の芯粒子を転動させながらＰＶＤ法により被覆することができるとされている。しかし、これらの容器の振動により芯粒子粉体の粒子を転動させながら被覆する装置或いは方法では、実際には、準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子は何層にも重なった状態で摺動するのみで単一粒子状態で被覆できなかった。
【０００６】
特開平３−１５３８６４号公報に開示されている装置及び方法は、内面に障壁及び／又は凹凸を備えた回転容器内に粒子を入れ、回転容器を回転しながら蒸着法により芯粒子表面に被覆を行なうことを目的とするものであるが、このような装置或いは方法において、準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子は、何層にも重なった状態で多くの粒子が接触したまま軽く撹拌されるだけで、単一粒子状態で被覆できなかった。
【０００７】
特開昭５８−１４１３７５号公報には、反応ガス雰囲気中に置かれた粉体を反応ガスの流れと重力の作用とによって浮遊させて、反応ガスの化学反応により生成される析出物質によって粉体の表面を被覆する装置が開示されている。又、特開平２−４３３７７号公報には、粒子を減圧下において流動化させながら、熱化学反応処理を行い被覆を行なう方法が開示されている。又、特開昭６４−８０４３７号公報には、低・高周波合成音波により芯粒子粉体の凝集体を崩して流動化させ被覆する方法が開示されている。しかし、これらの気流や振動により準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子の流動層利用する方法又は装置では、全ての芯粒子を同じ様に単一粒子状態で独立に流動、浮遊させることは事実上不可能であり、粒子同士が陰になってできる各粒子の被覆むらをなくすことができなかった。
【０００８】
特開昭５４−１５３７８９号公報には、金属の蒸気を発生させた真空容器内を粉末材料を落下させ金属を被覆する装置が開示されている。又、特開昭６０−４７００４号公報には真空槽中の高周波プラズマ領域にモノマーガスと粉体粒子を導入し、プラズマ重合により有機物の被覆膜を形成させる方法が開示されている。これらの装置或いは方法の如く、導入するたけでは準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子は、単一粒子状態でない凝集体を形成して落下するだけで、粒子の陰ができて被覆むらができたり、凝集体の内部の粒子は全く被覆されなかったり、或いは単一粒子に被覆されたものにくらべ被覆量の違いが生じてしまった。
【０００９】
特開昭６２−２５０１７２号公報には、前処理として、ジェットミル処理した粉体を、減圧加熱処理室で滞留せしめ、ここで加熱処理を施した後、粉体フィーダーでスパッタリング室に自然落下により導入せしめ、ターゲットを垂直に設けた円筒状のスパッタリング室に自然落下させ被覆させる装置及び方法が開示されている。又、特開平２−１５３０６８号公報には、前処理として、ジェットミル処理した粉体を、減圧加熱処理室で滞留させ、ここで加熱処理を施した後、粉体フィーダーでスパッタリング室のスパッタリング源を納めた回転容器に（単一粒子でない）粉体状で導入し、容器を回転させた状態でスパッタリングする装置及び方法が開示されている。これら装置及び方法では、被覆前の加熱工程で、ジェットミル処理した芯粒子粉体を滞留させる工程があり、加熱工程でのこの粉体の滞留のため再び単一粒子状態でない凝集体を形成し、結局被覆工程ではこの凝集体は単一粒子状態にはならない。
【００１０】
以上のように、従来公知の技術では、いずれも準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子に被覆する装置或いは方法としての問題解決はなされておらず、準微粒子の芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子は、現実には接触したままの凝集体の状態で被覆処理に供され、そのために各粒子への高度に制御された均一な被覆がなされることはなかった。すなわち高度に制御された均一な被覆がなされる被覆準微粒子の製造方法もそのための製造装置もなかった。それが為、事実上、上記問題が解消出来なかった。
【００１１】
【発明が解決しようとする課題】
従って、現実に、例えば準微粒子が１０μｍを越える粒子である準微粒子の芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子への、高度に制御された均一な被覆、即ち個々の粒子の表面の大きな領域にわたって未被覆部分が残らない均一な被覆で、且つこの均一な被覆が全ての粒子に漏れがなく成される被覆が要求されている。しかも、その粒子径が大きいものについては、より一層未被覆部分が少ない均一な被覆ができる被覆準微粒子の製造方法とそのための装置が強く求められている。
【００１２】
本発明は、準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子への、高度に制御された均一な被覆、即ち個々の粒子の表面の大きな領域にわたって未被覆部分が残らない均一な被覆で、且つこの均一な被覆が全ての粒子に漏れがなく成される被覆で、しかもその粒子径が大きいものについては、より一層未被覆部分が少ない均一な被覆ができる被覆準微粒子の製造方法とそのための装置を提供することを目的とする。
【００１３】
【課題を解決するための手段】
前記課題を解決するために、本発明者が鋭意研究を重ねた結果、準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子への、高度に制御された均一な被覆、即ち個々の粒子の表面の大きな領域にわたって未被覆部分が残らない均一な被覆で、且つ均一な被覆が全ての粒子に漏れがなく成される被覆で、しかも、その粒子径が大きいものについては、より一層未被覆部分が少ない均一な被覆を成すためには、（１）体積基準頻度分布で平均粒子径が１０μｍを越え、２０μｍ以下の芯粒子粉体の粒子が主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物中の芯粒子粉体の粒子を、分散度βが８０％以上である高い分散状態の被覆空間の被覆開始領域でか、又は（２）体積基準頻度分布で平均粒子径が２０μｍを越え、５０μｍ以下の芯粒子粉体の粒子が主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物中の芯粒子粉体の粒子を、分散度βが９０％以上である高い分散状態の被覆空間の被覆開始領域でか、又は（３）体積基準頻度分布で平均粒子径が５０μｍを越え、３００μｍ以下の芯粒子粉体の粒子が主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物中の芯粒子粉体の粒子を、分散度βが９５％以上である高い分散状態の被覆空間の被覆開始領域でか、又は（４）体積基準頻度分布で平均粒子径が３００μｍを越え、８００μｍ以下の芯粒子粉体の粒子が主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物中の芯粒子粉体の粒子を、分散度βが９７％以上である高い分散状態の被覆空間の被覆開始領域でか、又は（５）体積基準頻度分布で平均粒子径が８００μｍを越える芯粒子粉体の粒子が主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物中の芯粒子粉体の粒子を、分散度βが９９％以上である高い分散状態の被覆空間の被覆開始領域で被覆を開始しなければならないことを見い出した。
【００１４】
より詳しくは、（Ｉ）芯粒子粉体の粒子が主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物の状態の芯粒子粉体の粒子は、滞留させなくとも、時間の経過と共に主に乱流凝集等により再凝集する傾向にあり、一旦再凝集すると、前記分散処理前の凝集体と同じく特別に高い分散性能を有する分散処理手段により分散させなければこの再凝集の状態を崩して高度に分散、即ち一個一個の単位の単一粒子状態へ再分散させることが困難であり、このため、（１）体積基準頻度分布で平均粒子径が１０μｍを越え、２０μｍ以下の芯粒子粉体の粒子が主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物中の芯粒子粉体の粒子を、分散度βが８０％以上である高い分散状態でか、又は（２）体積基準頻度分布で平均粒子径が２０μｍを越え、５０μｍ以下の芯粒子粉体の粒子が主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物中の芯粒子粉体の粒子を、分散度βが９０％以上である高い分散状態でか、又は（３）体積基準頻度分布で平均粒子径が５０μｍを越え、３００μｍ以下の芯粒子粉体の粒子が主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物中の芯粒子粉体の粒子を、分散度βで９５％以上である高い分散状態でか、又は（４）体積基準頻度分布で平均粒子径が３００μｍを越え、８００μｍ以下の芯粒子粉体の粒子が主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物中の芯粒子粉体の粒子を、分散度βが９７％以上である高い分散状態の被覆空間の被覆開始領域でか、又は（５）体積基準頻度分布で平均粒子径が８００μｍを越える芯粒子粉体の粒子が主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物中の芯粒子粉体の粒子を、分散度βが９９％以上である高い分散状態で被覆空間の被覆開始領域に導く必要があること、またそのためには、（II）この芯粒子粉体からなる凝集体を崩し、且つ粒子径に応じた非常に高い分散度で気中に分散せしめる、一以上からなる特別に高い分散性能を有する分散処理手段群が必要であることを見い出して本発明に至った。
【００１５】
即ち、本発明は芯粒子粉体を被覆空間に投入し、気相を経て生成する被覆形成物質前駆体及び／又は気相状態の被覆形成物質前駆体を、芯粒子粉体の粒子に接触及び／又は衝突させて、芯粒子粉体の粒子の表面を被覆形成物質で被覆する被覆準微粒子の製造装置において、
（Ａ） 準微粒子高分散処理手段群の最終処理手段が、
（ａ） この芯粒子粉体の粒子を気中に分散させる分散手段、及び
（ｂ） 芯粒子粉体の粒子を気中に分散させた芯粒子粉体の粒子と気体の混合物において低分散芯粒子粉体部分を分離し、芯粒子粉体の粒子が主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物を選択する高分散芯粒子粉体の粒子・気体混合物選択手段とこの高分散芯粒子粉体の粒子・気体混合物選択手段により分離された低分散芯粒子粉体部分を準微粒子高分散処理手段群中の分散手段の内の最終分散手段及び／又は最終分散手段以前の処理手段に搬送するフィードバック手段とを備えた高分散芯粒子粉体の粒子・気体混合物選択手段、
から選ばれる準微粒子高分散処理手段群により、体積基準頻度分布で平均粒子径が１０μｍを越える準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、気中に分散させて高分散芯粒子粉体の粒子・気体混合物とする分散工程、
（Ｂ） この分散工程で分散させた芯粒子粉体の粒子を、
その平均粒子径が１０μｍを越え２０μｍ以下のときには分散度βが８０％以上、
２０μｍを越え５０μｍ以下のときには分散度βが９０％以上、
５０μｍを越え３００μｍ以下のときには分散度βが９５％以上、
３００μｍを越え８００μｍ以下のときは分散度βが９７％以上、そして
８００μｍを越えるときは分散度βが９９％以上
の分散状態で、被覆空間の被覆開始領域において被覆形成物質前駆体と接触及び／又は衝突させて被覆を開始する被覆工程、
を設けたことを特徴とする、被覆準微粒子の製造方法を提供するものである。
【００１６】
更に本発明は前記した被覆準微粒子の製造方法において体積基準頻度分布で平均粒径が１０μｍを越え、２０μｍ以下の芯粒子粉体を準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを８０％以上とするか、又は体積基準頻度分布で平均粒径が２０μｍを越え、５０μｍ以下の芯粒子粉体を準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物としその芯粒子粉体の粒子の分散度βを９０％以上とするか、又は体積基準頻度分布で平均粒径が５０μｍを越え、３００μｍ以下の芯粒子粉体を準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物としその芯粒子粉体の粒子の分散度βを９５％以上とするか、又は体積基準頻度分布で平均粒子径が３００μｍを越え８００μｍ以下の芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９７％以上とするか、又は体積基準頻度分布で平均粒子径が８００μｍを越える芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９９％以上とする分散性能を有する準微粒子高分散処理手段群による分散工程を設け、準微粒子高分散処理手段群による高分散芯粒子粉体の粒子・気体混合物を被覆工程に直接放出するか、又は分散工程と被覆工程の間に、準微粒子高分散処理手段群の高分散芯粒子粉体の粒子・気体混合物を放出する放出部から、直接放出するか、又は搬送に不可避の、中空部材、中空を形成せしめる部材からなる中間部材、及びパイプから選択される一種類又はそれ以上の部材を介して搬送するか、及び／又は、前記分散性能で気中に分散させた高分散芯粒子粉体の粒子・気体混合物中の粒子の気中分散状態を維持する気中分散維持手段、前記分散性能で気中に分散させた高分散芯粒子粉体の粒子・気体混合物中の粒子の気中分散状態を高める気中分散促進手段、芯粒子粉体の粒子と気体との混合物の内の、低分散芯粒子粉体部分を分離し、芯粒子粉体の粒子が主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物を選択する高分散芯粒子粉体の粒子・気体混合物選択手段の一種又はそれ以上を介して搬送する、搬送工程を設けることを特徴とする被覆準微粒子の製造方法にも関する。
【００１７】
更に本発明は、前記した被覆準微粒子の製造方法において、体積基準頻度分布で平均粒子径が１０μｍを越え、２０μｍ以下の芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを８０％以上とするか、又は体積基準頻度分布で平均粒子径が２０μｍを越え、５０μｍ以下の芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９０％以上とするか、又は体積基準頻度分布で平均粒子径が５０μｍを越え、３００μｍ以下の芯粒子粉体を準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９５％以上とするか、又は体積基準頻度分布で平均粒子径が３００μｍを越え８００μｍ以下の芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９７％以上とする分散性能を有する準微粒子高分散処理手段群、又は体積基準頻度分布で平均粒子径が８００μｍを越える芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９９％以上とする分散性能を有する準微粒子高分散処理手段群による分散工程の一部以上と前記被覆工程の一部以上とを、空間を一部以上共有して行うことを特徴とする被覆準微粒子の製造方法にも関する。
【００１８】
更に本発明はまた、前記した被覆準微粒子の製造方法において、体積基準頻度分布で平均粒子径が１０μｍを越え２０μｍ以下の芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを８０％以上とする空間領域、
体積基準頻度分布で平均粒子径が２０μｍを越え５０μｍ以下の芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９０％以上とする空間領域、
体積基準頻度分布で平均粒子径が５０μｍを越え３００μｍ以下の芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９５％以上とする空間領域、
体積基準頻度分布で平均粒子径が、３００μｍを越え８００μｍ以下の芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９７％以上とする空間領域、
体積基準頻度分布で平均粒子径が、８００μｍを越える芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９９％以上とする空間領域の内の高分散芯粒子粉体の粒子・気体混合物中の芯粒子粉体の粒子の全ての粒子が通過する面を含む空間領域に、被覆空間の被覆開始領域を位置せしめるか、又は
体積基準頻度分布で平均粒子径が１０μｍを越え２０μｍ以下の芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを８０％以上とする空間領域、
体積基準頻度分布で平均粒子径が２０μｍを越え５０μｍ以下の芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９０％以上とする空間領域、
体積基準頻度分布で平均粒子径が５０μｍを越え３００μｍ以下の芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９５％以上とする空間領域、
体積基準頻度分布で平均粒子径が、３００μｍを越え８００μｍ以下の芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９７％以上とする空間領域、
体積基準頻度分布で平均粒子径が、８００μｍを越える芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９９％以上とする空間領域の内の、回収手段の回収部に回収する全ての粒子が通過する面を含む空間領域に、被覆空間の被覆開始領域を位置せしめることを特徴とする被覆準微粒子の製造方法にも関する。
【００１９】
更に本発明はまた、芯粒子粉体の粒子の粒度分布が、平均粒子径をＤMとしたとき、体積基準頻度分布で（〔ＤM／５，５ＤM〕，≧９０％）であることを特徴とする被覆準微粒子の製造方法にも関する。
【００２０】
また本発明は上記した被覆粒子の製造方法を実施するための装置、すなわち芯粒子粉体を被覆空間に投入し、気相を経て生成する被覆形成物質前駆体及び／又は気相状態の被覆形成物質前駆体を、芯粒子粉体の粒子に接触及び／又は衝突させて、芯粒子粉体の粒子の表面を被覆形成物質で被覆する被覆準微粒子の製造装置において、
（Ａ） 準微粒子高分散処理手段群の最終処理手段が、
（ａ） この芯粒子粉体の粒子を気中に分散させる分散手段、および
（ｂ） 芯粒子粉体の粒子を気中に分散させた芯粒子粉体の粒子と気体の混合物において低分散芯粒子粉体部分を分離し、芯粒子粉体の粒子が主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物を選択する高分散芯粒子粉体の粒子・気体混合物選択手段とこの高分散芯粒子粉体の粒子・気体混合物選択手段により分離された低分散芯粒子粉体部分を準微粒子高分散処理手段群中の分散手段の内の最終分散手段及び／又は最終分散手段以前の処理手段に搬送するフィードバック手段とを備えた高分散芯粒子粉体の粒子・気体混合物選択手段、
から選ばれる準微粒子高分散処理手段群により、体積基準頻度分布で平均粒子径が１０μｍを越え、３００μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、気中に分散させて高分散芯粒子粉体の粒子・気体混合物とする分散処理手段、
（Ｂ） この分散処理手段で分散した芯粒子粉体の粒子を、
その平均粒子径が１０μｍを越え２０μｍ以下のときには分散度βが８０％以上、
２０μｍを越え５０μｍ以下のときには分散度βが９０％以上、
５０μｍを越え３００μｍ以下のときには分散度βが９５％以上、
３００μｍを越え８００μｍ以下のときは分散度βが９７％以上、そして
８００μｍを越えるときは分散度βが９９％以上
の分散状態で、被覆空間の被覆開始領域において被覆形成物質前駆体と接触及び／又は衝突させて被覆を開始する被覆室、
を設けたことを特徴とする、被覆準微粒子の製造装置を提供するものである。
【００２１】
更に本発明は前記した被覆準微粒子の製造装置において体積基準頻度分布で平均粒径が１０μｍを越え２０μｍ以下の芯粒子粉体を準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを８０％以上とするか、又は体積基準頻度分布で平均粒径が２０μｍを越え５０μｍ以下の芯粒子粉体を準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物としその芯粒子粉体の粒子の分散度βを９０％以上とするか、又は体積基準頻度分布で平均粒径が５０μｍを越え３００μｍ以下の芯粒子粉体を準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物としその芯粒子粉体の粒子の分散度βを９５％以上とするか、又は体積基準頻度分布で平均粒子径が３００μｍを越え８００μｍ以下の芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９７％以上とする分散性能を有する準微粒子高分散処理手段群、又は体積基準頻度分布で平均粒子径が８００μｍを越える芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９９％以上とする分散性能を有する準微粒子高分散処理手段群による処理手段を設け、準微粒子高分散処理手段群の最終処理により生成させた高分散芯粒子粉体の粒子・気体混合物を、準微粒子高分散処理手段群から放出する、準微粒子高分散処理手段群の放出部を、被覆準微粒子の製造装置の被覆空間を有する被覆室に、直結させ又は搬送に不可避の、中空部材、中空を形成せしめる部材からなる中間部材及びパイプから選択される一種類又はそれ以上の部材を介して接続し、及び／又は、分散性能で気中に分散させた高分散芯粒子粉体の粒子・気体混合物中の粒子の気中分散状態を維持させる気中分散維持手段、分散性能で気中に分散させた高分散芯粒子粉体の粒子・気体混合物中の粒子の気中分散状態を高める気中分散促進手段、芯粒子粉体の粒子と気体との混合物において、低分散芯粒子粉体部分を分離し、芯粒子粉体の粒子が主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物を選択する高分散芯粒子粉体の粒子・気体混合物選択手段の内の一種又はそれ以上を介して接続したことを特徴とする被覆準微粒子の製造装置にも関する。
【００２２】
更に本発明は、前記した被覆準微粒子の製造装置において、体積基準頻度分布で平均粒子径が１０μｍを越え２０μｍ以下の芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを８０％以上とするか、又は体積基準頻度分布で平均粒子径が２０μｍを越え５０μｍ以下の芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９０％以上とするか、又は体積基準頻度分布で平均粒子径が５０μｍを越え３００μｍ以下の芯粒子粉体を準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９５％以上とするか、又は体積基準頻度分布で平均粒子径が３００μｍを越え８００μｍ以下の芯粒子粉体を、準微粒子高分散処理手段群の最終処理により高い分散させて芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９７％以上とするか、又は体積基準頻度分布で平均粒子径が８００μｍを越える芯粒子粉体を、準微粒子高分散処理手段群の最終処理により高分散させて芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９９％以上とする分散性能を有する準微粒子高分散処理手段群を含む分散処理手段の一部以上と、前記被覆室とを、それらが占める空間を一部以上共有するようにして設けることを特徴とする被覆準微粒子の製造装置にも関する。
【００２３】
更に本発明はまた、前記した被覆準微粒子の製造装置において、体積基準頻度分布で平均粒子径が１０μｍを越え２０μｍ以下の芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを８０％以上とする空間領域、
体積基準頻度分布で平均粒子径が２０μｍを越え５０μｍ以下の芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９０％以上とする空間領域、
体積基準頻度分布で平均粒子径が５０μｍを越え３００μｍ以下の芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９５％以上とする空間領域、
体積基準頻度分布で平均粒子径が、３００μｍを越え８００μｍ以下の芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９７％以上とする空間領域、
体積基準頻度分布で平均粒子径が、８００μｍを越える芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９９％以上とする空間領域の内の高分散芯粒子粉体の粒子・気体混合物中の芯粒子粉体の粒子の全ての粒子が通過する面を含む空間領域に、被覆空間の被覆開始領域を位置せしめるか、又は
体積基準頻度分布で平均粒子径が１０μｍを越え２０μｍ以下の芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを８０％以上とする空間領域、
体積基準頻度分布で平均粒子径が２０μｍを越え５０μｍ以下の芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９０％以上とする空間領域、
体積基準頻度分布で平均粒子径が５０μｍを越え３００μｍ以下の芯粒子粉体を準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９５％以上とする空間領域、
体積基準頻度分布で平均粒子径が、３００μｍを越え８００μｍ以下の芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９７％以上とする空間領域、
体積基準頻度分布で平均粒子径が、８００μｍを越える芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９９％以上とする空間領域の内の、回収手段の回収部に回収する全ての粒子が通過する面を含む空間領域に、被覆空間の被覆開始領域を位置せしめることを特徴とする被覆準微粒子の製造装置にも関する。
【００２４】
更に本発明はまた、芯粒子粉体の粒子の粒度分布が、平均粒子径をＤMとしたとき、体積基準頻度分布で（〔ＤM／５，５ＤM〕，≧９０％）であることを特徴とする被覆準微粒子の製造装置にも関する。
【００２５】
而して、本発明によれば、気中において、被覆形成物質の原料から気相法により気相を経て生成する被覆形成物質前駆体と、準微粒子高分散処理手段群の最終処理により気中に分散させた平均粒子径が１０μｍを越える準微粒子からなる高分散芯粒子粉体の粒子・気体混合物を、被覆空間の被覆開始領域で、高分散芯粒子粉体の粒子・気体混合物中の芯粒子粉体の粒子の分散度が粒子の平均粒径に応じてβ≧８０％、β≧９０％、β≧９５％、β≧９７又はβ≧９９％である高分散状態で合流させ、接触及び／又は衝突させて芯粒子粉体の粒子の表面を被覆形成物質で被覆するものである。この場合、被覆形成物質前駆体は、原子、分子、イオン、クラスター、原子クラスター、分子クラスター、クラスターイオン等からなる気相を経て生成したばかりのもので、それ自体はいわば発生期で非常に活性な状態にあり、高分散状態の芯粒子と接触及び／又は衝突を始めることにより、単一粒子状態の個々の芯粒子の表面に被覆形成物質は強固に結合し、その結果、芯粒子粉体の粒子の単一粒子単位で状態が均一な被覆形成物質で且つ各粒子ごとに量の均一な被覆形成物質で被覆してなる被覆粒子が製造できる。
【００２６】
以下に本発明を詳細に説明する前に、本明細書中に使用する用語をはじめに定義することとし、そして必要によってその用語の具体的内容を説明することにする。
【００２７】
被覆粒子
被覆粒子とは、被覆が施された粒子をいう。例えば、具体的には、前記被覆形成物質が、超微粒子状、島状、連続質状、一様な膜状、突起物状等の内の一種以上からなる形態で芯粒子に被覆された粒子をいう。
【００２８】
気相被覆法
気相被覆法とは、被覆形成物質の原料が、真空の分子流、イオン流、プラズマ、ガス、蒸気、エアロゾルの一種以上からなる気相状態を少なくとも一度は経て被覆する方法、又は気相状態の被覆形成物質の原料により被覆する方法をいう。
【００２９】
芯粒子
芯粒子とは、被覆を施す対象物となる粒子をいう。これはまた、母材粒子、種粒子或は被覆される粒子ともいう。
この芯粒子は、基本的にはそれを構成する物質に制限がなく、例えば無機材料、金属材料、有機材料などからなる公知の粉体粒子が芯粒子として使用可能である。
【００３０】
芯粒子粉体
芯粒子粉体とは、芯粒子からなる粉体をいう。芯粒子粉体の粒子とは、芯粒子粉体を構成する粒子をいう。本発明で被覆に供する準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子は、平均粒子径が体積基準頻度分布で１０μｍを越えるものである。
好ましくは、平均粒子径をＤMとしたとき、ＤMが１０μｍを越えて、粒度分布が体積基準頻度分布で（〔ＤM／５，５ＤM〕，≧９０％）である。このような比較的分布幅の狭い粉体では、平均粒子径で粉体の分散特性又は凝集特性が特徴付けられ、ＤMの値に適した条件で微粒子高分散処理手段群を作動させれば分散できる。
平均粒子径が１０μｍを越える芯粒子粉体の粒子の粒度分布が、幅広い分布又は互いに離れた複数のピークを持つ分布の粉体では、好適には適当な選択分離処理、例えば分級処理を行ってそれぞれ分級された粉体ごとに、本発明の被覆処理を施す。これにより、それぞれ分級された粉体ごとに上記条件の下で、被覆空間の被覆開始領域で分散度が平均粒子径に応じて分散度βで８０％以上、９０％以上、９５％以上、９７％以上又は９９％以上の状態で被覆が開始され、芯粒子粉体の粒子一つ一つの粒子に被覆が可能となる。
【００３１】
被覆形成物質
被覆形成物質とは、被覆を施す対象物に被覆を形成する物質をいう。例えば、具体的には、超微粒子状、島状、連続質状、一様な膜状、突起物状等の内の一種以上からなる形態で被覆を形成する物質をいう。
特に、被覆形成物質の形態が超微粒子状の場合、超微粒子の粒子径は、０.００５μｍ〜０.５μｍの範囲のものである。
この被覆形成物質は、得られる被覆粒子に対して希望される性質及び機能に応じて、芯粒子とは同一であるか又は異なった種々の無機材料、金属材料又は有機材料で構成され、例えば酸化物であるＡｌ2Ｏ3、ＳｉＯ2、ＺｒＯ2、Ｙ2Ｏ3、ＣａＯ、ＭｇＯ、ＭｇＡｌ2Ｏ4（スピネル）、Ａｌ2ＳｉＯ5（ムライト）など、窒化物であるＳｉ3Ｎ4、ＡｌＮ、ＴｉＮ、ＺｒＮ、Ｓｉ2Ｎ2Ｏ、ＨｆＮ、ＶxＮ（ｘ＝１〜３）、ＮｂＮ、ＴａＮ、Ｔａ2Ｎ、ＢＮなど、炭化物であるＷＣ、ＳｉＣ、Ｗ2Ｃ、ＨｆＣ、ＴａＣ、Ｔａ2Ｃ、ＮｂＣ、Ｍｏ2Ｃなど、ほう素化物であるＢＰ、ＴｉＢ、ＴｉＢ2、ＺｒＢ2、ＶＢ、Ｖ3Ｂ2、ＶＢ2、ＮｂＢ、ＮｂＢ2、ＴａＢ、ＴａＢ2、ＭｏＢ、ＭｏＢ2、ＭｏＢ4、Ｍｏ2Ｂ、ＷＢ、Ｗ2Ｂ、Ｗ2Ｂ5、ＬａＢ6、Ｂ13Ｐ2など、単体金属、例えばＳｉ、Ａｌ、Ｎｉ、Ｃｏ、Ｃｕ、Ｆｅ、Ｔｉ、Ｗ、Ｂ、Ｎｂ、Ｖ、Ｚｒ、Ｈｆ、Ｔａ、Ｒｅ、Ｃｒ、Ｍｏ、Ｙ、Ｌａなど、及び金属間化合物および合金の種々のもの例えばＴｉＡｌ、Ｔｉ2Ａｌ、ＴｉＡｌ3、ＴｉＮｉ、ＮｉＡｌ、Ｎｉ3Ａｌなどの材料、並びにこれらの材料を複合したものなど及びエポキシ樹脂、フェノール樹脂、ポリアクリルアミド樹脂、ポリアミド樹脂、ウレタン樹脂、ポリエステル樹脂、ポリ塩化ビニル樹脂、アクリル樹脂、ポリエチレン等を用いることができる。
【００３２】
均一な被覆
一様な膜状の被覆形成物質の場合には、単一粒子において被覆膜の厚さがいたるところで均一であることをいう。被覆形成物質が超微粒子状、島状又は突起物状の場合には、超微粒子状、島状又は突起物状の被覆形成物質が均一な分布で被覆することをいう。被覆形成物質の生成過程で、避けられない不均一さは、均一の範疇に含まれるものである。
【００３３】
被覆空間に投入の定義
被覆空間に投入とは、例えば、自由落下等の落下によって芯粒子粉体を被覆空間に導入することをいう。搬送ガスにより投入する場合には、芯粒子粉体を芯粒子粉体の粒子・気体混合物の流れの方向に乗せて導入したり、気体に乗せて流れの方向へ、或いは気体に乗り方向が変えられて導入することをいう。又は、搬送ガスの作用を受けて導入することをもいう。例えば搬送ガスの波動現象、具体的には非線系波動によって導入することをいう。或いは、ガス中の音波、超音波、磁場、電子線等によって被覆空間に導入することをもいう。又、外場、例えば電場、磁場、電子線等により導入することをもいう。具体的には、電場、磁場、電子線等により粉体粒子を帯電させ、又は帯磁させ引力又は斥力により被覆空間に導入することをいう。又、ガスの背圧や減圧によって吸い込まれ、導入することも含む。
【００３４】
被覆空間
被覆空間とは、被覆形成物質の原料から気相を経て生成する被覆形成物質前駆体及び／又は気相状態の被覆形成物質前駆体と芯粒子粉体の粒子が接触及び／又は衝突する空間をいう。或いは、芯粒子粉体の粒子の表面を被覆形成物質で被覆する空間領域をいう。
【００３５】
被覆室
被覆室とは、被覆空間を一部以上共有する室をいう。より具体的には、被覆室とは、被覆空間を含む仕切られた、又は略仕切られた（略閉じた、半閉じた）室であって、被覆空間を一部以上含む室である。
【００３６】
気中
気中とは、真空又は気相状態の空間内をいう。ここで、本発明において、気相状態とは、分子流、イオン流、プラズマ、ガス、蒸気、エアロゾルなどの状態をいう。真空とは、技術的には、減圧状態をさす。どんな減圧下でも、厳密にはガス、分子、原子、イオン等が含まれる。
【００３７】
被覆形成物質前駆体
被覆形成物質前駆体とは、被覆形成物質の前駆体である。より詳しくは、気相状態の被覆形成物質の原料がそのまま、又は被覆形成物質の原料から気相を経て形成及び／又は合成され、被覆を施す対象物となる粒子である芯粒子に被覆を形成する直前の物質をいう。被覆形成物質前駆体は、被覆形成物質の原料から、どこかで気相を経て形成及び／又は合成する限り、状態の制限はない。被覆形成物質の原料が気相の場合、原料が被覆形成物質前駆体にもなりうる。被覆形成物質前駆体そのものが気相であってもよい。又、反応前でも良く、反応中でもよく、反応後でもよい。被覆形成物質前駆体の具体例としては、イオン、原子、分子、クラスター、原子クラスター、分子クラスター、クラスターイオン、超微粒子、ガス、蒸気、エアロゾル等が挙げられる。
【００３８】
被覆形成物質の原料
被覆形成物質の原料とは、気相を経て被覆を形成する物質となる原料物質をいう。被覆形成物質の原料の形態の具体例として、塊状の固体、粉体粒子、気体、液体等が挙げられる。
【００３９】
分散度β
分散度βとは、粉体分散装置の分散性能を評価する指数として増田、後藤氏らが提案（化学工学、第２２回、秋季大会研究発表講演要旨集、Ｐ３４９（１９８９）参照）したように、全粒子の重量に対する、見かけの一次粒子状態の粒子の重量の割合と定義する。ここで、見かけの一次粒子状態の粒子とは、任意の分散状態の粉体粒子の質量基準の頻度分布ｆm2と完全分散されている粉体粒子の質量基準の頻度分布ｆm1のオーバーラップしている部分の割合を示し、次の式のβで表される。
【００４０】
【数１】
【００４１】
上式は質量基準で表した粒度分布を基にして分散度を評価しているが、本来分散度は体積基準で表した粒度分布を基にして評価されるべきものである。しかし粉体粒子密度が同じである場合には質量基準で表した粒度分布と体積基準で表した粒度分布は同じになる。そこで実用上測定が容易な質量基準の粒度分布を測定し、それを体積基準の粒度分布として用いている。従って本来の分散度βは次の式及び図１の斜線部分の面積で表される。
【００４２】
【数２】
そして芯粒子粉体の分布及び平均粒子径は、特に断らない限り基本的には体積基準を用いることとする。
【００４３】
体積基準頻度分布
体積基準頻度分布とは、粒子径の分布をある粒子径に含まれる体積割合をもって表したものをいう。
【００４４】
（〔Ｄ1，Ｄ2〕，≧９０％）の定義
（〔Ｄ1，Ｄ2〕，≧９０％）分布とは、Ｄ1、Ｄ2を粒子径、但しＤ1＜Ｄ2とするとき、Ｄ1以上でＤ2以下の粒子が体積で９０％以上含まれる分布を表し、図１（ｂ）のように斜線の部分の割合が９０％以上である粒子からなる粉体を表す。
【００４５】
体積基準頻度分布（〔ＤM／５，５ＤM〕，≧９０％）の定義
本発明で用いる、粒度分布が、体積基準頻度分布で（〔ＤM／５，５ＤM〕，≧９０％）分布とは、ＤMを体積基準の平均粒子径とするとき、ＤMの１／５倍の粒子径以上、ＤMの５倍の粒子径以下の粒子を体積で９０％以上含む分布を表す。例えば平均粒子径ＤMが２０μｍで体積基準頻度分布が（〔ＤM／５，５ＤM〕，≧９０％）とは、体積基準の平均粒子径が２０μｍで、４μｍ以上且つ１００μｍ以下の粒子径の粒子が体積で９０％以上含まれるような分布を表す。ここで、体積基準の平均粒子径ＤMは、
【数３】
ＤM＝Σ（ｖiＤi）／Σｖi
と表される。
【００４６】
被覆開始領域
準微粒子高分散処理手段群の最終処理後、初めて被覆が開始される領域を被覆開始領域という。従って、準微粒子高分散処理手段群の最終処理以前では、初めて被覆が開始される領域でも、本発明での被覆開始領域ではない。
【００４７】
被覆開始領域での分散度β
本発明では、（１）体積基準頻度分布で平均粒径が１０μｍを越え２０μｍ以下の芯粒子粉体を準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを８０％以上とするか、又は（２）体積基準頻度分布で平均粒径が２０μｍを越え５０μｍ以下の芯粒子粉体を準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９０％以上とするか、又は（３）体積基準頻度分布で平均粒径が５０μｍを越え３００μｍ以下の芯粒子粉体を準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９５％以上とするか、又は（４）体積基準頻度分布で平均粒子径が３００μｍを越え８００μｍ以下の芯粒子粉体を準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９７％以上とするか、又は（５）体積基準頻度分布で平均粒子径が８００μｍを越える芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９９％以上とした領域に被覆空間の被覆開始領域を位置せしめた被覆室を設ける。
【００４８】
上記した被覆空間の被覆開始領域における分散度であれば、芯粒子粉体の粒子が、体積基準頻度分布で平均粒子径が１０μｍを越える準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、実質的に気中に単一粒子状態に分散でき、被覆空間の被覆開始領域を通過する全ての芯粒子粉体の粒子の表面に、被覆形成物質前駆体が均等に接触及び／又は衝突するため、単一粒子に均一な量の被覆形成物質を付けることができる。
平均粒子径が１０μｍを越える準微粒子において、上記分散度βは、芯粒子粉体の平均粒子径と共に連続的に変化するが、表現困難なため便宜的に段階的な表現とした。
【００４９】
好適には、（１）体積基準頻度分布で平均粒径が１０μｍを越え２０μｍ以下の芯粒子粉体を準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９０％以上とするか、又は（２）体積基準頻度分布で平均粒径が２０μｍを越え５０μｍの芯粒子粉体を準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９５％以上とするか、又は（３）体積基準頻度分布で平均粒子径が５０μｍを越え３００μｍ以下の芯粒子粉体を準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９７％以上とするか、又は（４）体積基準頻度分布で平均粒子径が３００μｍを越える芯粒子粉体を準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９９％以上とした空間領域に被覆空間の被覆開始領域を位置せしめた被覆室を設けることである。被覆空間の被覆開始領域をこのように位置せしめた被覆室であれば、芯粒子粉体の粒子が、体積基準頻度分布で平均粒子径が１０μｍを越える準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子に対して、単一粒子単位で被覆形成物質をより均一に被覆でき、且つ各芯粒子ごとに被覆量のより均一な被覆ができる。
【００５０】
体積基準頻度分布で平均粒子径が１０μｍを越える準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子は、気中に於いては凝集作用が働き、粒子同士で接触及び／又は衝突しあい高分散芯粒子粉体の粒子・気体混合物中の芯粒子粉体の粒子の分布が不均一になる。しかし、上記、芯粒子粉体の粒子の粒径に応じた分散度のごとき分散状態で被覆を開始すれば、準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子単一粒子単位により均一に被覆形成物質を被覆でき、且つ各粒子ごとにより均一な量に被覆形成物質を被覆できる。
【００５１】
準微粒子高分散処理手段群
本発明に於いて、準微粒子高分散処理手段群とは、
（Ａ） 少なくとも分散手段を１以上有し、
（Ｂ） 最終の処理手段として、
（ａ）芯粒子粉体の粒子を気中に分散させる分散手段、又は、（ｂ）芯粒子粉体の粒子を気中に分散させた芯粒子粉体の粒子と気体との混合物において低分散芯粒子粉体部分を分離し、芯粒子粉体の粒子が主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物を選択する高分散芯粒子粉体の粒子・気体混合物選択手段とこの高分散芯粒子粉体の粒子・気体混合物選択手段により分離された低分散芯粒子粉体部分をこの準微粒子高分散処理手段群中の分散手段の内の最終分散手段及び／又は最終分散手段以前の処理手段に搬送するフィードバック手段とを備えた高分散芯粒子粉体の粒子・気体混合物選択手段を有するものである。
【００５２】
好適には、（１）体積基準頻度分布で平均粒径が１０μｍを越え２０μｍ以下の芯粒子粉体を準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを８０％以上とするか、又は（２）体積基準頻度分布で平均粒径が２０μｍを越え５０μｍ以下の芯粒子粉体を準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９０％以上とするか、又は（３）体積基準頻度分布で平均粒径が５０μｍを越え３００μｍ以下の芯粒子粉体を準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９５％以上とするか、又は（４）体積基準頻度分布で平均粒子径が３００μｍを越え８００μｍ以下の芯粒子粉体を準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９７％以上とするか、又は（５）体積基準頻度分布で平均粒子径が８００μｍを越える芯粒子粉体を、準微粒子高分散処理手段群の最終処理により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とし、その芯粒子粉体の粒子の分散度βを９９％以上とする分散性能を有するものである。
前記被覆開始領域における種々の分散度に対応してそれらと同等以上の分散性能の準微粒子高分散処理手段群を設けることにより、被覆開始領域において、各分散度に応じた高品位な被覆を施すことができる。
【００５３】
最終処理手段
準微粒子高分散処理手段群の最終の処理手段が分散手段の場合、この分散処理手段を微粒子高分散処理手段群の最終処理手段という。又、準微粒子高分散処理手段群の最終の処理手段が、準微粒子高分散処理手段の最終の分散手段へ、高分散芯粒子粉体の粒子・気体混合物選択処理工程時に於いて低分散状態であったために選択分離された部分を搬送するフィードバック手段を備えた高分散芯粒子粉体の粒子・気体混合物選択手段、又は最終の分散手段より前の処理手段に、高分散芯粒子粉体の粒子・気体混合物選択処理工程時に於いて低分散状態であったために選択分離された部分を搬送するフィードバック手段を備えた高分散芯粒子粉体の粒子・気体混合物選択手段の場合、この高分散芯粒子粉体の粒子・気体混合物選択手段を準微粒子高分散処理手段群の最終処理手段という。
【００５４】
尚、準微粒子高分散処理手段群の最終処理手段であるフィードバック手段を備えた高分散芯粒子粉体の粒子・気体混合物選択手段より前に設ける（例えば、このフィードバック手段を備えた高分散芯粒子粉体の粒子・気体混合物選択手段と最終分散手段の間、或いは最終分散手段より前）高分散芯粒子粉体の粒子・気体混合物選択手段は、フィードバック手段の有無にかかわらず微粒子高分散処理手段群の構成要素である。
【００５５】
分散手段
分散するために用いる手段を分散手段という。少しでも或いは僅かでも分散効果を有するものは分散手段として使用可能であり、本発明ではこれを分散手段とする。例えば、一般に供給手段として用いる空気輸送用のロータリーフィーダーやインジェクションフィーダー（粉体工学会編：“粉体工学便覧”、日刊工業新聞社（１９８６）Ｐ５６８、Ｐ５７１）は、分散効果も有するので、分散目的の手段として使用する場合は分散手段である。後述の分散維持・促進手段も分散目的で（βを高める目的で）使用する場合は分散手段となる。
【００５６】
本発明において、準微粒子高分散処理手段群は、芯粒子粉体の粒子の加速及び／又は速度勾配に置く気流による分散、芯粒子粉体の粒子の静止障害物及び／又は回転体である障害物への衝突による分散、芯粒子粉体の粒子の流動層及び／又は脈流及び／又は回転ドラム及び／又は振動及び／又は掻取りからなる機械的解砕による分散の内の選択された一種以上の分散の機構を備えたものである。
【００５７】
具体的には、準微粒子高分散処理手段群は、エジェクタ型分散機、ベンチュリ型分散機、細管、撹拌機、気流中の障害物を利用した分散機、ジェットの吹付けを利用した分散機、螺旋管、回転羽根を利用した分散機、回転するビンを利用した分散機（ケージミル）、流動層型分散機、脈流を利用した分散機、回転ドラムを利用した分散機、振動を利用した分散機、振動ふるい、スクレーパによる掻き取りを利用した分散機、SAEI、Gonell式分散機、中条式分散機、Roller式分散機、オリフィス型分散機、B.M式分散機、Timbrell式分散機、Wright式分散機の内の選択された一種以上からなる分散手段を備えた物である。（粉体工学会編：“粉体工学便覧”、日刊工業新聞社（１９８６）Ｐ４３０）。
【００５８】
また、特開昭５６−１３３６号に記載の撹拌羽根を利用した分散機、特開昭５８−１６３４５４号に記載の高速気流と分散ノズルを利用した分散機、特開昭５９−１９９０２７号に記載の回転羽根による分散作用とプラズマイオンによる分散作用を利用した分散機、特開昭５９−２０７３１９号に記載のプラズマイオンによる分散作用を利用した分散機、特開昭５９−２１６６１６号に記載のエジェクタとプラズマイオンによる分散作用を利用した分散機、特開昭５９−２２５７２８号に記載のエジェクタとイオン流の分散作用を利用した分散機、特開昭５９−１８３８４５号に記載のプラズマイオンの分散作用を利用した分散機、特開昭６３−１６６４２１号に記載の分散羽根と圧力気体による分散作用を利用した分散機、特開昭６２−１７６５２７号に記載のライン状又はリング状スリット型噴出口を用いた分散機、特開昭６３−２２１８２９号に記載の網状羽根を利用した分散機、特開昭６３−１６２９号に記載の噴射ノズルからの高速気流による分散作用を利用した分散機、実開昭６３−９２１８号に記載の多数の細孔を利用した分散機、実開昭６２−１５６８５４号に記載のエジェクタ型分散機、実開昭６３−６０３４号に記載の細孔とオリフィスを利用した分散機等に記載のものも使用可能である。
【００５９】
準微粒子高分散処理手段群に好適な分散手段として、特願昭６３−３１１３５８号、特願平１−７１０７１号、特願平２−２１８５３７号等に記載の装置が挙げられる。
【００６０】
高分散芯粒子粉体の粒子・気体混合物選択手段
芯粒子粉体の粒子・気体混合物のなかから、主に単一粒子状態の粒子を含む高分散芯粒子粉体の粒子・気体混合物以外の低分散芯粒子粉体部分を分離し、主に単一粒子状態の粒子を含む高分散芯粒子粉体の粒子・気体混合物を選択する手段をいう。一次粒子の集合体である凝集粒子は、見かけの粒子径が一次粒子の粒子径に比べ大きくなることから、例えば乾式分級手段により分離が可能である。この高分散芯粒子粉体の粒子・気体混合物選択手段の例としては、重力を利用した分級手段、慣性力を利用した分級手段、遠心力を利用した分級手段、静電気を利用した分級手段、流動層を利用した分級手段等から一種以上選択された乾式分級手段が挙げられる。
【００６１】
この高分散芯粒子粉体の粒子・気体混合物選択手段の例としては、重力分級機、慣性分級機、遠心分級機、サイクロン、エアセパレータ、ミクロンセパレータ、ミクロプレックス、ムルチプレックス、ジグザグ分級機、アキュカット、コニカルセパレータ、ターボクラシファイア、スーパセパレータ、ディスパージョンセパレータ、エルボジェット、流動層分級機、バーチュアルインパクタ、O-Sepa、ふるい、バイブレーティングスクリーン、シフタ（粉体工学会編：“粉体工学便覧”日刊工業新聞社、Ｐ５１４（１９８６））等が挙げられる。
【００６２】
芯粒子粉体の粒子・気体混合物
芯粒子粉体の粒子・気体混合物とは、(ａ)芯粒子粉体の粒子が気中に一様に浮遊した均質流れ（一様な浮遊流れ）、(ｂ)芯粒子粉体の粒子が気中のある領域で非一様な分布を示す不均質流れ（非均質浮遊流れ）、(ｃ)芯粒子粉体の粒子の摺動層を伴う流れ（摺動流れ）、又は(ｄ)芯粒子粉体の粒子の静止層を伴う流れをいう。
【００６３】
低分散芯粒子粉体の粒子・気体混合物
芯粒子粉体の粒子・気体混合物の内、芯粒子粉体の粒子が主に単一粒子状態以外の状態で気中に存在する芯粒子粉体の粒子・気体混合物をいう。
【００６４】
高分散芯粒子粉体の粒子・気体混合物
芯粒子粉体の粒子が主に単一粒子状態で気中に存在する芯粒子粉体の粒子・気体混合物をいう。高分散芯粒子粉体の粒子・気体混合物は、極めて高分散であっても、実際には凝集粒子を含む。低分散芯粒子粉体の粒子・気体混合物は、実際には、凝集していない単粒子を含み、選択分離して低分散芯粒子粉体の粒子・気体混合物と高分散芯粒子粉体の粒子・気体混合物に分けられる。低分散芯粒子粉体の粒子・気体混合物は、凝集粒子の選択分離及び／又は再分散により、高分散芯粒子粉体の粒子・気体混合物となる。
【００６５】
回収手段
被覆空間で被覆した被覆準微粒子を取り出す手段を回収手段という。回収手段の内で回収処理の行われる部分を回収部という。被覆空間の被覆開始領域を通過して被覆した被覆準微粒子は、気中から直接取り出して回収するか、又は気中から取り出して一時的に蓄えてから回収するか、又は、気体と共に回収される。
回収手段の回収部としては、隔壁（障害物）を利用した回収手段の回収部、重力を利用した回収手段の回収部、慣性力を利用した回収手段の回収部、遠心力を利用した回収手段の回収部、帯電による引力を利用した回収手段の回収部、熱泳動力を利用した回収手段の回収部、ブラウン拡散を利用した回収手段の回収部、ガスの背圧や減圧等による吸引力を利用した回収手段の回収部等が利用可能である。
この回収手段の回収部の好適な例として、重力集塵機、慣性集塵機、遠心力集塵機、濾過集塵機、電気集塵機、洗浄集塵機、粒子充填層、サイクロン、バグフィルター、セラミックスフィルター、スクラバー等が挙げられる。
【００６６】
準微粒子高分散処理手段群の図の説明
図２(ａ)は本発明の準微粒子高分散処理手段群の基本的な構成の一例を表すブロック図である。芯粒子粉体の粒子を分散させる最終の分散手段Ａ、最終の分散手段以前の分散処理手段群の構成要素ｄで構成されている。εは、芯粒子粉体の粒子の内、主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物である。構成要素ｄとしては、分散手段、供給手段、高分散芯粒子粉体の粒子・気体混合物選択手段等任意の処理手段を単独又は組み合わせて使用できる。構成要素ｄは、必ずしも設けなくとも良い。準微粒子高分散処理手段群は、、最終の処理手段である分散手段Ａの処理後、（１）体積基準頻度分布で平均粒子径が１０μｍを越え２０μｍ以下の芯粒子粉体に対し、分散度がβで８０％以上、又は（２）体積基準頻度分布で平均粒子径が２０μｍを越え５０μｍ以下の芯粒子粉体に対し、分散度がβで９０％以上、又は（３）体積基準頻度分布で平均粒子径が５０μｍを越え３００μｍ以下の芯粒子粉体に対し、分散度がβで９５％以上、又は（４）体積基準頻度分布で平均粒子径が３００μｍを越え８００μｍ以下の芯粒子粉体に対し、分散度がβで９７％以上、又は（５）体積基準頻度分布で平均粒子径が８００μｍを越える芯粒子粉体に対し、分散度がβで９９％以上を実現できる構成のものである。
【００６７】
図２(ｂ)は、本発明の準微粒子高分散処理手段群の基本的な構成の他の一例を表すブロック図である。芯粒子粉体の粒子を分散させる最終の分散手段Ａ、最終の分散手段Ａへ芯粒子粉体の粒子が、主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物、以外の低分散芯粒子粉体の粒子・気体混合物ηをフィードバックさせるフィードバック手段Ｃを備えた最終の高分散芯粒子粉体の粒子・気体混合物選択手段Ｂ、最終の分散手段以前の分散処理手段群の構成要素ｄ、最終分散手段と最終選択手段の間の準微粒子高分散処理手段群の構成要素ｅで構成されている。εは、芯粒子粉体の粒子の内、主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物である。構成要素ｄとしては、分散手段、供給手段、選択手段等任意の処理手段を単独又は組み合わせて使用できる。構成要素ｅとしては、分散手段以外の処理手段、例えば供給手段、選択手段等任意の処理手段を単独又は組み合わせて使用できる。構成要素ｄ及びｅは、必ずしも設けなくとも良い。準微粒子高分散処理手段群は、最終の処理手段である選択手段Ｂによる処理後、前記平均粒子径の芯粒子粉体に対し前記分散度を実現できる構成のものである。
【００６８】
図２(ｃ)は、本発明の準微粒子高分散処理手段群の基本的な構成の他の一例を表すブロック図である。芯粒子粉体の粒子を分散させる最終の分散手段Ａ、最終の分散手段Ａより前の処理手段へ芯粒子粉体の粒子が、主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物、以外の低分散芯粒子粉体の粒子・気体混合物ηをフィードバックさせるフィードバック手段Ｃを備えた高分散芯粒子粉体の粒子・気体混合物選択手段Ｂ、最終の分散手段以前の準微粒子高分散処理手段群の構成要素ｄ、最終の分散手段と最後の選択手段の間の準微粒子高分散処理手段群の構成要素ｅで構成されている。εは、芯粒子粉体の粒子の内、主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物である。構成要素ｄとしては、分散手段、供給手段、選択手段等任意の処理手段を単独又は組み合わせて使用できる。構成要素ｄとしては、分散手段以外の処理手段、例えば供給手段、選択手段等任意の処理手段を単独又は組み合わせて使用できる。構成要素ｄ及びｅは、必ずしも設けなくとも良い。準微粒子高分散処理手段群は、最終の処理手段である選択手段Ｂによる処理後、前記平均粒子径の芯粒子粉体に対し前記分散度を実現できる構成のものである。
【００６９】
なお、以上のような構成であるから、供給槽、芯粒子生成手段等の粉体の供給源も本準微粒子高分散処理手段群の構成に含めてもよい。例えば図２(ｃ)の場合、フィードバック手段Ｃのフィードバック先を供給槽とする構成も高分散処理手段群の構成として良いことは言うまでもない。又、準微粒子高分散処理手段群の分散工程の前に、芯粒子粉体の粒子を解砕及び／又は粉砕する解砕工程を入れても良いことは言うまでもない。
【００７０】
上記した準微粒子高分散処理手段群の基本的な構成をより詳細にしたブロック図に基づいて更に詳しく説明することにする。
【００７１】
構成１
図３(ａ)は、本発明の準微粒子高分散処理手段群の第１の構成を説明するブロック図であって図２(ａ)に対応するものである。本例は、被覆される芯粒子粉体を供給する供給槽１００、被覆される芯粒子粉体を分散させる最終分散手段Ａから構成されている。εは、芯粒子粉体の粒子の内、主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物である。
【００７２】
構成２
図３(ｂ)は、本発明の準微粒子高分散処理手段群の第２の構成を説明するブロック図であって図２(ａ)に対応するものである。本例は、被覆される芯粒子粉体を供給する供給槽１００、被覆される芯粒子粉体を分散させる分散手段ａ、被覆される芯粒子粉体を分散させる最終分散手段Ａから構成されている。εは、芯粒子粉体の粒子の内、主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物である。
【００７３】
構成３
図３(ｃ)は、本発明の準微粒子高分散処理手段群の第３の構成を説明するブロック図であって図２(ｂ)に対応するものである。本例は、被覆される芯粒子粉体を供給する供給槽１００、被覆される芯粒子粉体を分散させる分散手段ａ、分散手段ａで分散させた芯粒子粉体の粒子・気体混合物のうちから主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物、以外の低分散芯粒子粉体の粒子・気体混合物ηを分散手段ａへフィードバックさせるフィードバック手段Ｃ、主に高分散芯粒子粉体の粒子・気体混合物を最終の分散手段Ａへ導入する高分散芯粒子粉体の粒子・気体混合物選択手段ｂ、被覆される芯粒子粉体を分散させる最終分散手段Ａ、から構成されている。εは、芯粒子粉体の粒子の内、主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物である。
【００７４】
構成４
図３(ｄ)は、本発明の準微粒子高分散処理手段群の第４の構成を説明するブロック図であって図２(ｂ)に対応するものである。本例は、被覆される芯粒子粉体を供給する供給槽１００、被覆される芯粒子粉体を分散させる最終分散手段Ａ、最終分散手段Ａで分散させた芯粒子粉体の粒子・気体混合物のうちから主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物、以外の低分散芯粒子粉体の粒子・気体混合物ηを分散手段Ａへフィードバックするフィードバック手段Ｃ、高分散芯粒子粉体の粒子・気体混合物を放出する最終の高分散芯粒子粉体の粒子・気体混合物選択手段Ｂから構成されている。εは、芯粒子粉体の粒子の内、主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物である。
【００７５】
構成５
図３(ｅ)は、本発明の準微粒子高分散処理手段群の第５の構成を説明するブロック図であって図２(ｂ)に対応するものである。本例は、被覆される芯粒子粉体を供給する供給槽１００、被覆される芯粒子粉体を分散させる分散手段ａ、被覆される芯粒子粉体を分散させる最終分散手段Ａ、最終分散手段Ａで分散させた芯粒子粉体の粒子・気体混合物のうちから主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物、以外の低分散芯粒子粉体の粒子・気体混合物ηを分散手段Ａへフィードバックするフィードバック手段Ｃ、高分散芯粒子粉体の粒子・気体混合物を放出する最終の高分散芯粒子粉体の粒子・気体混合物選択手段Ｂから構成されている。εは、芯粒子粉体の粒子の内、主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物である。
【００７６】
構成６
図３(ｆ)は、本発明の準微粒子高分散処理手段群の第６の構成を説明するブロック図であって図２(ｂ)に対応するものである。本例は、被覆される芯粒子粉体を供給する供給槽１００、芯粒子粉体の粒子・気体混合物のうちから主に低分散芯粒子粉体の粒子・気体混合物を取り除き、主に高分散芯粒子粉体の粒子・気体混合物を分散手段Ａへ導入する高分散芯粒子粉体の粒子・気体混合物選択手段ｂ、選択分離された芯粒子粉体の粒子を分散させる最終分散手段Ａ、最終分散手段Ａで分散させた芯粒子粉体の粒子・気体混合物のうちから主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物、以外の低分散芯粒子粉体の粒子・気体混合物ηを分散手段Ａへフィードバックさせるフィードバック手段Ｃ、高分散芯粒子粉体の粒子・気体混合物を放出する最終の高分散芯粒子粉体の粒子・気体混合物選択手段Ｂから構成されている。εは、芯粒子粉体の粒子の内、主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物である。
【００７７】
構成７
図３(ｇ)は、本発明の準微粒子高分散処理手段群の第７の構成を説明するブロック図であって図２(ｃ)に対応するものである。本例は、被覆される芯粒子粉体を供給する供給槽１００、被覆される芯粒子粉体を分散させる分散手段ａ、被覆される芯粒子粉体を分散させる最終分散手段Ａ、最終分散手段Ａで分散させた芯粒子粉体の粒子・気体混合物のうちから主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物、以外の低分散芯粒子粉体部分ηを分散手段ａへフィードバックするフィードバック手段Ｃ、高分散芯粒子粉体の粒子・気体混合物を放出する最終の高分散芯粒子粉体の粒子・気体混合物選択手段Ｂから構成されている。εは、芯粒子粉体の粒子の内、主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物である。
【００７８】
このようにして達成された準微粒子の高分散状態を維持するために、気中分散維持手段を準微粒子高分散処理手段群に付加することもできる。ここで気中分散維持手段とは、気中に分散担持された芯粒子粉体の粒子の再凝集を防止して分散度βを維持する手段をいう。又、このようにして達成された芯粒子の高分散状態を促進するために、気中分散促進手段を微粒子高分散処理手段群と被覆室の間に付加することもできる。ここでいう気中分散促進手段とは、気中に分散担持された芯粒子粉体の粒子のうち主に再凝集した粒子の再分散を促進し、分散状態の低下を鈍らせたり、一旦低下した分散状態を元の高分散の状態まで回復するように再分散を促す手段をいう。
この気中分散維持手段又は気中分散促進手段の好適な例としては、パイプ振動装置、パイプ加熱装置、プラズマ発生装置、荷電装置等が挙げられる。
【００７９】
パイプ振動装置は、発振器を設置したパイプの振動により、気中に分散している粒子に分散機とは言えない振動を与えることで、再凝集を抑制し高分散状態を維持する手段又は再凝集した粒子の分散を促進する手段である。
パイプ加熱装置は、加熱したパイプにより搬送気体の外側から熱を加えて搬送気体を膨張させ、分散機とは言えないほどに流速を加速して再凝集を抑制し、再凝集した粒子の分散を促進する手段である。
【００８０】
プラズマ発生装置は、芯粒子粉体を分散担持している気中にプラズマを発生させ、そのプラズマイオンと芯粒子との衝突により、再凝集を抑制し高分散状態を維持する手段又は再凝集した粒子の分散を促進する手段である。
荷電装置は、芯粒子粉体を分散担持している気中に、コロナ放電、電子ビーム、放射線等の方法で単極イオンを発生させ、単極イオン雰囲気中を通過させることで粒子を単極に帯電させ、静電気の斥力により再凝集を抑制し高分散状態を維持する手段又は再凝集した粒子の分散を促進する手段である。
【００８１】
このようにして形成された準微粒子の高分散状態の芯粒子粉体は粒子の表面を被覆形成物質で被覆するために被覆室に送られる。この被覆室には被覆開始領域を含む被覆空間が設けられている。
【００８２】
準微粒子高分散処理手段群と被覆室とは直結することが望ましいが、搬送に不可避の中空部材及び／又はパイプを使って接続しても良い。この場合にも、被覆開始領域での分散度βを上記した範囲の値とすることが不可欠である。
準微粒子高分散処理手段群と被覆室を別々に置いてその間を連結する場合は、芯粒子粉体をその分散状態のまま被覆室へ導入してやれば良い。そのためには、この間に芯粒子粉体の分散状態を維持するための装置である気中分散維持手段及び／又は分散状態を高めるための装置である気中分散促進手段及び／又は芯粒子粉体の粒子・気体混合物から、低分散芯粒子粉体部分を分離し、主に単一粒子状態の粒子を含む高分散芯粒子粉体の粒子・気体混合物を選択する高分散芯粒子粉体の粒子・気体混合物選択手段を設けることもできる。
【００８３】
準微粒子高分散処理手段群において気中分散された直後の芯粒子粉体の中から、主に凝集した粒子からなる低分散状態の粒子と主に一次粒子からなる高分散状態の芯粒子粉体を選択分離し、高分散状態の部分のみを被覆室に送り出す高分散芯粒子粉体の粒子・気体混合物選択手段を介して、準微粒子高分散処理手段群を被覆室へ接続すれば、効果的に被覆処理を行うことができる。
又、本発明においては、準微粒子高分散処理手段群が、(１)被覆室、又は(２)被覆空間、又は(３)被覆開始領域と一部以上空間を共有することもできる。
【００８４】
すなわち、準微粒子高分散処理手段群中の分散空間と被覆室とを、または準微粒子高分散処理手段群中の分散空間と被覆開始領域を有する被覆空間とを、または準微粒子高分散処理手段群中の分散空間と被覆開始領域とを、空間的に共有することもできる。
ここで被覆開始領域とは、(１)体積基準頻度分布で平均粒径が１０μｍを越え２０μｍ以下の芯粒子粉体にあっては粒子の分散度βが８０％以上、(２)体積基準頻度分布で平均粒径が２０μｍを越え５０μｍ以下の芯粒子粉体にあっては粒子の分散度βが９０％以上、又は(３)体積基準頻度分布で平均粒径が５０μｍを越え３００μｍ以下の芯粒子粉体にあっては粒子の分散度βが９５％以上、（４）体積基準頻度分布で平均粒径が３００μｍを越え８００μｍ以下の芯粒子粉体にあっては粒子の分散度βが９７％以上、（５）体積基準頻度分布で平均粒径が８００μｍを越える芯粒子粉体にあっては粒子の分散度βが９９％以上である分散状態で搬送された高分散状態の芯粒子粉体に気相を経て生成する被覆形成物質前駆体及び／又は気相状態の被覆形成物質前駆体が接触及び／又は衝突し、被覆を開始する領域を指し、次の図４(ａ)〜(ｅ)で示される態様が考慮される。
【００８５】
すなわち、図４(ａ)〜(ｅ)において被覆開始領域は２で示される領域である。図４(ａ)において、芯粒子の平均粒子径に応じて上記した分散度βの分散状態で被覆を始める被覆空間の被覆開始領域２を準微粒子高分散処理手段群又は準微粒子高分散処理手段群の一部、好適には準微粒子高分散処理手段群の放出部１を覆って設ける。
図４(ｂ)において準微粒子高分散処理手段群又は準微粒子高分散処理手段群の一部、好適には準微粒子高分散処理手段群の放出部１から放出される芯粒子粉体の粒子４が全て通る前記被覆空間の被覆開始領域２を設ける。
上記の構成により、全ての芯粒子粉体の粒子は上記した分散度βの分散状態で被覆始められる。
図４(ｃ)において準微粒子高分散処理手段群又は準微粒子高分散処理手段群の一部で好適には準微粒子高分散処理手段群の放出部１から放出される芯粒子粉体の粒子４の内、回収部５に入る粒子は必ず通過する前記被覆空間の被覆開始領域２を設ける。
図４(ｄ)において回収部５を囲む前記被覆空間の被覆開始領域２を設ける。
図４(ｅ)において高分散芯粒子粉体の粒子・気体混合物の粒子のみが到達可能な位置に回収部５を設ける。従って、ここでの領域６は重力を利用した選択手段となる。回収部に入る高分散芯粒子粉体の粒子・気体混合物の粒子が、必ず通過する前記被覆空間の被覆開始領域２を図の斜線部のように設ける。このようにすることで上記した分散度βの分散状態で被覆始めた芯粒子のみ回収でき、被覆開始領域を通っていない芯粒子と被覆開始領域を通過した被覆準微粒子とは混ざることはない。
【００８６】
上記したところから、本発明を実施する装置は、準微粒子高分散処理手段群と被覆室又は準微粒子高分散処理手段群と被覆室と回収手段から構成されるものであるが、これらの装置の構成要素は、種々の組み合わせ方をすることが可能で、これらの装置の構成例を図面にもとづいて説明するとつぎのとおりである。
【００８７】
装置の構成１
図５(ａ)は、本発明を実施する第一の装置の構成を説明するブロック図である。本例のこの装置は、被覆装置の製造装置本体２−Ａ、被覆室２−Ｂ１、被覆空間２−Ｂ２、被覆開始領域２−Ｂ３、準微粒子高分散処理手段群２−Ｃ１、回収手段２−Ｄから構成されている。準微粒子高分散処理手段群２−Ｃ１は、被覆室２−Ｂ１に直結してある。
【００８８】
装置の構成２
図５(ｂ)は、本発明を実施する第二の装置の構成を説明するブロック図である。本例のこの装置は、被覆装置の製造装置本体２−Ａ、被覆室２−Ｂ１、被覆空間２−Ｂ２、被覆開始領域２−Ｂ３、準微粒子高分散処理手段群２−Ｃ１、不可避の中空部材２−Ｃ２、回収手段２−Ｄから構成されている。準微粒子高分散処理手段群２−Ｃ１は、被覆室２−Ｂ１に不可避の中空部材２−Ｃ２を介して接続してある。
【００８９】
装置の構成３
図５(ｃ)は、本発明を実施する第三の装置の構成を説明するブロック図である。本例のこの装置は、被覆装置の製造装置本体２−Ａ、被覆室２−Ｂ１、被覆空間２−Ｂ２、被覆開始領域２−Ｂ３、準微粒子高分散処理手段群２−Ｃ１、気中分散維持手段２−Ｃ３、回収手段２−Ｄから構成されている。準微粒子高分散処理手段群２−Ｃ１は、被覆室２−Ｂ１に気中分散維持手段２−Ｃ３を介して接続してある。
【００９０】
装置の構成４
図５(ｄ)は、本発明を実施する第四の装置の構成を説明するブロック図である。本例のこの装置は、被覆装置の製造装置本体２−Ａ、被覆室２−Ｂ１、被覆空間２−Ｂ２、被覆開始領域２−Ｂ３、準微粒子高分散処理手段群２−Ｃ１、回収手段２−Ｄから構成されている。準微粒子高分散処理手段群２−Ｃ１は、被覆室２−Ｂ１と空間を共有している。
【００９１】
装置の構成５
図５(ｅ)は、本発明を実施する第五の装置の構成を説明するブロック図である。本例のこの装置は、被覆装置の製造装置本体２−Ａ、被覆室２−Ｂ１、被覆空間２−Ｂ２、被覆開始領域２−Ｂ３、準微粒子高分散処理手段群２−Ｃ１、回収手段２−Ｄから構成されている。準微粒子高分散処理手段群２−Ｃ１は、被覆室２−Ｂ１中に設けている。
【００９２】
装置の構成６
図５(ｆ)は、本発明を実施する第六の装置の構成を説明するブロック図である。本例のこの装置は、被覆装置の製造装置本体２−Ａ、被覆室２−Ｂ１、被覆空間２−Ｂ２、被覆開始領域２−Ｂ３、準微粒子高分散処理手段群２−Ｃ１、回収手段２−Ｄから構成されている。準微粒子高分散処理手段群２−Ｃ１の分散空間中に、被覆室２−Ｂ１を設けている。
【００９３】
装置の構成７
図５(ｇ)は、本発明を実施する第七の装置の構成を説明するブロック図である。本例のこの装置は、被覆装置の製造装置本体２−Ａ、被覆室２−Ｂ１、被覆空間２−Ｂ２、被覆開始領域２−Ｂ３、準微粒子高分散処理手段群２−Ｃ１、回収手段２−Ｄ、再被覆供給手段２−Ｅから構成されている。回収手段２−Ｄから被覆後の被覆準微粒子を高分散処理手段群２−Ｃ１に再被覆供給手段２−Ｅにより搬送して、繰り返して被覆処理が行える。
かかる構成の装置のすべてが本発明に含まれるものである。
【００９４】
上記のようにして芯粒子粉体を被覆形成物質で被覆した被覆準微粒子について、再び被覆形成物質で被覆すること、またはこの再被覆を反復することができる。この場合、被覆準微粒子は再被覆供給手段に送られる。ここで、再被覆供給手段とは、再被覆を行うために被覆後の被覆準微粒子を準微粒子高分散処理手段群へ搬送する手段をいう。具体的には、(ａ)被覆準微粒子を回収する回収手段、及び(ｂ)回収手段から準微粒子高分散処理手段群に被覆準微粒子を搬送する被覆粒子搬送手段を備えた手段である。または、(ａ)被覆準微粒子を回収する回収手段、(ｂ)回収手段から準微粒子高分散処理手段群に被覆準微粒子を搬送する被覆粒子搬送手段、(ｃ)及び被覆後の被覆準微粒子を分級する被覆粒子分級手段を備えた手段である。被覆量が多い場合、被覆前の芯粒子粉体の粒子の粒度分布と被覆後の被覆準微粒子の粒度分布は変わってしまう。そこで、被覆後の被覆準微粒子の粒度分布を被覆粒子分級手段により調整し、再被覆処理を行えば効果的である。
【００９５】
この再被覆処理は、必要によって繰り返すことが出来、そして被覆形成物質の被覆量を所望のものに設定することが出来る。更に、この被覆形成物質の種類を変えてこの被覆処理を繰り返すことが出来、このようにして複数成分の物質を被覆形成物質として多重被覆することも出来る。
【００９６】
本発明に適用する被覆準微粒子の製造装置は、被覆形成物質が、気相を経る気相法によって、芯粒子粉体の粒子表面に被覆される被覆準微粒子の製造装置であれば制限はない。例えば、化学蒸着（ＣＶＤ）装置としては、熱ＣＶＤ装置、プラズマＣＶＤ装置、電磁波を利用したＣＶＤ（可視光線ＣＶＤ、レーザＣＶＤ、紫外線ＣＶＤ、赤外線ＣＶＤ、遠赤外線ＣＶＤ）装置、ＭＯＣＶＤ装置等、或いは、物理蒸着（ＰＶＤ）装置としては、真空蒸着装置、イオンスパッタリング装置、イオンプレーティング装置等が適用可能である。より具体的には、例えば、特開平３−７５３０２号公報の超微粒子で表面が被覆された粒子およびその製造方法に記載の被覆粒子製造装置が好適である。
【００９７】
以上述べた通り、本発明では準微粒子芯粒子粉体、又は主に準微粒子からなる芯粒子粉体の粒子を被覆空間に投入し気相を経て生成する被覆形成物質前駆体及び／又は気相状態の被覆形成物質前駆体をこの芯粒子粉体の粒子に接触及び／又は衝突させてこの芯粒子粉体の粒子の表面を被覆形成物質で被覆する被覆準微粒子が製造されるが、本発明の基本的な工程を要約すると次の通りである。
【００９８】
Ｉ
（Ａ） 準微粒子高分散処理手段群により、体積基準頻度分布で平均粒子径が１０μｍを越える準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、気中に分散させて高分散芯粒子粉体の粒子・気体混合物とする分散工程、
（Ｂ） この分散工程で分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子を、
その平均粒子径が１０μｍを越え２０μｍ以下のときには分散度βが８０％以上、
２０μｍを越え５０μｍ以下のときには分散度βが９０％以上、
５０μｍを越え３００μｍ以下のときには分散度βが９５％以上、
３００μｍを越え８００μｍ以下のときには分散度βが９７％以上、
８００μｍを越えるときには分散度βが９９％以上、
の分散状態で、被覆空間の被覆開始領域において被覆形成物質前駆体と接触及び／又は衝突させて被覆を開始する被覆工程、
を設けた被覆法。
【００９９】
II
（Ａ） 体積基準頻度分布で平均粒子径が１０μｍを越え２０μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが８０％以上を実現する準微粒子高分散処理手段群、
体積基準頻度分布で平均粒子径が２０μｍを越え５０μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９０％以上を実現する準微粒子高分散処理手段群、
体積基準頻度分布で平均粒子径が５０μｍを越え３００μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９５％以上を実現する準微粒子高分散処理手段群、
体積基準頻度分布で平均粒子径が３００μｍを越え８００μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９７％以上を実現する準微粒子高分散処理手段群、
体積基準頻度分布で平均粒子径が８００μｍを越える準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９９％以上を実現する準微粒子高分散処理手段群、
により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とする分散工程、
（Ｂ） この分散工程で分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子を、
その平均粒子径が１０μｍを越え２０μｍ以下のときには分散度βが８０％以上、
２０μｍを越え５０μｍ以下のときには分散度βが９０％以上、
５０μｍを越え３００μｍ以下のときには分散度βが９５％以上、
３００μｍを越え８００μｍ以下のときには分散度βが９７％以上、
８００μｍを越えるときには分散度βが９９％以上、
の分散状態で、被覆空間の被覆開始領域において被覆形成物質前駆体と接触及び／又は衝突させて被覆を開始する被覆工程、
を設けた被覆法。
【０１００】
III
（Ａ） 体積基準頻度分布で平均粒子径が１０μｍを越え２０μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが８０％以上を実現する準微粒子高分散処理手段群、
体積基準頻度分布で平均粒子径が２０μｍを越え５０μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９０％以上を実現する準微粒子高分散処理手段群、
体積基準頻度分布で平均粒子径が５０μｍを越え３００μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９５％以上を実現する準微粒子高分散処理手段群、
体積基準頻度分布で平均粒子径が３００μｍを越え８００μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９７％以上を実現する準微粒子高分散処理手段群、
体積基準頻度分布で平均粒子径が８００μｍを越える準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９９％以上を実現する準微粒子高分散処理手段群、
により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とする分散工程、
（Ｂ） この分散工程で分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子を、被覆工程に直接搬送する搬送工程、
（Ｃ） この搬送工程で搬送した高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子を、
その平均粒子径が１０μｍを越え２０μｍ以下のときには分散度βが８０％以上、
２０μｍを越え５０μｍ以下のときには分散度βが９０％以上、
５０μｍを越え３００μｍ以下のときには分散度βが９５％以上、
３００μｍを越え８００μｍ以下のときには分散度βが９７％以上、
８００μｍを越えるときには分散度βが９９％以上、
の分散状態で、被覆空間の被覆開始領域において被覆形成物質前駆体と接触及び／又は衝突させて被覆を開始する被覆工程、
を設けた被覆法。
【０１０１】
IV
（Ａ） 体積基準頻度分布で平均粒子径が１０μｍを越え２０μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが８０％以上を実現する準微粒子高分散処理手段群、
体積基準頻度分布で平均粒子径が２０μｍを越え５０μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９０％以上を実現する準微粒子高分散処理手段群、
体積基準頻度分布で平均粒子径が５０μｍを越え３００μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９５％以上を実現する準微粒子高分散処理手段群、
体積基準頻度分布で平均粒子径が３００μｍを越え８００μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９７％以上を実現する準微粒子高分散処理手段群、
体積基準頻度分布で平均粒子径が８００μｍを越える準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９９％以上を実現する準微粒子高分散処理手段群、
により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とする分散工程、
（Ｂ） この分散工程で分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子を、搬送に不可避の、中空部材、中空を形成する部材からなる中間部材、及びパイプから選択される１種類又はそれ以上の部材を介して搬送する搬送工程、
（Ｃ） この搬送工程で搬送した高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子を、
その平均粒子径が１０μｍを越え２０μｍ以下のときには分散度βが８０％以上、
２０μｍを越え５０μｍ以下のときには分散度βが９０％以上、
５０μｍを越え３００μｍ以下のときには分散度βが９５％以上、
３００μｍを越え８００μｍ以下のときには分散度βが９７％以上、
８００μｍを越えるときには分散度βが９９％以上、
の分散状態で、被覆空間の被覆開始領域において被覆形成物質前駆体と接触及び／又は衝突させて被覆を開始する被覆工程、
を設けた被覆法。
【０１０２】
Ｖ
（Ａ） 体積基準頻度分布で平均粒子径が１０μｍを越え２０μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが８０％以上を実現する準微粒子高分散処理手段群、
体積基準頻度分布で平均粒子径が２０μｍを越え５０μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９０％以上を実現する準微粒子高分散処理手段群、
体積基準頻度分布で平均粒子径が５０μｍを越え３００μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９５％以上を実現する準微粒子高分散処理手段群、
体積基準頻度分布で平均粒子径が３００μｍを越え８００μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９７％以上を実現する準微粒子高分散処理手段群、
体積基準頻度分布で平均粒子径が８００μｍを越える準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９９％以上を実現する準微粒子高分散処理手段群、
により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とする分散工程、
（Ｂ） この分散工程で分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子を、この分散性能で気中に分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の気中分散状態を維持する気中分散維持手段、この高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の気中分散状態を高める気中分散促進手段、芯粒子粉体の粒子と気体との混合物において低分散芯粒子粉体の粒子・気体混合物を分離し、芯粒子粉体の粒子が主に単一粒子状態で気中に存在する高分散芯粒子粉体の粒子・気体混合物を選択する高分散芯粒子粉体の粒子・気体混合物選択手段の１種類又はそれ以上を介して搬送する搬送工程、
（Ｃ） この搬送工程で搬送した高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子を、
その平均粒子径が１０μｍを越え２０μｍ以下のときには分散度βが８０％以上、
２０μｍを越え５０μｍ以下のときには分散度βが９０％以上、
５０μｍを越え３００μｍ以下のときには分散度βが９５％以上、
３００μｍを越え８００μｍ以下のときには分散度βが９７％以上、
８００μｍを越えるときには分散度βが９９％以上、
の分散状態で、被覆空間の被覆開始領域において被覆形成物質前駆体と接触及び／又は衝突させて被覆を開始する被覆工程、
を設けた被覆法。
【０１０３】
以上、１〜Ｖの全てにおいて、好適には、体積基準頻度分布で平均粒子径が１０μｍを越え２０μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが８０％以上を実現する空間領域、
体積基準頻度分布で平均粒子径が２０μｍを越え５０μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９０％以上を実現する空間領域、
体積基準頻度分布で平均粒子径が５０μｍを越え３００μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９５％以上を実現する空間領域、
体積基準頻度分布で平均粒子径が３００μｍを越え８００μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９７％以上を実現する空間領域、
体積基準頻度分布で平均粒子径が８００μｍを越える準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９９％以上を実現する空間領域の内の高分散芯粒子粉体の粒子・気体混合物中の芯粒子粉体の粒子の全ての粒子が通過する面を含む空間領域に、被覆空間の被覆開始領域を位置させるか、又は、
体積基準頻度分布で平均粒子径が１０μｍを越え２０μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが８０％以上を実現する空間領域、
体積基準頻度分布で平均粒子径が２０μｍを越え５０μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９０％以上を実現する空間領域、
体積基準頻度分布で平均粒子径が５０μｍを越え３００μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９５％以上を実現する空間領域、
体積基準頻度分布で平均粒子径が３００μｍを越え８００μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９７％以上を実現する空間領域、
体積基準頻度分布で平均粒子径が８００μｍを越える準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９９％以上を実現する空間領域
の内の回収手段の回収部に回収する全てに粒子が通過する面を含む空間領域に、被覆空間の被覆開始領域を位置させて行うものである。
【０１０４】
又は、前記Ｉ及びIIにおいて、好適には、
体積基準頻度分布で平均粒子径が１０μｍを越え２０μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが８０％以上を実現する準微粒子高分散処理手段群、
体積基準頻度分布で平均粒子径が２０μｍを越え５０μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９０％以上を実現する準微粒子高分散処理手段群、
体積基準頻度分布で平均粒子径が５０μｍを越え３００μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９５％以上を実現する準微粒子高分散処理手段群、
体積基準頻度分布で平均粒子径が３００μｍを越え８００μｍ以下の準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９７％以上を実現する準微粒子高分散処理手段群、
体積基準頻度分布で平均粒子径が８００μｍを越える準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子を、準微粒子高分散処理手段群により分散させた高分散芯粒子粉体の粒子・気体混合物の芯粒子粉体の粒子の分散度βが９９％以上を実現する準微粒子高分散処理手段群、
により気中に分散させて高分散芯粒子粉体の粒子・気体混合物とする分散工程の一部以上と前記被覆工程の一部以上とを、空間を一部以上共有して行うものである。
【０１０５】
次いで本発明を実施例によって更に詳細に説明することにする。
【０１０６】
実施例１
以下、図５(ａ)に示した構成の装置の具体例としての図６およびその部分拡大図である図７に示した本発明の実施例に基づいて詳細に説明する。
【０１０７】
本例の装置は、プラズマトーチ３−Ａ、プラズマ室３−ａ、被覆形成物質前駆体生成室の冷却槽３−Ｂ、被覆形成物質前駆体生成室３−ｂ、狭義の被覆室冷却槽３−Ｃ、狭義の被覆室３−ｃ、被覆準微粒子冷却室の冷却槽３−Ｄ、被覆準微粒子冷却室３−ｄ、被覆形成物質の原料の供給側に、供給装置３−Ｅ１、芯粒子粉体の供給側に、撹拌式分散機３−Ｆ１とエジェクター式分散機３−Ｈ１、細管分散機１０７及び被覆準微粒子回収部３−Ｇより成る。供給装置３−Ｅ１は被覆形成物質の原料粉体の供給槽１１２に、撹拌式分散機３−Ｆ１は芯粒子粉体の供給槽を備えた供給機１１１にそれぞれ結合される。本例における被覆室は、定義ではプラズマ室３−ａ、被覆形成物質前駆体生成室３−ｂ、狭義の被覆室３−ｃ、被覆準微粒子冷却室３−ｄから構成されており、ここではこれらを広義の被覆室と称する。広義の被覆室の内、主に被覆処理の行われる室３−ｃを狭義の被覆室と称する。
【０１０８】
本準微粒子高分散処理手段群αは、供給槽を備えた供給機１１１、撹拌式分散機３−Ｆ１とエジェクター式分散機３−Ｈ１及び内径４mmのステンレス製細管分散機１０７で構成されており、図２(ａ)の準微粒子高分散処理手段群の構成である。準微粒子高分散処理手段群は、ＤM＝４０μｍの（〔ＤM／５，５ＤM〕，≧９０％）の粉体に対して出力時β≧９０％を実現できるように構成されている。準微粒子高分散処理手段群の最終処理手段である細管１０７は被覆室３−Ｃに直結してあり、被覆空間の３−Ｌ２の被覆開始領域３−Ｌ１においてＤM＝４０μｍの（〔ＤM／５，５ＤM〕，≧９０％）の粉体に対しβ≧９０％を実現できるように構成されている。
【０１０９】
プラズマトーチ３−Ａは、例えば、内径４４mm、長さ２００mmの石英管を主体とし、外側に高周波発振用のコイルが取り付けられ、その外側には冷却用の外套管が設けられている。プラズマトーチ３−Ａの上部には噴出方向が接線方向、軸方向及び半径方向のガス噴出口１０１が設けられている。
プラズマトーチ３−Ａの下部は被覆形成物質の原料の供給口１０４が設けられ、被覆形成物質の原料の供給槽を備えた供給機１１２から供給される被覆形成物質の原料の粉体がキャリアガス１０３に担持されてプラズマ焔中に導入される構成である。
【０１１０】
被覆形成物質前駆体生成室３−ｂは、内径１２０mm、長さ２００mmの石英管と、その外側の冷却用外套管３−Ｂとから成る。
狭義の被覆室３−ｃは、内径１２０mm、長さ１００mmの内管とその外側の冷却用の外套管３−Ｃとから成る。狭義の被覆室３−ｃは、芯粒子粉体の供給槽を備えた供給機１１１から供給される芯粒子が、撹拌式分散機３−Ｆ１、エジェクター式分散機３−Ｈ１及び細管分散機１０７からなる準微粒子高分散処理手段群αにより分散させて、狭義の被覆室３−ｃの中央部に設けられた芯粒子粉体の供給口から導入される構成である。被覆空間３−Ｌ２及び被覆空間の被覆開始領域は、狭義の被覆室３−ｃ内に設けてある。
被覆準微粒子冷却室３−ｄは、内径４４０mm、長さ８００mmの管１１６とその外側の冷却用の外套管３−Ｄとから成る。
被覆準微粒子の回収部３−Ｇの出口部１０９は、真空ポンプに連結され、被覆準微粒子がフィルター１１０上に集められ取り出される構成である。
【０１１１】
本発明の、実施例の被覆準微粒子の製造装置により、芯粒子粉体の粒子として、ＤM＝４０μｍで（〔ＤM／５，５ＤM〕，≧９０％）分布のダイヤモンドの準微粒子粉体の粒子に、被覆形成物質として酸化けい素を被覆した。
プラズマトーチ３−Ａの上部に設けられたガス噴出口１０１に供給源１０２からアルゴンガスを２０リットル／分の割合で供給する。このアルゴンガスは印加された高周波によってプラズマ化され、プラズマトーチ３−Ａ内プラズマ室３−ａでプラズマ焔を形成する。
【０１１２】
被覆形成物質の原料の供給槽を備えた供給機１１２から供給した被覆形成物質の原料である酸化けい素粉末は、５リットル／分のキャリアガス１０３に担持されて、プラズマトーチ３−Ａの下部に設けられた被覆形成物質の原料の投入口１０４から、プラズマ焔中に０.５ｇ／分の割合で導入され、プラズマ焔の熱により蒸発し、被覆形成物質前駆体生成室３−ｂで急冷、凝縮して被覆形成物質前駆体となる。
【０１１３】
芯粒子粉体の供給槽を備えた供給機１１１から１.５ｇ／分で供給されるダイヤモンドの芯粒子は、撹拌式分散機３−Ｆ１により分散せしめ、５リットル／分の割合で供給されるキャリアガス１０５により担持され、１０リットル／分の流量の分散ガス１０６によるエジェクター式分散機３−Ｈ１及び細管分散機１０７により気中に分散させる。
【０１１４】
本実施例の供給槽を備えた供給機１１１、撹拌式分散機３−Ｆ１とエジェクター式分散機３−Ｈ１及び細管分散機１０７で構成される準微粒子高分散処理手段群αは、体積基準の頻度分布として、ＤM＝４０μｍの（〔ＤM／５，５ＤM〕，≧９０％）分布の芯粒子粉体の粒子を、最終処理手段である細管分散機１０７で、分散度β＝９４％に分散できる。又、被覆空間の被覆開始領域３−Ｌ１で、分散度β＝９４％の分散状態で被覆が始められる。
【０１１５】
このようにして生成した、被覆形成物質で表面が被覆された被覆準微粒子は、気体と共に被覆準微粒子冷却室３−ｄを降下し、被覆準微粒子回収部３−Ｇに至る。この被覆準微粒子からなる製品は、フィルター１１０により気体と分離し、集められ取り出される。
【０１１６】
得られた被覆準微粒子である、酸化けい素で表面を被覆したダイヤモンド準微粒子を走査型電子顕微鏡で観察したところ、図８に示す通り、一次粒子である個々のダイヤモンド準微粒子に酸化けい素が超微粒子状に被覆したものであった。
【０１１７】
比較例
分散手段を設けず、準微粒子粉体を供給機１１１から直接被覆室３−ｃに導入するようにした点を除いて本実施例で用いた装置とは同一の構成の装置を用い、本実施例で用いたものと全く同じダイヤモンド準微粒子粉体を、被覆形成物質の酸化けい素で被覆した。被覆室への投入口におけるダイヤモンド準微粒子の分散度βは７５％であった。得られた被覆粒子である、酸化けい素で表面を被覆したダイヤモンド準微粒子を走査型電子顕微鏡で観察したところ、図９に示すとおり部分的に酸化けい素が被覆していない酸化けい素被覆ダイヤモンド準微粒子しか得られなかった。
【０１１８】
実施例２
図１０およびその部分拡大図である図１１に示した装置は、図５(ｄ)に示した構成の装置の１つの具体例である。
【０１１９】
本例の被覆形成物質前駆体を生成せしめる装置の構成は実施例１と同一である。準微粒子高分散処理手段群αは、供給槽を備えた供給機２１４、撹拌式分散機５−Ｆ１、細管分散機２１１及び衝突板を利用した分散機５−Ｈ２で構成されており、図２(ａ)の準微粒子高分散処理手段群の構成の一例である。細管分散機２１１は、内径４mmのステンレス製である。準微粒子高分散処理手段群αの最終分散手段である衝突板を利用した分散機５−Ｈ２は、ＳｉＣ製の衝突板２１３がステンレス製のホルダー２１２により設置された構成である。この衝突板を利用した分散機５−Ｈ２は狭義の被覆室５−ｃの中に設けられており、準微粒子高分散処理手段群αと狭義の被覆室５−ｃは共有の空間を有している。また、被覆空間５−Ｌ１及び被覆空間の被覆開始領域５−Ｌ２は、狭義の被覆室５−ｃ内に設けてある。本装置の準微粒子高分散処理手段群によれば、体積基準頻度分布として、ＤM＝２００μｍの（〔ＤM／５，５ＤM〕，≧９０％）分布に相当する芯粒子粉体の粒子を、最終の分散処理である衝突板を利用した分散機５−Ｈ２の衝突板２１５を衝突直後、分散度β≧９５％に分散できる。したがって、分散度β≧９５％の状態で被覆が開始される。
【０１２０】
本例の被覆準微粒子の製造装置により、芯粒子粉体の粒子として、体積基準の平均粒子径ＤM＝２００μｍで（〔ＤM／５，５ＤM〕，≧９０％）分布の酸化アルミニウムの準微粒子粉体の粒子に、被覆形成物質として金属アルミニウムを被覆した。
プラズマトーチ５−Ａの上部に設けられたガス噴出口２０１に供給源２０２から２０リットル／分のアルゴンガスを供給する。このアルゴンガスは印加された高周波によってプラズマ化され、プラズマトーチ５−Ａ内プラズマ室５−ａでプラズマ焔を形成する。
【０１２１】
被覆形成物質の原料の供給槽を備えた供給機２１５から０.５ｇ／分で供給した被覆形成物質の原料である金属アルミニウム粉末は、５リットル／分のキャリアガス２０３に担持されて、プラズマトーチ５−Ａの下部に設けられた被覆形成物質の原料の投入口２０４から、プラズマ焔中に導入され、プラズマ焔の熱により蒸発し、被覆形成物質前駆体生成室５−ｂで急冷、凝縮して被覆形成物質前駆体となる。
【０１２２】
芯粒子粉体の供給槽を備えた供給機２１４から２.０ｇ／分で供給される酸化アルミニウムの芯粒子は、撹拌式分散機５−Ｆ１により分散せしめ、２０リットル／分の割合で供給されるキャリアガス２０５により担持され、細管分散機２１１を経て衝突板を利用した分散機５−Ｈ２によって、分散度β＝９７％に気中に分散せしめる。被覆室の中で分散せしめた芯粒子を、被覆空間５−Ｌ２の被覆開始領域５−Ｌ１で分散度β＝９７％の分散状態で被覆し始める。
このようにして生成した、被覆形成物質で表面が被覆された被覆準微粒子は、気体と共に被覆準微粒子冷却室５−ｄを降下し、被覆準微粒子回収部５−Ｇに至る。この被覆準微粒子からなる製品は、フィルター２１０により気体と分離し、集められ取り出される。
【０１２３】
得られた被覆準微粒子である、金属アルミニウムで表面を被覆した酸化アルミニウム準微粒子は、走査型電子顕微鏡で観察したところ、一次粒子である個々の酸化アルミニウム準微粒子に金属アルミニウムが被覆したものである。被覆形態は実施例１で得たものと同様であった。
【０１２４】
実施例３
図１２およびその部分拡大図である図１３に示した装置は、図５(ｂ)に示した構成の装置の１つの具体例である。
【０１２５】
本例の被覆形成物質前駆体を生成せしめる装置の構成は、実施例１と同一である。準微粒子高分散処理手段群αは、供給槽を備えた供給機３１３、分散手段である撹拌式分散機６−Ｆ１、高分散芯粒子粉体の粒子・気体混合物選択手段であるサイクロン６−Ｉで構成されており、図２(ｂ)のブロック図の構成の一例である。サイクロン６−Ｉの高分散芯粒子粉体の粒子・気体混合物の放出部は、搬送に不可避のパイプ３０７で狭義の被覆室６−ｃへ接続してあり、低分散芯粒子粉体の粒子・気体混合物の放出部は、ホッパー６−Ｊ、ロータリーバルブ６−Ｋを介して搬送管３１０で撹拌式分散機６−Ｆ１へ接続してある。本装置の準微粒子高分散処理手段群によれば、体積基準の粒度分布として、ＤM＝１５μｍの（〔ＤM／５，５ＤM〕，≧９０％）分布に相当する芯粒子粉体の粒子を、最終の処理手段であるサイクロン６−Ｉの高分散芯粒子粉体流の放出部で、分散度β≧９０％に分散できる。狭義の被覆室６−ｃに図のごとく被覆空間６−Ｌ２及び被覆空間の被覆開始領域６−Ｌ１が設けてある。６−Ｃと６−Ｄを結合するフランジ部の制約による不可避のパイプ３０７による分散度βの低下は少なくとどめられる。したがって、被覆開始領域において、分散度β≧８０％で被覆が開始される。
【０１２６】
本例の被覆準微粒子の製造装置により、芯粒子粉体の粒子として、ＤM＝１５μｍの（〔ＤM／５，５ＤM〕，≧９０％）分布の立方晶窒化硼素の準微粒子粉体の粒子に、被覆形成物質として金属アルミニウムを被覆した。
プラズマトーチ６−Ａの上部に設けられたガス噴出口３０１に供給源３０２からアルゴンガスを２０リットル／分で供給する。このアルゴンガスは印加された高周波によってプラズマ化され、プラズマトーチ６−Ａ内プラズマ室６−ａでプラズマ焔を形成する。
【０１２７】
被覆形成物質の原料の供給槽を備えた供給機３１４から０.５ｇ／分で供給した被覆形成物質の原料である金属アルミニウム粉末は、５リットル／分のキャリアガス３０３に担持されて、プラズマトーチ６−Ａの下部に設けられた被覆形成物質の原料の投入口３０４から、プラズマ焔中に導入され、プラズマ焔の熱により蒸発し、被覆形成物質前駆体生成室６−ｂで急冷、凝縮して被覆形成物質前駆体となる。
【０１２８】
芯粒子粉体の供給槽を備えた供給機３１３から１.７ｇ／分で供給される立方晶窒化硼素の芯粒子は、撹拌式分散機６−Ｆ１により分散させ、１５リットル／分のキャリアガス３０５により担持されパイプ３０６を介してサイクロン６−Ｉに搬送される。サイクロン６−Ｉは、微粉側の最大粒子径が２０μｍとなるように調節されており、単一粒子を主に含む高分散芯粒子粉体の粒子・気体混合物は、搬送に不可避のパイプ３０７を介し放出口３０８から狭義の被覆室６−ｃに放出させる。一方、サイクロン６−Ｉにより選択分離した主に凝集粒子からなる低分散芯粒子粉体の粒子・気体混合物分散芯粒子粉体流は、ホッパー６−Ｊ、ロータリーバルブ６−Ｋを経て、１０リットル／分のキャリアガス３０９によりパイプ３１０中を搬送され、撹拌式分散機６−Ｆ１へフィードバックせしめる。準微粒子高分散処理手段群αからの放出部であるサイクロン６−Ｉの高分散芯粒子粉体の粒子・気体混合物の放出部での分散度は分散度β＝９０％であり、被覆空間の被覆開始領域６−Ｌ１での分散度は、β＝８５％である。
このようにして生成した、被覆形成物質で表面が被覆された被覆準微粒子は、気体と共に被覆準微粒子冷却室６−ｄを降下し、被覆準微粒子回収部６−Ｇに至る。この被覆準微粒子からなる製品は、フィルター３１２により気体と分離し、集められ取り出される。
【０１２９】
得られた被覆準微粒子である、金属アルミニウムで表面を被覆した立方晶窒化硼素準微粒子は、走査型電子顕微鏡で観察したところ、一次粒子である個々の立方晶窒化硼素準微粒子に金属アルミニウムが被覆したものである。被覆形態は実施例１と同様であった。
【０１３０】
【発明の効果】
本発明の、被覆準微粒子の製造方法および装置によって、準微粒子芯粒子粉体の粒子又は主に準微粒子からなる芯粒子粉体の粒子であっても個々の粒子に被覆形成物質を被覆可能となり、凝集体の表面を被覆形成物質で被覆した被覆凝集体を生成することによる未被覆の粒子や未被覆を持つ粒子を生成することが無くなった。これにより、未被覆の芯粒子或いは未被覆部分を有する芯粒子が存在しなくなり工業生産上のメリットは、頗る大きい。
【図面の簡単な説明】
【図１】粉体粒子の分布図であり、(ａ)は本来の分散度βを表わし、(ｂ)は粒径Ｄ1〜Ｄ2の範囲の粒子が体積で９０％を占める粉体の粒径対体積基準頻度を表わす。
【図２】(ａ)〜(ｃ)は準微粒子高分散処理手段群の基本構成を示すブロック図。
【図３】(ａ)〜(ｇ)は準微粒子高分散処理手段群の構成をより詳細に説明するブロック図。
【図４】(ａ)〜(ｅ)は芯粒子粉体に被覆が開始される態様を示す図。
【図５】(ａ)〜(ｇ)は本発明の装置の構成を説明するブロック図。
【図６】実施例１の装置を示す図。
【図７】実施例１の装置の部分拡大図。
【図８】実施例１の装置で得られた被覆準微粒子の走査型電子顕微鏡写真。
【図９】比較例で得られた被覆準微粒子の走査型電子顕微鏡写真。
【図１０】実施例２の装置を示す図。
【図１１】実施例２の装置の部分拡大図。
【図１２】実施例３の装置を示す図。
【図１３】実施例３の装置の部分拡大図。[0001]
[Industrial applications]
The present invention relates to a method for producing coated quasi-fine particles and an apparatus therefor. More specifically, the present invention relates to a method for producing coated quasi-fine particles in which particles of quasi-fine particle core particle powder or particles of core particle powder mainly composed of quasi-fine particles are coated with a coating forming substance, and an apparatus therefor.
[0002]
[Prior art]
The method of coating the surface of a powder particle with a coating material such as an inorganic material or a metal material in various forms such as a film by a vapor phase method is, in principle, (1) easy to control the atmosphere. (2) There is basically no limitation on the selection of the coating forming material, and various kinds of materials such as an active metal and other simple metal materials, alloys, nitrides, carbides, borides, oxides, etc. are powder particles. There are great features that cannot be achieved by other coating methods, such as being able to coat the surface, (3) being able to coat a high-purity substance, and (4) being able to arbitrarily control the coating amount of the coating-forming substance.
[0003]
Then, highly controlled uniform coating of particles of the core particle powder of quasi-fine particles having a particle diameter exceeding 10 μm or particles of the core particle powder mainly composed of quasi-fine particles, ie, individual There is a demand for a uniform coating in which the uncoated portion does not remain over a large area of the surface of the particles, and in which the uniform coating is formed without leakage of all the particles. In addition, as for this highly controlled uniform coating, for those having a large particle size, a uniform coating with less uncoated portions is required.
[0004]
However, the highly controlled and uniform coating has not yet been achieved with various coating apparatuses and coating methods proposed as known techniques.
[0005]
For example, according to the apparatus and method disclosed in Japanese Patent Application Laid-Open No. 58-31076, core particles are placed in a container installed in a PVD apparatus, and the container is vibrated by an electromagnetic method. Then, the core particles in the container are rolled and coated by the PVD method. According to the apparatus disclosed in Japanese Patent Application Laid-Open No. 61-30663, particles of core particle powder are put in a container installed in a PVD apparatus, and the container is vibrated by a mechanical method. It is stated that the core particles in the container can be coated by a PVD method while rolling. However, in the apparatus or the method of coating while rolling the particles of the core particle powder by the vibration of these containers, in practice, the particles of the quasi-fine particle core particles or the core particle powder mainly composed of the quasi-fine particles are used. The particles could only be slid in multiple layers and could not be coated in a single particle state.
[0006]
The apparatus and method disclosed in Japanese Patent Application Laid-Open No. 3-153864 discloses a method in which particles are placed in a rotating container having a barrier and / or unevenness on the inner surface, and the surface of the core particles is coated by vapor deposition while rotating the rotating container. In such an apparatus or method, in such an apparatus or method, the particles of the quasi-fine particle core particle powder or the particles of the core particle powder mainly composed of the quasi-fine particle are superposed in many layers. Many particles were only agitated lightly in contact and could not be coated in a single particle state.
[0007]
Japanese Patent Application Laid-Open No. 58-141375 discloses that a powder placed in a reaction gas atmosphere is suspended by the flow of the reaction gas and the action of gravity, and the powder is deposited by a precipitate formed by a chemical reaction of the reaction gas. An apparatus for coating the surface of a surface is disclosed. In addition, Japanese Patent Application Laid-Open No. 2-43377 discloses a method of performing coating by performing a thermochemical reaction treatment while fluidizing particles under reduced pressure. Also, Japanese Patent Application Laid-Open No. 64-80437 discloses a method in which agglomerates of core particle powders are broken down and fluidized by low- and high-frequency synthetic sound waves to coat them. However, in the method or the apparatus using the fluidized bed of the particles of the quasi-fine particle core particles or the particles of the core particle powder mainly composed of the quasi-fine particles by these air currents and vibrations, all the core particles are similarly converted into a single particle. It was practically impossible to flow and float independently in this state, and it was not possible to eliminate the uneven coating of each particle, which could be caused by the particles being shaded.
[0008]
Japanese Patent Application Laid-Open No. 54-153789 discloses an apparatus for coating a metal by dropping a powder material in a vacuum vessel in which metal vapor is generated. Japanese Patent Application Laid-Open No. 60-47004 discloses a method in which a monomer gas and powder particles are introduced into a high-frequency plasma region in a vacuum chamber and an organic coating film is formed by plasma polymerization. As in these apparatuses or methods, the particles of the quasi-fine particle core particle powder or the particles of the core particle powder mainly composed of quasi-fine particles simply fall and form an aggregate that is not a single particle state. In addition, the particles were shaded, resulting in uneven coating, the particles inside the aggregate were not coated at all, or the coating amount was different from that coated with a single particle.
[0009]
Japanese Patent Application Laid-Open No. 62-250172 discloses that, as a pretreatment, a powder subjected to jet mill treatment is retained in a reduced pressure heat treatment chamber, and then subjected to heat treatment, and then spontaneously falls into a sputtering chamber with a powder feeder. An apparatus and a method for introducing and spontaneously dropping and coating a target in a vertically arranged cylindrical sputtering chamber are disclosed. Japanese Patent Application Laid-Open No. Hei 2-153068 discloses that, as a pretreatment, a powder subjected to jet mill treatment is retained in a reduced pressure heat treatment chamber, subjected to heat treatment, and then subjected to a sputtering source in a sputtering chamber by a powder feeder. An apparatus and a method are disclosed in which a powder (not a single particle) is introduced into a rotatable container in which the powder is introduced, and sputtering is performed while the container is rotated. In these apparatuses and methods, in the heating step before coating, there is a step of retaining the core particles powder jet-milled, due to the retention of this powder in the heating step to form an aggregate that is not a single particle state again After all, in the coating step, this aggregate does not become a single particle state.
[0010]
As described above, in the conventionally known technology, any problem has not been solved as an apparatus or a method for coating the particles of the quasi-fine particle core particles or the particles of the core particle powder mainly composed of the quasi-fine particles, The particles of the core particle powder of the quasi-fine particles or the particles of the core particle powder mainly composed of the quasi-fine particles are actually subjected to the coating treatment in an agglomerate state while in contact with each other, and therefore, a high degree of There was no controlled uniform coating. That is, there has been no method for producing coated quasi-fine particles capable of providing a highly controlled and uniform coating, and no production apparatus therefor. As a result, the above problem could not be effectively solved.
[0011]
[Problems to be solved by the invention]
Therefore, in practice, for example, highly controlled uniform coating on the particles of the core particle powder of the quasi-fine particles whose quasi-fine particles exceed 10 μm or the particles of the core particle powder mainly consisting of the quasi-fine particles, that is, There is a need for a uniform coating that leaves no uncoated portions over a large area of the surface of the individual particles, and that this uniform coating is leak-free to all particles. Moreover, for those having a large particle diameter, there is a strong demand for a method for producing coated quasi-fine particles capable of uniform coating with less uncoated portions and an apparatus therefor.
[0012]
The present invention provides a highly controlled and uniform coating of the particles of the quasi-fine particle core powder or the particles of the core particle powder consisting mainly of quasi-fine particles, i.e. the uncoated part over a large area of the surface of the individual particles. A uniform coating with no residue, and a coating in which this uniform coating is formed without leakage of all the particles, and a coating having a large particle diameter can provide a uniform coating with less uncoated portions. An object of the present invention is to provide a method for producing quasi-fine particles and an apparatus therefor.
[0013]
[Means for Solving the Problems]
In order to solve the above-described problems, the present inventors have conducted intensive studies and found that the particles of the quasi-fine particle core particles or the particles of the core particle powder mainly composed of quasi-fine particles are highly controlled and uniform. Coating, i.e., a uniform coating in which no uncoated portions remain over a large area of the surface of the individual particles, and a coating in which a uniform coating is formed on all particles without leakage, and having a large particle size In order to form a uniform coating with less uncoated portions, (1) the core particle powder having an average particle size exceeding 10 μm and 20 μm or less in a volume-based frequency distribution is mainly in a single particle state. The particles of the high-dispersion core particles in the air and the particles of the core particles in the gas mixture are dispersed in the coating start region of the coating space in a highly dispersed state in which the degree of dispersion β is 80% or more, or (2) Volume-based frequency distribution with an average particle size of 20μ And the particles of the core particle powder in the gas mixture and the particles of the core particle powder in the gas mixture in which the particles of the core particle powder having a particle diameter of In the coating start region of the coating space in a highly dispersed state of 90% or more, or (3) core particles having an average particle size of more than 50 μm and 300 μm or less in a volume-based frequency distribution are mainly single particles. The particles of the high-dispersion core particles and the particles of the core particles in the gas mixture that are present in the air in the air in the air are dispersed in the coating start region of the coating space in the high dispersion state where the degree of dispersion β is 95% or more, Or (4) a particle / gas mixture of highly dispersed core particle powder in which the particles of the core particle powder having an average particle diameter of more than 300 μm and 800 μm or less in the volume-based frequency distribution are mainly present in the air in a single particle state. The particles of the core particle powder in the dispersion in a highly dispersed state in which the degree of dispersion β is 97% or more. In the coating start region of the space or (5) the core particle powder having an average particle diameter exceeding 800 μm in the volume-based frequency distribution is present in the air mainly in a single particle state. It has been found that the coating of the particles of the core particle powder in the particle / gas mixture must be started in the coating start region of the coating space in a highly dispersed state where the degree of dispersion β is 99% or more.
[0014]
More specifically, (I) the particles of the core particle powder in the state of the particles / gas mixture of the highly dispersed core particle powder in which the particles of the core particle powder are mainly present in the air in a single particle state are allowed to stay. At least, there is a tendency to re-agglomerate mainly due to turbulent agglomeration etc. with the passage of time, and once re-agglomerated, it must be dispersed by a dispersion treatment means having particularly high dispersion performance like the aggregate before the dispersion treatment. It is difficult to disintegrate this re-agglomeration state to highly disperse, that is, to re-disperse into a single particle state of each unit. Therefore, (1) the average particle diameter exceeds 10 μm in the volume-based frequency distribution. The particles of the core particles having a particle diameter of 20 μm or less are mainly present in the air in a single particle state. In a highly dispersed state as described above, or (2) the volume-based frequency The average particle diameter exceeds 20 μm and the particles of the core particle powder having a particle diameter of 50 μm or less are mainly present in the air in a single particle state. In a highly dispersed state in which the degree of dispersion β is 90% or more, or (3) the core particle powder having an average particle diameter of more than 50 μm and 300 μm or less in a volume-based frequency distribution is mainly in a single particle state. The particles of the high-dispersion core particles in the air and the particles of the core particles in the gas mixture are dispersed in a highly dispersed state having a degree of dispersion β of 95% or more, or (4) volume-based frequency distribution The average particle diameter exceeds 300 μm, and the particles of the core particle powder in the gas mixture, in which the particles of the core particle powder in which the particles of the core particle powder having a particle diameter of 800 μm or less are mainly present in the air in a single particle state. In the covering start area of the covering space in a highly dispersed state where the degree of dispersion β is 97% or more, (5) Core particles in a gas-gas mixture of highly dispersed core particles in which particles of core particles having an average particle diameter exceeding 800 μm in a volume-based frequency distribution are mainly present in the air in a single particle state. It is necessary to guide the particles of the powder to the coating start region of the coating space in a high dispersion state in which the degree of dispersion β is 99% or more. The inventors have found that a group of dispersion processing means having at least one or more particularly high dispersibility, which breaks down and disperses in the air with a very high degree of dispersion according to the particle size, is required, and has led to the present invention.
[0015]
That is, according to the present invention, the core particle powder is charged into the coating space, and the coating forming substance precursor generated via the gas phase and / or the coating forming substance precursor in the gas phase are brought into contact with the particles of the core particle powder. And / or in the apparatus for producing coated quasi-fine particles, wherein the surface of the particles of the core particle powder is coated with a coating-forming substance by collision.
(A) The final processing means of the quasi-fine particle high dispersion processing means group is
(A) dispersing means for dispersing the particles of the core particle powder in the air; and
(B) separating the low-dispersion core particle powder portion in a mixture of the core particle powder and the gas in which the core particle powder is dispersed in the air; Highly dispersed core particle powder particles / gas mixture selecting means for selecting particles / gas mixture of highly dispersed core particle powder present in the air in a state and particles / gas mixture selecting means of this highly dispersed core particle powder A high-dispersion core provided with a feedback means for conveying the separated low-dispersion core particle powder portion to a final dispersing means and / or a processing means prior to the final dispersing means among the dispersing means in the quasi-fine particle high dispersion processing means group; Means for selecting a particle / gas mixture of the particle powder,
By means of a group of quasi-fine particle high dispersion treatment means selected from, the particles of the quasi-fine particle core particle powder having an average particle diameter exceeding 10 μm in the volume-based frequency distribution or the particles of the core particle powder mainly consisting of the quasi-fine particles are airborne. A dispersing step of dispersing into a particle / gas mixture of highly dispersed core particle powder,
(B) The particles of the core particle powder dispersed in this dispersion step are
When the average particle diameter is more than 10 μm and 20 μm or less, the degree of dispersion β is 80% or more,
When it exceeds 20 μm and is 50 μm or less, the degree of dispersion β is 90% or more,
When it exceeds 50 μm and is 300 μm or less, the degree of dispersion β is 95% or more,
When it exceeds 300 μm and is 800 μm or less, the degree of dispersion β is 97% or more, and
When it exceeds 800 μm, the degree of dispersion β is 99% or more.
In a dispersed state of, a coating step of starting coating by contacting and / or colliding with a coating forming substance precursor in a coating starting area of a coating space,
And a method for producing coated quasi-fine particles.
[0016]
Further, the present invention provides a method for producing coated quasi-fine particles as described above, wherein the core particle powder having an average particle size exceeding 10 μm in volume-based frequency distribution and 20 μm or less is dispersed in the air by the final treatment of the quasi-fine particle high dispersion processing means group. To obtain a particle / gas mixture of the highly dispersed core particle powder, and the degree of dispersion β of the particles of the core particle powder is 80% or more, or the average particle diameter exceeds 20 μm and 50 μm or less in a volume-based frequency distribution. The core particle powder is dispersed in the air by the final treatment of the quasi-fine particle high dispersion treatment means group to form a highly dispersed core particle powder particle / gas mixture, and the degree of dispersion β of the core particle powder is 90% or more. Or the core particle powder having an average particle size of more than 50 μm and not more than 300 μm in the volume-based frequency distribution is dispersed in the air by the final treatment of the quasi-fine particle high dispersion processing means group, and the particles of the high-dispersion core particle powder .Gaseous mixture and its core particle powder Or a core particle powder having an average particle diameter of more than 300 μm and not more than 800 μm in the volume-based frequency distribution is airborne by the final treatment of the quasi-fine particle high dispersion processing means group. The particles are dispersed to form a particle / gas mixture of highly dispersed core particles, and the degree of dispersion β of the particles of the core particles is set to 97% or more, or the core particles having an average particle diameter exceeding 800 μm in a volume-based frequency distribution. The powder is dispersed in the air by the final treatment of the quasi-fine particle high dispersion processing means group to form a particle / gas mixture of highly dispersed core particle powder, and the degree of dispersion β of the core particle powder is 99% or more. Providing a dispersion step by a group of quasi-fine particles high dispersion processing means having a dispersing performance, or directly discharging the particles / gas mixture of the highly dispersed core particle powder by the group of quasi-fine particles high dispersion processing means to the coating step, or the dispersion step During the coating process, quasi-fine particles From the discharge section for discharging the particles / gas mixture of the high-dispersion core particle powder of the dispersion processing means group, directly discharge or inevitable for transportation, a hollow member, an intermediate member formed of a member that forms a hollow, and a pipe. The air-dispersed state of the particles in the particles / gas mixture of the high-dispersion core particle powder which is conveyed through one or more kinds of selected members and / or dispersed in the air with the dispersion performance described above. Aerial dispersion maintaining means for maintaining the dispersion performance, aerial dispersion promoting means for enhancing the aerial dispersion state of the particles in the gas / gas mixture of the highly dispersed core particle powder dispersed in the air with the dispersion performance, and the core particle powder The low-dispersion core particle powder portion of the mixture of the particles and the gas is separated, and the particles of the high-dispersion core particle powder in which the particles of the core particle powder are mainly present in the air in a single particle state. Select gas / gas mixture Select particle / gas mixture of highly dispersed core particle powder Conveying stage of one or through more also relates to a method for producing a coated semi particles and providing a conveying step.
[0017]
Furthermore, the present invention provides the method for producing coated quasi-fine particles described above, wherein the core particle powder having an average particle diameter of more than 10 μm and not more than 20 μm in the volume-based frequency distribution is aerated by the final treatment of the quasi-fine particle high dispersion processing means group. To a particle / gas mixture of the highly dispersed core particle powder, and the degree of dispersion β of the particles of the core particle powder is 80% or more, or the average particle diameter exceeds 20 μm in a volume-based frequency distribution, The core particle powder having a particle diameter of 50 μm or less is dispersed in the air by the final treatment of the quasi-fine particle high dispersion treatment means group to form a particle / gas mixture of the highly dispersed core particle powder. To 90% or more, or a core particle powder having an average particle diameter of more than 50 μm and 300 μm or less in the volume-based frequency distribution is dispersed in the air by the final treatment of the quasi-fine particle high dispersion processing means group to obtain a highly dispersed core. Particle / gas mixture of particle powder The dispersion degree β of the particles of the core particle powder is set to 95% or more, or the core particle powder having an average particle diameter of more than 300 μm and 800 μm or less in a volume-based frequency distribution is subjected to a quasi-fine particle high dispersion treatment group. Quasi-fine particle high dispersion processing means having a dispersing performance of dispersing in the air by the final treatment of the above into a particle / gas mixture of highly dispersed core particle powder, wherein the degree of dispersion β of the particles of the core particle powder is 97% or more. A group, or a core particle powder having an average particle size exceeding 800 μm in a volume-based frequency distribution, is dispersed in the air by the final treatment of a group of quasi-fine particle high dispersion processing means to form a particle / gas mixture of the high dispersion core particle powder. A part or more of the dispersing step and a part of the coating step by the quasi-fine particle high dispersion processing means group having a dispersing property of making the degree of dispersion β of the core particle powder 99% or more, Or more than one copy Also it relates to a process for the preparation of quasi-particles.
[0018]
Further, the present invention also provides the method for producing coated quasi-fine particles as described above, wherein the core particle powder having an average particle diameter of more than 10 μm and not more than 20 μm in a volume-based frequency distribution is airborne by the final treatment of the quasi-fine particle high dispersion processing means group. To form a particle / gas mixture of highly dispersed core particle powder, and a dispersion region in which the degree of dispersion β of the particles of the core particle powder is 80% or more,
The core particle powder having an average particle diameter of more than 20 μm and not more than 50 μm in the volume-based frequency distribution is dispersed in the air by the final treatment of the quasi-fine particle high dispersion processing means group to form a particle / gas mixture of the highly dispersed core particle powder. A spatial region in which the degree of dispersion β of the particles of the core particle powder is 90% or more;
The core particle powder having an average particle diameter of more than 50 μm and not more than 300 μm in the volume-based frequency distribution is dispersed in the air by the final treatment of the quasi-fine particle high dispersion processing means group to form a particle / gas mixture of the highly dispersed core particle powder. A spatial region in which the degree of dispersion β of the particles of the core particle powder is 95% or more,
A particle / gas mixture of highly dispersed core particle powder is obtained by dispersing core particle powder having an average particle diameter of more than 300 μm and not more than 800 μm in the volume-based frequency distribution in the air by the final treatment of the quasi-fine particle high dispersion processing means group. A spatial region in which the degree of dispersion β of the particles of the core particle powder is 97% or more,
The core particle powder having an average particle diameter exceeding 800 μm in the volume-based frequency distribution is dispersed in the air by the final treatment of the quasi-fine particle high dispersion processing means group to form a particle / gas mixture of the high dispersion core particle powder. Includes a surface through which all of the particles of the high-dispersion core particles and the particles of the core particles in the gas mixture within the space region where the degree of dispersion β of the core particles is 99% or more are passed. In the space area, the covering start area of the covering space is located, or
The core particle powder having an average particle diameter of more than 10 μm and not more than 20 μm in the volume-based frequency distribution is dispersed in the air by the final treatment of the quasi-fine particle high dispersion processing means group to form a particle / gas mixture of the highly dispersed core particle powder. A spatial region in which the degree of dispersion β of the particles of the core particle powder is 80% or more;
The core particle powder having an average particle diameter of more than 20 μm and not more than 50 μm in the volume-based frequency distribution is dispersed in the air by the final treatment of the quasi-fine particle high dispersion processing means group to form a particle / gas mixture of the highly dispersed core particle powder. A spatial region in which the degree of dispersion β of the particles of the core particle powder is 90% or more;
The core particle powder having an average particle diameter of more than 50 μm and not more than 300 μm in the volume-based frequency distribution is dispersed in the air by the final treatment of the quasi-fine particle high dispersion processing means group to form a particle / gas mixture of the highly dispersed core particle powder. A spatial region in which the degree of dispersion β of the particles of the core particle powder is 95% or more,
A particle / gas mixture of highly dispersed core particle powder is obtained by dispersing core particle powder having an average particle diameter of more than 300 μm and not more than 800 μm in the volume-based frequency distribution in the air by the final treatment of the quasi-fine particle high dispersion processing means group. A spatial region in which the degree of dispersion β of the particles of the core particle powder is 97% or more,
The core particle powder having an average particle diameter exceeding 800 μm in the volume-based frequency distribution is dispersed in the air by the final treatment of the quasi-fine particle high dispersion processing means group to form a particle / gas mixture of the high dispersion core particle powder. In the space region where the degree of dispersion β of the particles of the core particle powder is 99% or more, a space region including a surface through which all the particles to be collected by the collection unit of the collection unit passes, the coating start region of the coating space is set. The present invention also relates to a method for producing coated quasi-fine particles, which is characterized by being positioned.
[0019]
Furthermore, the present invention also provides that the particle size distribution of the coreM, And ([DM/ 5, 5DM], ≧ 90%).
[0020]
The present invention also provides an apparatus for carrying out the above-described method for producing coated particles, that is, a core-forming material is charged into a coating space, and a coating-forming substance precursor is generated through a gas phase and / or a coating is formed in a gas-phase state. In the apparatus for producing coated quasi-fine particles, the substance precursor is brought into contact with and / or collides with the particles of the core particle powder to coat the surfaces of the particles of the core particle powder with the coating forming substance.
(A) The final processing means of the quasi-fine particle high dispersion processing means group is
(A) a dispersing means for dispersing the particles of the core particle powder in the air; and
(B) separating the low-dispersion core particle powder portion in a mixture of the core particle powder and the gas in which the core particle powder is dispersed in the air; Highly dispersed core particle powder particles / gas mixture selecting means for selecting particles / gas mixture of highly dispersed core particle powder present in the air in a state and particles / gas mixture selecting means of this highly dispersed core particle powder A high-dispersion core provided with a feedback means for conveying the separated low-dispersion core particle powder portion to a final dispersing means and / or a processing means prior to the final dispersing means among the dispersing means in the quasi-fine particle high dispersion processing means group; Means for selecting a particle / gas mixture of the particle powder,
By a group of quasi-fine particle high dispersion processing means selected from the following, the average particle diameter in the volume-based frequency distribution exceeds 10 μm, the particles of the quasi-fine particle core particle powder of 300 μm or less or the particles of the core particle powder mainly consisting of quasi-fine particles Dispersion processing means to be dispersed in the air to form a particle / gas mixture of highly dispersed core particle powder,
(B) The particles of the core particle powder dispersed by the dispersing means are
When the average particle diameter is more than 10 μm and 20 μm or less, the degree of dispersion β is 80% or more,
When it exceeds 20 μm and is 50 μm or less, the degree of dispersion β is 90% or more,
When it exceeds 50 μm and is 300 μm or less, the degree of dispersion β is 95% or more,
When it exceeds 300 μm and is 800 μm or less, the degree of dispersion β is 97% or more, and
When it exceeds 800 μm, the degree of dispersion β is 99% or more.
A coating chamber which starts coating by contacting and / or colliding with a coating forming substance precursor in a coating starting area of a coating space in a dispersed state of
The present invention provides an apparatus for producing coated quasi-fine particles, characterized in that:
[0021]
Further, in the present invention, in the above-mentioned apparatus for producing coated quasi-fine particles, core particle powder having an average particle diameter of more than 10 μm and not more than 20 μm in a volume-based frequency distribution is dispersed in the air by the final treatment of the quasi-fine particle high dispersion processing means group. A particle / gas mixture of highly dispersed core particle powder, wherein the degree of dispersion β of the particles of the core particle powder is 80% or more, or a core particle having an average particle size of more than 20 μm and 50 μm or less in a volume-based frequency distribution. The powder is dispersed in the air by the final treatment of the quasi-fine particle high dispersion treatment means group to form a highly dispersed core particle powder particle / gas mixture, and the dispersion degree β of the core particle powder is set to 90% or more. Or a particle / gas mixture of highly dispersed core particle powder by dispersing core particle powder having an average particle size of more than 50 μm and not more than 300 μm in volume-based frequency distribution in the air by the final treatment of the quasi-fine particle high dispersion treatment means group. And the core particles of the powder Or a core particle powder having an average particle diameter of more than 300 μm and 800 μm or less in a volume-based frequency distribution is dispersed in the air by the final treatment of the quasi-fine particle high dispersion processing means group. A high-dispersion core particle powder particle / gas mixture, and a quasi-fine particle high dispersion treatment means group having a dispersing ability to make the degree of dispersion β of the core particle powder 97% or more, or an average in a volume-based frequency distribution. The core particle powder having a particle diameter exceeding 800 μm is dispersed in the air by the final treatment of the quasi-fine particle high dispersion treatment means group to form a particle / gas mixture of the high dispersion core particle powder, and the particles of the core particle powder Particles / gases of highly dispersed core particle powder generated by the final treatment of the quasi-fine particle high dispersion processing means group having a quasi-fine particle high dispersion processing means group having a dispersibility of 99% or more. Mix the mixture A member for forming a hollow member or a hollow which is indirectly connected to a coating chamber having a coating space of an apparatus for producing coated quasi-fine particles, or unavoidable for transportation, and which has a discharge part of the quasi-fine particle high dispersion processing means group released from the processing means group. And / or particles in a gas / gas mixture of highly dispersed core particle powder connected through one or more members selected from an intermediate member and a pipe, and / or dispersed in the air with dispersion performance. Aerial dispersion maintaining means for maintaining the in-air dispersion state of, aerial dispersion promotion means for increasing the aerial dispersion state of particles in the particles / gas mixture of highly dispersed core particle powder dispersed in the air with dispersion performance, In the mixture of the core particle powder and the gas, the low dispersion core particle powder portion is separated, and the high dispersion core particle powder in which the core particle powder particles are mainly present in the air in a single particle state. Highly dispersed core particle powder for selecting particle / gas mixture Also it relates to apparatus for producing a coated semi microparticles, characterized in that connected via one or more of the particles selecting a mixture of a gas means.
[0022]
Further, the present invention provides the above-mentioned apparatus for producing coated quasi-fine particles, wherein the core particle powder having an average particle diameter of more than 10 μm and not more than 20 μm in volume-based frequency distribution is airborne by the final treatment of the quasi-fine particle high dispersion processing means group. Disperse into a particle-gas mixture of highly dispersed core particle powder, and the degree of dispersion β of the particles of the core particle powder is 80% or more, or the average particle diameter is more than 20 μm and less than 50 μm in a volume-based frequency distribution. Is dispersed in the air by the final treatment of the quasi-fine particle high dispersion treatment means group to form a particle / gas mixture of the highly dispersed core particle powder, and the degree of dispersion β of the particles of the core particle powder is 90. % Or more, or a core particle powder having an average particle diameter of more than 50 μm and not more than 300 μm in volume-based frequency distribution is dispersed in the air by the final treatment of the quasi-fine particle high dispersion processing means group. Particle / gas mixture The dispersion degree β of the particles of the core particle powder is set to 95% or more, or the core particle powder having an average particle diameter of more than 300 μm and 800 μm or less in the volume-based frequency distribution is converted to the final particles of the quasi-fine particle high dispersion processing means group. A core / particle mixture having a high degree of dispersion and having a degree of dispersion β of 97% or more, or a core having an average particle diameter exceeding 800 μm in a volume-based frequency distribution. The particle powder is highly dispersed by the final treatment of the quasi-fine particle high dispersion processing means group to form a particle / gas mixture of the core particle powder, and the dispersibility of the core particle powder having a degree of dispersion β of 99% or more. Production of coated quasi-fine particles, characterized in that at least a part of the dispersion processing means including the group of quasi-fine particle dispersion processing means having the above and the coating chamber are provided so as to share at least a part of the space occupied by them. It also relates to equipment.
[0023]
Further, the present invention also provides the above-mentioned apparatus for producing coated quasi-fine particles, wherein the core particle powder having an average particle diameter of more than 10 μm and not more than 20 μm in a volume-based frequency distribution is airborne by the final treatment of the quasi-fine particle high dispersion processing means group. To form a particle / gas mixture of highly dispersed core particle powder, and a dispersion region in which the degree of dispersion β of the particles of the core particle powder is 80% or more,
The core particle powder having an average particle diameter of more than 20 μm and not more than 50 μm in the volume-based frequency distribution is dispersed in the air by the final treatment of the quasi-fine particle high dispersion processing means group to form a particle / gas mixture of the highly dispersed core particle powder. A spatial region in which the degree of dispersion β of the particles of the core particle powder is 90% or more;
The core particle powder having an average particle diameter of more than 50 μm and not more than 300 μm in the volume-based frequency distribution is dispersed in the air by the final treatment of the quasi-fine particle high dispersion processing means group to form a particle / gas mixture of the highly dispersed core particle powder. A spatial region in which the degree of dispersion β of the particles of the core particle powder is 95% or more,
A particle / gas mixture of highly dispersed core particle powder is obtained by dispersing core particle powder having an average particle diameter of more than 300 μm and not more than 800 μm in the volume-based frequency distribution in the air by the final treatment of the quasi-fine particle high dispersion processing means group. A spatial region in which the degree of dispersion β of the particles of the core particle powder is 97% or more,
The core particle powder having an average particle diameter exceeding 800 μm in the volume-based frequency distribution is dispersed in the air by the final treatment of the quasi-fine particle high dispersion processing means group to form a particle / gas mixture of the high dispersion core particle powder. Includes a surface through which all of the particles of the high-dispersion core particles and the particles of the core particles in the gas mixture within the space region where the degree of dispersion β of the core particles is 99% or more are passed. In the space area, the covering start area of the covering space is located, or
The core particle powder having an average particle diameter of more than 10 μm and not more than 20 μm in the volume-based frequency distribution is dispersed in the air by the final treatment of the quasi-fine particle high dispersion processing means group to form a particle / gas mixture of the highly dispersed core particle powder. A spatial region in which the degree of dispersion β of the particles of the core particle powder is 80% or more,
The core particle powder having an average particle diameter of more than 20 μm and not more than 50 μm in the volume-based frequency distribution is dispersed in the air by the final treatment of the quasi-fine particle high dispersion processing means group to form a particle / gas mixture of the highly dispersed core particle powder. A spatial region in which the degree of dispersion β of the particles of the core particle powder is 90% or more;
The core particle powder having an average particle diameter of more than 50 μm and not more than 300 μm in a volume-based frequency distribution is dispersed in the air by the final treatment of the quasi-fine particle high dispersion treatment means group to form a particle / gas mixture of the highly dispersed core particle powder, A spatial region in which the degree of dispersion β of the particles of the core particle powder is 95% or more,
A particle / gas mixture of highly dispersed core particle powder is obtained by dispersing core particle powder having an average particle diameter of more than 300 μm and not more than 800 μm in the volume-based frequency distribution in the air by the final treatment of the quasi-fine particle high dispersion processing means group. A spatial region in which the degree of dispersion β of the particles of the core particle powder is 97% or more,
The core particle powder having an average particle diameter exceeding 800 μm in the volume-based frequency distribution is dispersed in the air by the final treatment of the quasi-fine particle high dispersion processing means group to form a particle / gas mixture of the high dispersion core particle powder. In the space region where the degree of dispersion β of the particles of the core particle powder is 99% or more, in the space region including the surface through which all the particles collected by the collection unit of the collection unit pass, the coating start region of the coating space is set. The present invention also relates to an apparatus for producing coated quasi-fine particles, which is characterized by being positioned.
[0024]
Furthermore, the present invention also provides that the particle size distribution of the coreM, And ([DM/ 5, 5DM], ≧ 90%).
[0025]
Thus, according to the present invention, in the air, a coating-forming substance precursor generated from a raw material of the coating-forming substance via a gas phase by a gas phase method, The particles / gas mixture of the high-dispersion core particle powder composed of the quasi-fine particles having an average particle diameter exceeding 10 μm dispersed in the core and the core of the particle / gas mixture of the high-dispersion core particle powder in the coating start region of the coating space. The particles are joined in a highly dispersed state in which the degree of dispersion of the particle powder is β ≧ 80%, β ≧ 90%, β ≧ 95%, β ≧ 97 or β ≧ 99% according to the average particle diameter of the particles, and And / or colliding to coat the surface of the core particle powder with the coating forming substance. In this case, the coating-forming substance precursor has just been generated through a gas phase consisting of atoms, molecules, ions, clusters, atomic clusters, molecular clusters, cluster ions, and the like, and is itself very active during nascent. In this state, the coating material is firmly bonded to the surface of the individual core particles in a single particle state by initiating contact and / or collision with the core particles in a highly dispersed state, and as a result, the core particle powder The coated particles can be produced by coating the particles with a uniform coating-forming substance in a single particle unit of the above-mentioned particles and in a uniform amount for each particle.
[0026]
Before describing the present invention in detail, the terms used in the present specification will be defined first, and the specific content of the terms will be explained as necessary.
[0027]
Coated particles
Coated particles refer to coated particles. For example, specifically, particles in which the coating material is coated on the core particles in a form comprising at least one of ultrafine particles, islands, continuous texture, uniform film, protrusions, etc. Say.
[0028]
Gas phase coating method
The vapor-phase coating method is a method in which a raw material of a coating-forming substance is coated at least once through a gas-phase state composed of one or more of a vacuum molecular flow, an ion flow, plasma, gas, vapor, and aerosol, or a gas-phase state. Means a method of coating with a raw material of the coating forming material.
[0029]
Core particles
Core particles refer to particles to be coated. It is also referred to as matrix particles, seed particles or particles to be coated.
As the core particles, there is basically no limitation on a substance constituting the core particles, and known powder particles made of, for example, an inorganic material, a metal material, and an organic material can be used as the core particles.
[0030]
Core particle powder
The core particle powder refers to a powder composed of core particles. The particles of the core particle powder refer to particles constituting the core particle powder. The particles of the quasi-fine particle core particle powder or the particles of the core particle powder mainly composed of quasi-fine particles to be coated in the present invention have an average particle diameter exceeding 10 μm in a volume-based frequency distribution.
Preferably, the average particle size is DMAnd DMExceeds 10 μm, and the particle size distribution is a volume-based frequency distribution ([DM/ 5, 5DM], ≧ 90%). In such a powder having a relatively narrow distribution width, the dispersion characteristics or agglomeration characteristics of the powder are characterized by the average particle size, and the DMWhen the group of means for high dispersion treatment of fine particles is operated under conditions suitable for the value of, the particles can be dispersed.
In the case of a powder having a core particle powder having an average particle diameter of more than 10 μm, the particle size distribution of which has a wide distribution or a distribution having a plurality of peaks separated from each other, a suitable selective separation treatment such as a classification treatment is preferably performed. The coating treatment of the present invention is applied to each of the classified powders. Thus, under the above-mentioned conditions, the degree of dispersion is 80% or more, 90% or more, 95% or more, 97% or more in the degree of dispersion β in the covering start region of the covering space according to the average particle diameter under the above conditions for each of the classified powders. % Or 99% or more, the coating is started, and it becomes possible to coat each core particle powder.
[0031]
Coating material
The coating-forming substance refers to a substance that forms a coating on an object to be coated. For example, specifically, it refers to a substance that forms a coating in a form composed of one or more of ultrafine particles, islands, continuous textures, uniform films, protrusions, and the like.
In particular, when the form of the coating-forming substance is in the form of ultrafine particles, the particle diameter of the ultrafine particles is in the range of 0.005 μm to 0.5 μm.
Depending on the properties and functions desired for the resulting coated particles, the coating-forming substance may be composed of various inorganic, metallic or organic materials which are the same or different from the core particles, e.g. AlTwoOThree, SiOTwo, ZrOTwo, YTwoOThree, CaO, MgO, MgAlTwoOFour(Spinel), AlTwoSiOFive(Mullite) such as SiThreeNFour, AlN, TiN, ZrN, SiTwoNTwoO, HfN, VxN (x = 1 to 3), NbN, TaN, TaTwoWC, SiC, W which are carbides such as N and BNTwoC, HfC, TaC, TaTwoC, NbC, MoTwoBorides such as C, BP, TiB, TiBTwo, ZrBTwo, VB, VThreeBTwo, VBTwo, NbB, NbBTwo, TaB, TaBTwo, MoB, MoBTwo, MoBFour, MoTwoB, WB, WTwoB, WTwoBFive, LaB6, B13PTwoAnd simple metals such as Si, Al, Ni, Co, Cu, Fe, Ti, W, B, Nb, V, Zr, Hf, Ta, Re, Cr, Mo, Y, La, etc .; Various types of alloys such as TiAl, TiTwoAl, TiAlThree, TiNi, NiAl, NiThreeMaterials such as Al, composites of these materials, and epoxy resins, phenol resins, polyacrylamide resins, polyamide resins, urethane resins, polyester resins, polyvinyl chloride resins, acrylic resins, polyethylene, and the like can be used.
[0032]
Uniform coating
In the case of a uniform film-like coating forming substance, it means that the thickness of the coating film in a single particle is uniform everywhere. When the coating forming material is in the form of ultrafine particles, islands or protrusions, it means that the coating forming material in the form of ultrafine particles, islands or protrusions is coated with a uniform distribution. The inevitable non-uniformity in the process of forming the coating forming material is included in the category of uniformity.
[0033]
Definition of Injection into Covered Space
To be introduced into the coating space means to introduce the core particle powder into the coating space by dropping, for example, free fall. When charging by carrier gas, the core particle powder is introduced in the direction of the flow of the particle / gas mixture of the core particle powder, or in the direction of the flow on the gas, or the direction of the gas is changed. Refers to being introduced. Alternatively, it also refers to introduction under the action of a carrier gas. For example, it refers to introduction by a wave phenomenon of a carrier gas, specifically, a non-linear wave. Alternatively, it refers to introduction into a coating space by a sound wave, an ultrasonic wave, a magnetic field, an electron beam, or the like in a gas. It also refers to introduction by an external field, for example, an electric field, a magnetic field, an electron beam, or the like. Specifically, it means charging or magnetizing the powder particles with an electric field, a magnetic field, an electron beam, or the like, and introducing the particles into the coating space by attractive or repulsive force. In addition, it includes that the gas is sucked and introduced by the back pressure or reduced pressure of the gas.
[0034]
Covered space
The coating space is defined as a space where the coating-forming substance precursor generated from the raw material of the coating-forming substance via the gas phase and / or the coating-forming substance precursor in the gaseous state and the particles of the core particle powder come into contact with and / or collide with each other. Say. Alternatively, it refers to a space region in which the surface of the core particle powder is coated with the coating forming material.
[0035]
Coating room
The coating chamber refers to a chamber sharing at least a part of the coating space. More specifically, the coating room is a partitioned or substantially partitioned (substantially closed, semi-closed) room including the coating space, and a room including at least a part of the coating space.
[0036]
Feeling
The air refers to a space in a vacuum or gas phase state. Here, in the present invention, the gas phase state refers to a state of a molecular flow, an ion flow, plasma, gas, vapor, aerosol, and the like. The term "vacuum" refers to a state of reduced pressure technically. At any reduced pressure, strictly speaking, it includes gases, molecules, atoms, ions, and the like.
[0037]
Coating substance precursor
A coating forming material precursor is a coating forming material precursor. More specifically, the raw material of the coating-forming substance in a gaseous phase is formed and / or synthesized as it is or from the raw material of the coating-forming substance through the gas phase to form a coating on the core particles which are the particles to be coated. Substance immediately before The state of the coating forming material precursor is not limited as long as it is formed and / or synthesized from the raw material of the coating forming material somewhere via the gas phase. When the raw material of the coating forming material is in the gas phase, the raw material can also be a coating forming material precursor. The coating forming material precursor itself may be in the gas phase. Further, it may be before the reaction, during the reaction, or after the reaction. Specific examples of the coating material precursor include ions, atoms, molecules, clusters, atomic clusters, molecular clusters, cluster ions, ultrafine particles, gas, vapor, aerosol, and the like.
[0038]
Raw material of coating forming material
The raw material of the coating forming material refers to a raw material that becomes a material that forms a coating via a gas phase. Specific examples of the form of the raw material of the coating-forming substance include massive solids, powder particles, gases, and liquids.
[0039]
Dispersion degree β
The degree of dispersion β is an index for evaluating the dispersion performance of a powder disperser, as proposed by Masuda and Goto et al. (Chemical Engineering, The 22nd Autumn Meeting Abstracts, P349 (1989)). , Defined as the ratio of the weight of particles in the apparent primary particle state to the weight of all particles. Here, the particle in the apparent primary particle state is a mass-based frequency distribution f of powder particles in an arbitrary dispersed state.m2And mass-based frequency distribution f of powder particles completely dispersedm1And the ratio of the overlapping portion of is represented by β in the following equation.
[0040]
(Equation 1)
[0041]
Although the above equation evaluates the degree of dispersion based on the particle size distribution expressed on a mass basis, the degree of dispersion should be originally evaluated based on the particle size distribution expressed on a volume basis. However, when the powder particle density is the same, the particle size distribution on a mass basis and the particle size distribution on a volume basis are the same. Therefore, a mass-based particle size distribution that is practically easy to measure is measured and used as a volume-based particle size distribution. Accordingly, the original dispersion degree β is expressed by the following equation and the area of the hatched portion in FIG.
[0042]
(Equation 2)
The distribution and the average particle diameter of the core particle powder are basically used on a volume basis unless otherwise specified.
[0043]
Volume-based frequency distribution
The volume-based frequency distribution refers to a distribution of particle diameters represented by a volume ratio included in a certain particle diameter.
[0044]
([D1, DTwo], ≧ 90%)
([D1, DTwo], ≧ 90%) distribution is D1, DTwoIs the particle size, where D1<DTwoAnd D1DTwoThe following particles represent a distribution in which 90% or more are contained by volume, and as shown in FIG. 1B, a powder composed of particles having a ratio of a hatched portion of 90% or more.
[0045]
Volume-based frequency distribution ([DM/ 5, 5DM], ≧ 90%)
The particle size distribution used in the present invention is a volume-based frequency distribution ([DM/ 5, 5DM], ≧ 90%) distribution is DMIs a volume-based average particle size, DMAt least 1/5 times the particle size ofMRepresents a distribution containing 90% or more by volume of particles having a particle diameter of 5 times or less. For example, the average particle diameter DMIs 20 μm and the volume-based frequency distribution is ([DM/ 5, 5DM], ≧ 90%) indicates a distribution in which the volume-based average particle diameter is 20 μm and the particles having a particle diameter of 4 μm or more and 100 μm or less are 90% or more in volume. Here, the volume-based average particle diameter DMIs
(Equation 3)
DM= Σ (viDi) / Σvi
It is expressed as
[0046]
Coating start area
The area where the coating is started for the first time after the final processing by the group of quasi-fine particle high dispersion processing means is referred to as a coating start area. Therefore, even before the final processing of the group of quasi-fine particle high dispersion processing means, the region where coating is started for the first time is not the coating start region in the present invention.
[0047]
Dispersion β in coating start area
In the present invention, (1) the core particle powder having an average particle diameter of more than 10 μm and not more than 20 μm in the volume-based frequency distribution is dispersed in the air by the final treatment of the quasi-fine particle high dispersion processing means group, and A particle / gas mixture of the above, and the degree of dispersion β of the particles of the core particle powder is set to 80% or more, or (2) a core particle powder having an average particle diameter of more than 20 μm and 50 μm or less in a volume-based frequency distribution. The particles are dispersed in the air by the final treatment of the quasi-fine particle high dispersion treatment means group to form particles / gas mixture of highly dispersed core particle powder, and the degree of dispersion β of the particles of the core particle powder is 90% or more, or (3) Particles / gases of highly dispersed core particle powder by dispersing core particle powder having an average particle size of more than 50 μm and not more than 300 μm in the volume-based frequency distribution in the air by the final treatment of the quasi-fine particle high dispersion processing means group. A mixture, and the degree of dispersion β of the particles of the core particle powder is 95 Or (4) core particles having an average particle diameter of more than 300 μm and not more than 800 μm in a volume-based frequency distribution are dispersed in the air by the final treatment of the group of quasi-fine particles and a high dispersion processing means, and A powder / particle mixture of the powder, and the degree of dispersion β of the particles of the core particle powder is 97% or more, or (5) a core particle powder having an average particle diameter exceeding 800 μm in a volume-based frequency distribution, It is dispersed in the air by the final treatment of the quasi-fine particle high dispersion processing means group to form a highly dispersed core particle powder particle / gas mixture, and covers a region where the dispersion degree β of the core particle powder is 99% or more. A coating chamber is provided in which the coating start area of the space is located.
[0048]
If the degree of dispersion is in the coating start region of the coating space described above, the particles of the core particle powder are composed of particles of the quasi-fine particle core particle powder having an average particle diameter exceeding 10 μm or mainly quasi-fine particles in a volume-based frequency distribution. The core particle powder particles can be substantially dispersed in the air into a single particle state, and the coating forming substance precursor is evenly distributed on the surface of all the core particle powder particles passing through the coating start area of the coating space. A single particle can be provided with a uniform amount of coating-forming material because it contacts and / or collides with the particles.
In the quasi-fine particles having an average particle diameter of more than 10 μm, the above-mentioned dispersion degree β continuously changes with the average particle diameter of the core particle powder, but is difficult to express.
[0049]
Preferably, (1) core particle powder having an average particle size of more than 10 μm and not more than 20 μm in volume-based frequency distribution is dispersed in the air by final treatment of a group of quasi-fine particle high dispersion processing means, and A particle / gas mixture of the above, and the degree of dispersion β of the particles of the core particle powder is set to 90% or more, or (2) a core particle powder having an average particle diameter exceeding 20 μm and 50 μm in a volume-based frequency distribution is used. The particles are dispersed in the air by the final treatment of the fine particle high dispersion treatment means group to form a particle / gas mixture of highly dispersed core particle powder, and the degree of dispersion β of the particles of the core particle powder is 95% or more, or ( 3) A particle / gas mixture of highly dispersed core particle powder by dispersing core particle powder having an average particle diameter of more than 50 μm and not more than 300 μm in volume-based frequency distribution in the air by the final treatment of the group of quasi-fine particle high dispersion processing means. And the degree of dispersion β of the core particle powder is 97% or less. Or (4) the core particle powder having an average particle diameter exceeding 300 μm in volume-based frequency distribution is dispersed in the air by the final treatment of the group of quasi-fine particle high dispersion processing means, and the particles of the high dispersion core particle powder A coating chamber in which the coating start area of the coating space is located in a space area in which a gas mixture is used and the degree of dispersion β of the particles of the core particle powder is 99% or more. In the case of the coating chamber in which the coating start area of the coating space is positioned in this manner, the particles of the core particle powder, the particles of the quasi-fine particle core particle powder having an average particle diameter exceeding 10 μm in volume-based frequency distribution or mainly With respect to the particles of the core particle powder composed of the quasi-fine particles, the coating forming substance can be more uniformly coated in a single particle unit, and the coating amount can be more uniform for each core particle.
[0050]
Particles of the quasi-fine particle core particle powder having an average particle diameter exceeding 10 μm in the volume-based frequency distribution or the particles of the core particle powder mainly composed of the quasi-fine particles have an agglomeration action in the air and come into contact with each other. And / or colliding with each other, the distribution of the particles of the core particle powder in the particle / gas mixture of the highly dispersed core particle powder becomes uneven. However, if the coating is started in a dispersed state such as the degree of dispersion according to the particle size of the core particle powder, the particles of the quasi-fine particle core particles or the particles of the core particle powder mainly composed of quasi-fine particles The coat forming substance can be uniformly coated by a single particle unit, and the coat forming substance can be coated in a more uniform amount for each particle.
[0051]
Quasi-fine particle high dispersion processing means
In the present invention, the quasi-fine particle high dispersion treatment means group,
(A) at least one dispersing means,
(B) As a final processing means,
(A) dispersion means for dispersing the particles of the core particle powder in the air, or (b) low dispersion in the mixture of the particles of the core particle powder and the gas in which the particles of the core particle powder are dispersed in the air The particles of the high-dispersion core particles are separated from the core particle powder, and the particles of the high-dispersion core particles are selected mainly from a single particle state in the air. The gas mixture selecting means and the particles of the high-dispersion core particle powder The low-dispersion core particle powder portion separated by the gas mixture selecting means is finally dispersed in the dispersion means in the quasi-fine particle high dispersion processing means group. And / or feedback means for conveying the particles to the processing means before the final dispersing means.
[0052]
Preferably, (1) core particle powder having an average particle size of more than 10 μm and not more than 20 μm in volume-based frequency distribution is dispersed in the air by final treatment of a group of quasi-fine particle high dispersion processing means, and A particle / gas mixture of the above, and the degree of dispersion β of the particles of the core particle powder is set to 80% or more, or (2) a core particle powder having an average particle diameter of more than 20 μm and 50 μm or less in a volume-based frequency distribution. The particles are dispersed in the air by the final treatment of the quasi-fine particle high dispersion treatment means group to form particles / gas mixture of highly dispersed core particle powder, and the degree of dispersion β of the particles of the core particle powder is 90% or more, or (3) Particles / gases of highly dispersed core particle powder by dispersing core particle powder having an average particle size of more than 50 μm and not more than 300 μm in the volume-based frequency distribution in the air by the final treatment of the quasi-fine particle high dispersion processing means group. 95% dispersion degree β of particles of the core particle powder Or (4) core particles having an average particle diameter of more than 300 μm and not more than 800 μm in the volume-based frequency distribution are dispersed in the air by the final treatment of the quasi-fine particle high dispersion processing means group to obtain highly dispersed core particles. A powder / particle mixture of the powder, and the degree of dispersion β of the particles of the core particle powder is 97% or more, or (5) a core particle powder having an average particle diameter exceeding 800 μm in a volume-based frequency distribution, By the final treatment of the quasi-fine particle high dispersion treatment means group, the particles are dispersed in the air to form a highly dispersed core particle powder particle / gas mixture, and the dispersibility of the core particle powder having a degree of dispersion β of 99% or more is improved. Have
By providing a group of quasi-fine particle high dispersion processing means having a dispersion performance equal to or higher than those corresponding to various dispersities in the coating start area, high-quality coating corresponding to each dispersity is performed in the coating start area. be able to.
[0053]
Final processing means
When the final processing means of the group of quasi-fine particle high dispersion processing means is a dispersion means, this dispersion processing means is referred to as the final processing means of the fine particle high dispersion processing means group. In addition, the final processing means of the quasi-fine particle high dispersion processing means group is transferred to the final dispersion means of the quasi-fine particle high dispersion processing means in the low dispersion state during the particle / gas mixture selection processing step of the high-dispersion core particle powder. The particles / gas mixture selection means of the high-dispersion core particle powder provided with a feedback means for conveying the portion selectively separated because of the presence thereof, or the processing means before the final dispersion means, the particles of the high-dispersion core particle powder -Highly dispersed core particle powder particles provided with a feedback means for transporting a portion selectively separated due to a low dispersion state at the time of the gas mixture selection treatment step. In the case of the gas mixture selection means, the highly dispersed core particles The means for selecting a powder particle / gas mixture is referred to as the final processing means of the group of quasi-fine particle high dispersion processing means.
[0054]
In addition, it is provided before the means for selecting the particle / gas mixture of the highly dispersed core particle powder provided with the feedback means which is the final processing means of the group of quasi-fine particle high dispersion processing means (for example, the highly dispersed core particles provided with this feedback means). Between the means for selecting the particle / gas mixture of the powder and the final dispersing means or before the means for final dispersing) The means for selecting the particle / gas mixture of the high-dispersion core particle powder is a means for highly dispersing fine particles with or without the feedback means. It is a member of a group.
[0055]
Dispersal means
The means used for dispersion is called dispersion means. Those having a little or little dispersing effect can be used as dispersing means, and in the present invention, this is used as dispersing means. For example, a rotary feeder or an injection feeder for pneumatic transportation generally used as a supply unit (edited by the Society of Powder Technology, “Powder Engineering Handbook”, Nikkan Kogyo Shimbun (1986) P568, P571) also has a dispersing effect. When used as an intended means, it is a dispersion means. When the dispersion maintaining / promoting means described below is used for the purpose of dispersion (for the purpose of increasing β), it is also a dispersion means.
[0056]
In the present invention, the quasi-fine particle high-dispersion processing means is a group of means for accelerating and / or dispersing the particles of the core particle powder by an air flow placed on a velocity gradient, obstructing stationary particles and / or rotating bodies of the core particle powder. Selected one of dispersion by collision with an object, dispersion by fluidized bed and / or pulsating flow of particles of core particle powder and / or mechanical disintegration comprising vibration and / or scraping This is provided with the above dispersing mechanism.
[0057]
Specifically, the quasi-fine particle high dispersion processing means group includes an ejector type disperser, a Venturi type disperser, a thin tube, a stirrer, a disperser using obstacles in an air stream, a disperser using jet spray, Spiral tube, disperser using rotating blades, disperser using a rotating bottle (cage mill), fluidized bed disperser, disperser using pulsating flow, disperser using rotating drum, dispersion using vibration Machine, vibrating sieve, disperser using scraping by scraper, SAEI, Gonel type disperser, Nakajo type disperser, Roller type disperser, orifice type disperser, BM type disperser, Timbrell type disperser, Wright type The dispersing machine is provided with dispersing means comprising at least one selected from the dispersing machines. (Edited by the Society of Powder Engineering: “Handbook of Powder Engineering”, Nikkan Kogyo Shimbun (1986) P430).
[0058]
Also, a dispersing machine using a stirring blade described in JP-A-56-1336, a dispersing machine using a high-speed airflow and a dispersing nozzle described in JP-A-58-163454, and a dispersing machine described in JP-A-59-199027 are described. A dispersing machine utilizing the dispersing action of the rotating blades and the dispersing action of plasma ions, a dispersing machine utilizing the dispersing action of plasma ions described in JP-A-59-207319, and an ejector described in JP-A-59-216616. And a dispersing machine utilizing the dispersing action of plasma ions, an ejector described in JP-A-59-225728 and a dispersing machine utilizing the dispersing action of ion flow, and a dispersing action of plasma ions described in JP-A-59-183845. A dispersing machine utilizing a dispersing action of a dispersing blade and a pressure gas described in JP-A-63-166421; No. 6527, a dispersing machine using a line-shaped or ring-shaped slit-type nozzle, a dispersing machine using a mesh blade described in JP-A-63-221829, and a spraying nozzle described in JP-A-63-1629. A dispersing machine utilizing the dispersing action of a high-speed air flow from a disperser, a dispersing machine utilizing a large number of pores described in Japanese Utility Model Laid-Open No. 63-9218, an ejector-type dispersing machine described in Japanese Utility Model Application Laid-Open No. 62-156854, Those described in a disperser utilizing pores and orifices described in JP-A-63-6034 can also be used.
[0059]
Apparatuses described in Japanese Patent Application No. 63-31358, Japanese Patent Application No. 1-71071, Japanese Patent Application No. 2-218537, and the like are preferable as dispersion means suitable for the group of high dispersion processing means.
[0060]
Means for selecting particle / gas mixture of highly dispersed core particle powder
From the core-particle powder / gas mixture, a low-dispersion core particle powder portion other than the high-dispersion core particle powder / gas mixture mainly containing particles in a single particle state is separated and mainly separated. Means for selecting a particle / gas mixture of highly dispersed core particle powder containing particles in a single particle state. Agglomerated particles, which are aggregates of primary particles, can be separated by, for example, dry classification means because the apparent particle size is larger than the primary particle size. Examples of the means for selecting a particle / gas mixture of this highly dispersed core particle powder include a classification means using gravity, a classification means using inertial force, a classification means using centrifugal force, a classification means using static electricity, a flow Dry classifying means selected from one or more of classifying means using a layer is exemplified.
[0061]
Examples of the means for selecting a particle / gas mixture of this highly dispersed core particle powder include a gravity classifier, an inertial classifier, a centrifugal classifier, a cyclone, an air separator, a micron separator, a microplex, a multiplex, a zigzag classifier, and an accu classifier. Cut, conical separator, turbo classifier, super separator, dispersion separator, elbow jet, fluidized bed classifier, virtual impactor, O-Sepa, sieve, vibrating screen, shifter (Powder Engineering Handbook) Nikkan Kogyo Shimbun, P514 (1986)).
[0062]
Particle / gas mixture of core particle powder
The particle / gas mixture of the core particle powder is defined as (a) a homogeneous flow in which the particles of the core particle powder are uniformly suspended in the air (uniform floating flow), and (b) a particle of the core particle powder. Heterogeneous flow (non-homogeneous floating flow) showing a non-uniform distribution in a certain region in the air, (c) flow with sliding layer of core particle powder (sliding flow), or (d) core Refers to a flow of particles of a particle powder with a stationary layer.
[0063]
Particle / gas mixture of low dispersion core particle powder
Among the particle / gas mixture of the core particle powder, it refers to the particle / gas mixture of the core particle powder in which the particles of the core particle powder are present in the air mainly in a state other than the single particle state.
[0064]
Particle / gas mixture of highly dispersed core particle powder
A particle / gas mixture of the core particle powder in which the particles of the core particle powder are mainly present in the air in a single particle state. The particle / gas mixture of the highly dispersed core particle powder actually contains agglomerated particles even if it is extremely highly dispersed. The particle / gas mixture of the low-dispersion core particle powder actually contains single particles that are not agglomerated, and is selectively separated into particles / gas mixture of the low-dispersion core particle powder and particles of the high-dispersion core particle powder. -Divided into gaseous mixtures. The particle / gas mixture of the low-dispersion core particle powder becomes a particle / gas mixture of the high-dispersion core particle powder by selective separation and / or redispersion of the aggregated particles.
[0065]
Collection means
Means for taking out the coated quasi-fine particles coated in the coating space is referred to as recovery means. A portion of the collection unit where the collection process is performed is referred to as a collection unit. Coated quasi-fine particles coated by passing through the coating start area of the coating space are directly taken out of the air and collected, or taken out of the air and temporarily stored and collected, or collected together with the gas. .
The collecting unit of the collecting unit includes a collecting unit of a collecting unit using a partition (obstacle), a collecting unit of a collecting unit using gravity, a collecting unit of a collecting unit using inertial force, and a collecting unit using centrifugal force. Recovery section, recovery section of recovery means using attractive force due to electrification, recovery section of recovery means using thermophoretic force, recovery section of recovery means using Brownian diffusion, suction force due to back pressure and decompression of gas etc. The collection unit or the like of the used collection means can be used.
Preferable examples of the collecting section of the collecting means include a gravity dust collector, an inertial dust collector, a centrifugal dust collector, a filter dust collector, an electric dust collector, a washing dust collector, a particle packed bed, a cyclone, a bag filter, a ceramics filter, and a scrubber.
[0066]
Explanation of figure of quasi-fine particle high dispersion processing means group
FIG. 2A is a block diagram showing an example of a basic configuration of the quasi-fine particle high dispersion processing means group of the present invention. It is composed of a final dispersing means A for dispersing the particles of the core particle powder, and a component d of a dispersion processing means group before the final dispersing means. ε is a particle / gas mixture of highly dispersed core particle powder that exists in the air mainly in a single particle state among the particles of the core particle powder. As the component d, any treatment means such as a dispersion means, a supply means, and a means for selecting a particle / gas mixture of highly dispersed core particle powder can be used alone or in combination. The component d need not always be provided. The group of quasi-fine particle high dispersion processing means, after the processing of the dispersing means A, which is the final processing means, (1) dispersibility of the core particle powder having an average particle diameter of more than 10 μm and not more than 20 μm in the volume-based frequency distribution. Is 80% or more in β, or (2) the core particle powder having an average particle diameter of more than 20 μm and 50 μm or less in a volume-based frequency distribution has a dispersity of 90% or more in β, or (3) a volume-based frequency distribution. The core particle powder having a dispersion degree of 95% or more in β with respect to the core particle powder having an average particle diameter of more than 50 μm and 300 μm or less, or (4) the core particle powder having an average particle diameter of more than 300 μm and 800 μm or less in a volume-based frequency distribution. On the other hand, a dispersion degree β of 97% or more, or (5) a core particle powder having an average particle diameter of more than 800 μm in a volume-based frequency distribution can realize a dispersion degree β of 99% or more. is there.
[0067]
FIG. 2B is a block diagram showing another example of the basic configuration of the quasi-fine particle high dispersion processing means group of the present invention. The final dispersing means A for dispersing the particles of the core particle powder, the particles of the core particle powder are present in the air mainly in a single particle state to the final dispersing means A. The final high-dispersion core particle powder particle / gas mixture selecting means B provided with feedback means C for feeding back the low-dispersion core particle powder / gas mixture η other than the gas mixture, the dispersion before the final dispersing means It comprises a component d of the processing means group and a component e of the quasi-fine particle high dispersion processing means group between the final dispersion means and the final selection means. ε is a particle / gas mixture of highly dispersed core particle powder that exists in the air mainly in a single particle state among the particles of the core particle powder. As the component d, any processing means such as a dispersion means, a supply means, and a selection means can be used alone or in combination. As the component e, any processing means other than the dispersing means, for example, any processing means such as a supplying means and a selecting means can be used alone or in combination. The components d and e are not necessarily provided. The quasi-fine particle high dispersion processing means group has a configuration capable of achieving the above-mentioned degree of dispersion with respect to the core particle powder having the above average particle diameter after the processing by the selection means B which is the final processing means.
[0068]
FIG. 2C is a block diagram showing another example of the basic configuration of the quasi-fine particle high dispersion processing means group of the present invention. The final dispersion means A for dispersing the particles of the core particle powder, and the high dispersion core particles in which the particles of the core particle powder are present in the air mainly in a single particle state to the processing means before the final dispersion means A High-dispersion core particle powder / gas mixture selecting means B provided with feedback means C for feeding back low-dispersion core particle powder particles / gas mixture η other than powder particles / gas mixture, final dispersing means It is composed of the component d of the previous group of high dispersion processing means for fine particles and the component e of the group of high dispersion processing means for fine particles between the last dispersion means and the last selection means. ε is a particle / gas mixture of highly dispersed core particle powder that exists in the air mainly in a single particle state among the particles of the core particle powder. As the component d, any processing means such as a dispersion means, a supply means, and a selection means can be used alone or in combination. As the component d, any processing means other than the dispersion means, for example, any processing means such as a supply means and a selection means can be used alone or in combination. The components d and e are not necessarily provided. The quasi-fine particle high dispersion processing means group has a configuration capable of achieving the above-mentioned degree of dispersion with respect to the core particle powder having the above average particle diameter after the processing by the selection means B which is the final processing means.
[0069]
In addition, since it is the above structure, the supply source of powder, such as a supply tank and a core particle generation means, may also be included in the structure of this quasi-fine particle high dispersion processing means group. For example, in the case of FIG. 2C, it goes without saying that the configuration in which the feedback destination of the feedback unit C is the supply tank may be the configuration of the high dispersion processing unit group. Needless to say, a crushing step of crushing and / or crushing the particles of the core particle powder may be inserted before the dispersion step of the quasi-fine particle high dispersion processing means group.
[0070]
The basic configuration of the quasi-fine particle high dispersion processing means group will be described in more detail based on a more detailed block diagram.
[0071]
FIG. 3A is a block diagram illustrating a first configuration of the quasi-fine particle high dispersion processing means group of the present invention, and corresponds to FIG. 2A. The present embodiment includes a
[0072]
FIG. 3 (b) is a block diagram illustrating a second configuration of the quasi-fine particle high dispersion processing means group of the present invention, and corresponds to FIG. 2 (a). This example is composed of a
[0073]
FIG. 3 (c) is a block diagram illustrating a third configuration of the quasi-fine particle high dispersion processing means group of the present invention, and corresponds to FIG. 2 (b). In this example, the
[0074]
FIG. 3D is a block diagram illustrating a fourth configuration of the quasi-fine particle high dispersion processing means group according to the present invention, and corresponds to FIG. 2B. In this example, a
[0075]
FIG. 3 (e) is a block diagram illustrating a fifth configuration of the quasi-fine particle high dispersion processing means group of the present invention, and corresponds to FIG. 2 (b). In this example, a
[0076]
FIG. 3 (f) is a block diagram illustrating a sixth configuration of the quasi-fine particle high dispersion processing means group of the present invention, and corresponds to FIG. 2 (b). In this example, the
[0077]
FIG. 3 (g) is a block diagram illustrating a seventh configuration of the quasi-fine particle high dispersion processing means group of the present invention, and corresponds to FIG. 2 (c). In this example, a
[0078]
In order to maintain the high dispersion state of the quasi-fine particles achieved in this way, air dispersion maintaining means may be added to the quasi-fine particle high dispersion processing means group. Here, the means for maintaining dispersion in the air refers to means for preventing the particles of the core particle powder dispersed and supported in the air from reaggregating and maintaining the degree of dispersion β. Further, in order to promote the high dispersion state of the core particles achieved in this way, an air dispersion promoting means may be added between the group of fine particle high dispersion processing means and the coating chamber. The means for promoting dispersion in the air here means promoting the redispersion of mainly reagglomerated particles among the particles of the core particle powder dispersed and supported in the air, slowing down the dispersion state or temporarily reducing the dispersion state. Means for promoting re-dispersion so as to restore the dispersed state to the original high-dispersion state.
Preferable examples of the air dispersion maintaining means or the air dispersion promotion means include a pipe vibrating device, a pipe heating device, a plasma generating device, a charging device, and the like.
[0079]
A pipe vibrating device is a means of suppressing reaggregation and maintaining a high dispersion state by giving vibrations that can not be called a disperser to particles dispersed in the air by the vibration of a pipe with an oscillator installed, or a reaggregation Means for promoting the dispersion of the particles.
The pipe heating device expands the carrier gas by applying heat from the outside of the carrier gas by the heated pipe, accelerates the flow rate so that it can not be called a disperser, suppresses reaggregation, and disperses the reaggregated particles. It is a means to promote.
[0080]
The plasma generating device generates plasma in the air carrying the core particle powder dispersed therein, and the collision between the plasma ions and the core particles suppresses the reaggregation and maintains the highly dispersed state or the reagglomerated means. It is a means to promote the dispersion of particles.
The charging device generates monopolar ions in the air in which the core particle powder is dispersed and supported by a method such as corona discharge, electron beam, or radiation, and passes the particles through a monopolar ion atmosphere to convert the particles into monopolar ions. And means for suppressing reaggregation by the repulsive force of static electricity and maintaining a highly dispersed state, or for promoting dispersion of reaggregated particles.
[0081]
The core particle powder in a highly dispersed state of the quasi-fine particles thus formed is sent to a coating chamber in order to coat the surface of the particles with the coating forming substance. The coating chamber is provided with a coating space including a coating start area.
[0082]
Although it is desirable that the quasi-fine particle high dispersion treatment means group and the coating chamber are directly connected, they may be connected using a hollow member and / or a pipe inevitable for transportation. Also in this case, it is indispensable to set the degree of dispersion β in the coating start region to a value in the above range.
When the quasi-fine particle high dispersion treatment means group and the coating chamber are separately provided and connected therebetween, the core particle powder may be introduced into the coating chamber in a dispersed state. For this purpose, air dispersion maintaining means which is a device for maintaining the dispersion state of the core particle powder and / or air dispersion promotion means and / or the core particle powder which is a device for increasing the dispersion state during this period The low-dispersion core particle powder is separated from the low-dispersion core particle powder portion of the high-dispersion core particle powder mainly containing single-particle particles. A gas mixture selection means may be provided;
[0083]
From the core particle powder immediately after being dispersed in the air in the quasi-fine particle high dispersion processing means group, a core particle powder in a low dispersion state mainly composed of agglomerated particles and a core particle powder in a high dispersion state mainly composed of primary particles It is effective if the quasi-fine particle high dispersion processing means group is connected to the coating chamber through the high-dispersion core particle powder particle / gas mixture selecting means for selectively separating and separating the highly dispersed state into the coating chamber. Can be coated.
Further, in the present invention, the quasi-fine particle high dispersion treatment means group can share at least a part of the space with (1) the coating chamber, or (2) the coating space, or (3) the coating start area.
[0084]
That is, the dispersion space and the coating chamber in the quasi-fine particle high dispersion processing means group, or the dispersion space and the coating space having the coating start area in the quasi-fine particle high dispersion processing means group, or the quasi-fine particle high dispersion processing means group The inside dispersion space and the coating start area can be spatially shared.
Here, the coating start region is defined as (1) a core particle powder having an average particle size of more than 10 μm and not more than 20 μm in a volume-based frequency distribution, the degree of dispersion β of the particles is 80% or more, and (2) the volume-based frequency. In the case of core particle powder having an average particle diameter of more than 20 μm and not more than 50 μm in the distribution, the degree of dispersion β of the particles is 90% or more, or (3) a core having an average particle diameter of more than 50 μm and not more than 300 μm in the volume-based frequency distribution. In the case of the particle powder, the degree of dispersion β of the particles is 95% or more. (4) In the case of the core particle powder in which the average particle diameter is more than 300 μm and not more than 800 μm in the volume-based frequency distribution, the degree of dispersion β of the particles is 97% or less. % Or more, (5) in the case of a core particle powder having a volume-based frequency distribution and an average particle diameter exceeding 800 μm, a core particle powder in a highly dispersed state transported in a dispersed state having a particle dispersion degree β of 99% or more. Coating-forming substance precursor and / or coating form in gaseous phase formed in the body via gas phase It refers to a region where the material precursor contacts and / or collides and starts coating, and the following embodiments shown in FIGS. 4A to 4E are considered.
[0085]
That is, in FIGS. 4A to 4E, the coating start area is an area indicated by 2. In FIG. 4 (a), the
In FIG. 4 (b), the
With the above configuration, coating of all the core particle powders is started in a dispersed state with the above-mentioned dispersity β.
In FIG. 4 (c), the
In FIG. 4D, a covering
In FIG. 4 (e), a collecting
[0086]
From the above description, the apparatus for carrying out the present invention is composed of the quasi-fine particle high dispersion processing means group and the coating chamber or the quasi-fine particle high dispersion processing means group, the coating chamber, and the recovery means. The components can be combined in various ways, and a configuration example of these devices will be described below with reference to the drawings.
[0087]
FIG. 5A is a block diagram illustrating a configuration of a first device that implements the present invention. This apparatus of this example includes a coating apparatus manufacturing apparatus main body 2-A, a coating chamber 2-B1, a coating space 2-B2, a coating start area 2-B3, a quasi-fine particle high dispersion processing means group 2-C1, and a collecting means 2. -D. The quasi-fine particle high dispersion processing means group 2-C1 is directly connected to the coating chamber 2-B1.
[0088]
FIG. 5B is a block diagram illustrating a configuration of a second device that implements the present invention. This apparatus of this example includes a coating apparatus manufacturing apparatus main body 2-A, a coating chamber 2-B1, a coating space 2-B2, a coating start area 2-B3, a quasi-fine particle high dispersion processing means group 2-C1, an unavoidable hollow. It is composed of a member 2-C2 and a collecting means 2-D. The quasi-fine particle high dispersion processing means group 2-C1 is connected to the coating chamber 2-B1 via an unavoidable hollow member 2-C2.
[0089]
FIG. 5C is a block diagram illustrating a configuration of a third device that embodies the present invention. This apparatus of this example includes a coating apparatus manufacturing apparatus main body 2-A, a coating chamber 2-B1, a coating space 2-B2, a coating start area 2-B3, a quasi-fine particle high dispersion processing means group 2-C1, and air dispersion. It is composed of a maintenance means 2-C3 and a recovery means 2-D. The quasi-fine particle high dispersion processing means group 2-C1 is connected to the coating chamber 2-B1 via the air dispersion maintaining means 2-C3.
[0090]
FIG. 5D is a block diagram illustrating a configuration of a fourth device that embodies the present invention. This apparatus of this example includes a coating apparatus manufacturing apparatus main body 2-A, a coating chamber 2-B1, a coating space 2-B2, a coating start area 2-B3, a quasi-fine particle high dispersion processing means group 2-C1, and a collecting means 2. -D. The quasi-fine particle high dispersion processing means group 2-C1 shares a space with the coating room 2-B1.
[0091]
FIG. 5E is a block diagram illustrating a configuration of a fifth device that embodies the present invention. This apparatus of this example includes a coating apparatus manufacturing apparatus main body 2-A, a coating chamber 2-B1, a coating space 2-B2, a coating start area 2-B3, a quasi-fine particle high dispersion processing means group 2-C1, and a collecting means 2. -D. The quasi-fine particle high dispersion processing means group 2-C1 is provided in the coating chamber 2-B1.
[0092]
FIG. 5F is a block diagram illustrating the configuration of a sixth device that embodies the present invention. This apparatus of this example includes a coating apparatus manufacturing apparatus main body 2-A, a coating chamber 2-B1, a coating space 2-B2, a coating start area 2-B3, a quasi-fine particle high dispersion processing means group 2-C1, and a collecting means 2. -D. A coating room 2-B1 is provided in the dispersion space of the quasi-fine particle high dispersion processing means group 2-C1.
[0093]
FIG. 5G is a block diagram illustrating a configuration of a seventh device that embodies the present invention. This apparatus of this example includes a coating apparatus manufacturing apparatus main body 2-A, a coating chamber 2-B1, a coating space 2-B2, a coating start area 2-B3, a quasi-fine particle high dispersion processing means group 2-C1, and a collecting means 2. -D, a recoating supply means 2-E. The coated quasi-fine particles after coating from the recovery means 2-D are transported to the high dispersion processing means group 2-C1 by the recoating supply means 2-E, and the coating processing can be repeatedly performed.
All the devices having such a configuration are included in the present invention.
[0094]
The coated quasi-fine particles obtained by coating the core particle powder with the coating forming material as described above can be coated again with the coating forming material, or this recoating can be repeated. In this case, the coated quasi-fine particles are sent to the recoating supply means. Here, the recoating supply means means means for transporting the coated quasi-fine particles after coating to a group of quasi-fine particle high dispersion processing means in order to perform recoating. Specifically, it is a means provided with (a) a collecting means for collecting coated quasi-fine particles, and (b) a coated particle conveying means for conveying the coated quasi-fine particles from the collecting means to a group of quasi-fine particle high dispersion processing means. Or (a) a collecting means for collecting the coated quasi-fine particles, (b) a coated particle conveying means for conveying the coated quasi-fine particles from the collecting means to the quasi-fine particle high dispersion processing means group, (c) and This is a means provided with a means for classifying coated particles for classification. When the coating amount is large, the particle size distribution of the core particle powder before coating and the particle size distribution of the coated quasi-fine particles after coating are different. Therefore, it is effective if the particle size distribution of the coated quasi-fine particles after coating is adjusted by the coated particle classification means and re-coating is performed.
[0095]
This recoating process can be repeated as necessary, and the coating amount of the coating forming substance can be set to a desired value. Further, the coating process can be repeated by changing the type of the coating forming material, and thus, a multi-component material can be multi-coated as a coating forming material.
[0096]
The apparatus for producing coated quasi-fine particles applied to the present invention is not limited as long as the coating forming substance is an apparatus for producing coated quasi-fine particles in which the particle surface of the core particle powder is coated by a gas phase method passing through a gas phase. . For example, as a chemical vapor deposition (CVD) device, a thermal CVD device, a plasma CVD device, a CVD (visible light beam CVD, laser CVD, ultraviolet CVD, infrared CVD, far infrared CVD) device using an electromagnetic wave, a MOCVD device, or the like, or As a physical vapor deposition (PVD) device, a vacuum vapor deposition device, an ion sputtering device, an ion plating device, or the like can be applied. More specifically, for example, a particle whose surface is coated with ultrafine particles of JP-A-3-75302 and a coated particle producing apparatus described in the method for producing the same are suitable.
[0097]
As described above, in the present invention, the particles of the quasi-fine particle core particle powder or the core particle powder mainly composed of the quasi-fine particle are introduced into the coating space, and the coating forming substance precursor and / or the gas phase are formed through the gas phase. The coating-forming substance precursor in a state is brought into contact with and / or collides with the particles of the core particle powder to produce coated quasi-fine particles for coating the surfaces of the particles of the core particle powder with the coating-forming substance. The basic steps of the above are summarized as follows.
[0098]
I
(A) By means of the quasi-fine particle high dispersion processing means group, particles of quasi-fine particle core particle powder having an average particle diameter exceeding 10 μm in volume-based frequency distribution or core particle powder mainly composed of quasi-fine particles are airborne. A dispersing step of dispersing into a particle / gas mixture of highly dispersed core particle powder,
(B) The particles of the highly dispersed core particle powder and the particles of the core particle powder of the gas mixture dispersed in this dispersion step are:
When the average particle diameter is more than 10 μm and 20 μm or less, the degree of dispersion β is 80% or more,
When it exceeds 20 μm and is 50 μm or less, the degree of dispersion β is 90% or more,
When it exceeds 50 μm and is 300 μm or less, the degree of dispersion β is 95% or more,
When it exceeds 300 μm and is 800 μm or less, the dispersity β is 97% or more,
When it exceeds 800 μm, the degree of dispersion β is 99% or more,
In a dispersed state of, a coating step of starting coating by contacting and / or colliding with a coating forming substance precursor in a coating starting area of a coating space,
Coating method provided with.
[0099]
II
(A) The particles of the core particle powder having a mean particle diameter of more than 10 μm and not more than 20 μm in the volume-based frequency distribution or the particles of the core particle powder mainly composed of the quasi-fine particles are dispersed by the quasi-fine particle high dispersion processing means group. A group of quasi-fine particle high dispersion processing means for realizing a degree of dispersion β of 80% or more of the particles of the core particle powder of the gas mixture and the particles of the highly dispersed core particle powder,
Particles of a quasi-fine particle core particle powder having an average particle diameter of more than 20 μm and not more than 50 μm in a volume-based frequency distribution or particles of a core particle powder mainly composed of quasi-fine particles are dispersed by a quasi-fine particle high dispersion treatment means group. A group of quasi-fine particle high dispersion processing means for realizing a degree of dispersion β of 90% or more of the particles of the core particle powder of the dispersed core particle powder and the gas mixture,
Particles of a quasi-fine particle core particle powder having an average particle diameter of more than 50 μm and not more than 300 μm in a volume-based frequency distribution or particles of a core particle powder mainly composed of quasi-fine particles are dispersed by a quasi-fine particle high dispersion treatment means group. A group of quasi-fine particle high dispersion processing means for realizing a degree of dispersion β of 95% or more of the particles of the core particle powder of the dispersed core particle powder / gas mixture,
Particles of a quasi-fine particle core particle powder having an average particle diameter of more than 300 μm and 800 μm or less in a volume-based frequency distribution or particles of a core particle powder mainly composed of quasi-fine particles are dispersed by a quasi-fine particle high dispersion treatment means group. A group of quasi-fine particle high dispersion processing means for realizing a degree of dispersion β of 97% or more of particles of the core particle powder of the dispersed core particle powder / gas mixture,
Highly dispersed core particles obtained by dispersing particles of a quasi-fine particle core particle powder having an average particle diameter exceeding 800 μm in a volume-based frequency distribution or particles of a core particle powder mainly consisting of quasi-fine particles by a quasi-fine particle high dispersion treatment means group A group of quasi-fine particle high dispersion processing means for realizing a dispersion degree β of 99% or more of the particles of the powder particles / core particles of the gas mixture,
A dispersion step of dispersing in the air to form a particle / gas mixture of highly dispersed core particle powder,
(B) The particles of the highly dispersed core particle powder and the particles of the core particle powder of the gas mixture dispersed in this dispersion step are:
When the average particle diameter is more than 10 μm and 20 μm or less, the degree of dispersion β is 80% or more,
When it exceeds 20 μm and is 50 μm or less, the degree of dispersion β is 90% or more,
When it exceeds 50 μm and is 300 μm or less, the degree of dispersion β is 95% or more,
When it exceeds 300 μm and is 800 μm or less, the dispersity β is 97% or more,
When it exceeds 800 μm, the degree of dispersion β is 99% or more,
In a dispersed state of, a coating step of starting coating by contacting and / or colliding with a coating forming substance precursor in a coating starting area of a coating space,
Coating method provided with.
[0100]
III
(A) The particles of the core particle powder having a mean particle diameter of more than 10 μm and not more than 20 μm in the volume-based frequency distribution or the particles of the core particle powder mainly composed of the quasi-fine particles are dispersed by the quasi-fine particle high dispersion processing means group. A group of quasi-fine particle high dispersion processing means for realizing a degree of dispersion β of 80% or more of the particles of the core particle powder of the gas mixture and the particles of the highly dispersed core particle powder,
Particles of a quasi-fine particle core particle powder having an average particle diameter of more than 20 μm and not more than 50 μm in a volume-based frequency distribution or particles of a core particle powder mainly composed of quasi-fine particles are dispersed by a quasi-fine particle high dispersion treatment means group. A group of quasi-fine particle high dispersion processing means for realizing a degree of dispersion β of 90% or more of the particles of the core particle powder of the dispersed core particle powder and the gas mixture,
Particles of a quasi-fine particle core particle powder having an average particle diameter of more than 50 μm and not more than 300 μm in a volume-based frequency distribution or particles of a core particle powder mainly composed of quasi-fine particles are dispersed by a quasi-fine particle high dispersion treatment means group. A group of quasi-fine particle high dispersion processing means for realizing a degree of dispersion β of 95% or more of the particles of the core particle powder of the dispersed core particle powder / gas mixture,
Particles of a quasi-fine particle core particle powder having an average particle diameter of more than 300 μm and 800 μm or less in a volume-based frequency distribution or particles of a core particle powder mainly composed of quasi-fine particles are dispersed by a quasi-fine particle high dispersion treatment means group. A group of quasi-fine particle high dispersion processing means for realizing a degree of dispersion β of 97% or more of particles of the core particle powder of the dispersed core particle powder / gas mixture,
Highly dispersed core particles obtained by dispersing particles of a quasi-fine particle core particle powder having an average particle diameter exceeding 800 μm in a volume-based frequency distribution or particles of a core particle powder mainly consisting of quasi-fine particles by a quasi-fine particle high dispersion treatment means group A group of quasi-fine particle high dispersion processing means for realizing a dispersion degree β of 99% or more of the particles of the powder particles / core particles of the gas mixture,
A dispersion step of dispersing in the air to form a particle / gas mixture of highly dispersed core particle powder,
(B) a conveying step of directly conveying the particles of the highly dispersed core particle powder and the particles of the core particle powder of the gas mixture dispersed in the dispersion step to the coating step;
(C) The particles of the highly dispersed core particle powder and the particles of the core particle powder of the gas mixture conveyed in this conveyance step are
When the average particle diameter is more than 10 μm and 20 μm or less, the degree of dispersion β is 80% or more,
When it exceeds 20 μm and is 50 μm or less, the degree of dispersion β is 90% or more,
When it exceeds 50 μm and is 300 μm or less, the degree of dispersion β is 95% or more,
When it exceeds 300 μm and is 800 μm or less, the dispersity β is 97% or more,
When it exceeds 800 μm, the degree of dispersion β is 99% or more,
In a dispersed state of, a coating step of starting coating by contacting and / or colliding with a coating forming substance precursor in a coating starting area of a coating space,
Coating method provided with.
[0101]
IV
(A) The particles of the core particle powder having a mean particle diameter of more than 10 μm and not more than 20 μm in the volume-based frequency distribution or the particles of the core particle powder mainly composed of the quasi-fine particles are dispersed by the quasi-fine particle high dispersion processing means group. A group of quasi-fine particle high dispersion processing means for realizing a degree of dispersion β of 80% or more of the particles of the core particle powder of the gas mixture and the particles of the highly dispersed core particle powder,
Particles of a quasi-fine particle core particle powder having an average particle diameter of more than 20 μm and not more than 50 μm in a volume-based frequency distribution or particles of a core particle powder mainly composed of quasi-fine particles are dispersed by a quasi-fine particle high dispersion treatment means group. A group of quasi-fine particle high dispersion processing means for realizing a degree of dispersion β of 90% or more of the particles of the core particle powder of the dispersed core particle powder and the gas mixture,
Particles of a quasi-fine particle core particle powder having an average particle diameter of more than 50 μm and not more than 300 μm in a volume-based frequency distribution or particles of a core particle powder mainly composed of quasi-fine particles are dispersed by a quasi-fine particle high dispersion treatment means group. A group of quasi-fine particle high dispersion processing means for realizing a degree of dispersion β of 95% or more of the particles of the core particle powder of the dispersed core particle powder / gas mixture,
Particles of a quasi-fine particle core particle powder having an average particle diameter of more than 300 μm and 800 μm or less in a volume-based frequency distribution or particles of a core particle powder mainly composed of quasi-fine particles are dispersed by a quasi-fine particle high dispersion treatment means group. A group of quasi-fine particle high dispersion processing means for realizing a degree of dispersion β of 97% or more of particles of the core particle powder of the dispersed core particle powder / gas mixture,
Highly dispersed core particles obtained by dispersing particles of a quasi-fine particle core particle powder having an average particle diameter exceeding 800 μm in a volume-based frequency distribution or particles of a core particle powder mainly consisting of quasi-fine particles by a quasi-fine particle high dispersion treatment means group A group of quasi-fine particle high dispersion processing means for realizing a dispersion degree β of 99% or more of the particles of the powder particles / core particles of the gas mixture,
A dispersion step of dispersing in the air to form a particle / gas mixture of highly dispersed core particle powder,
(B) The hollow member, the intermediate member including the member forming the hollow, and the pipe, inevitably transporting the particles of the highly dispersed core particle powder and the particles of the core particle powder of the gas mixture dispersed in the dispersion step. A transporting step of transporting through one or more members selected from
(C) The particles of the highly dispersed core particle powder and the particles of the core particle powder of the gas mixture conveyed in this conveyance step are
When the average particle diameter is more than 10 μm and 20 μm or less, the degree of dispersion β is 80% or more,
When it exceeds 20 μm and is 50 μm or less, the degree of dispersion β is 90% or more,
When it exceeds 50 μm and is 300 μm or less, the degree of dispersion β is 95% or more,
When it exceeds 300 μm and is 800 μm or less, the dispersity β is 97% or more,
When it exceeds 800 μm, the degree of dispersion β is 99% or more,
In a dispersed state of, a coating step of starting coating by contacting and / or colliding with a coating forming substance precursor in a coating starting area of a coating space,
Coating method provided with.
[0102]
V
(A) The particles of the core particle powder having a mean particle diameter of more than 10 μm and not more than 20 μm in the volume-based frequency distribution or the particles of the core particle powder mainly composed of the quasi-fine particles are dispersed by the quasi-fine particle high dispersion processing means group. A group of quasi-fine particle high dispersion processing means for realizing a degree of dispersion β of 80% or more of the particles of the core particle powder of the gas mixture and the particles of the highly dispersed core particle powder,
Particles of a quasi-fine particle core particle powder having an average particle diameter of more than 20 μm and not more than 50 μm in a volume-based frequency distribution or particles of a core particle powder mainly composed of quasi-fine particles are dispersed by a quasi-fine particle high dispersion treatment means group. A group of quasi-fine particle high dispersion processing means for realizing a degree of dispersion β of 90% or more of the particles of the core particle powder of the dispersed core particle powder and the gas mixture,
Particles of a quasi-fine particle core particle powder having an average particle diameter of more than 50 μm and not more than 300 μm in a volume-based frequency distribution or particles of a core particle powder mainly composed of quasi-fine particles are dispersed by a quasi-fine particle high dispersion treatment means group. A group of quasi-fine particle high dispersion processing means for realizing a degree of dispersion β of 95% or more of the particles of the core particle powder of the dispersed core particle powder / gas mixture,
Particles of a quasi-fine particle core particle powder having an average particle diameter of more than 300 μm and 800 μm or less in a volume-based frequency distribution or particles of a core particle powder mainly composed of quasi-fine particles are dispersed by a quasi-fine particle high dispersion treatment means group. A group of quasi-fine particle high dispersion processing means for realizing a degree of dispersion β of 97% or more of particles of the core particle powder of the dispersed core particle powder / gas mixture,
Highly dispersed core particles obtained by dispersing particles of a quasi-fine particle core particle powder having an average particle diameter exceeding 800 μm in a volume-based frequency distribution or particles of a core particle powder mainly consisting of quasi-fine particles by a quasi-fine particle high dispersion treatment means group A group of quasi-fine particle high dispersion processing means for realizing a dispersion degree β of 99% or more of the particles of the powder particles / core particles of the gas mixture,
A dispersion step of dispersing in the air to form a particle / gas mixture of highly dispersed core particle powder,
(B) The particles / gas of the highly dispersed core particle powder obtained by dispersing the particles of the core particle powder of the highly dispersed core particle powder / gas mixture dispersed in this dispersing step into the air with this dispersion performance. Aerial dispersion maintaining means for maintaining the aerial dispersion state of the particles of the core particle powder of the mixture, and an aerial state for enhancing the aerial dispersion state of the particles of the core particle powder of the particles / gas mixture of the highly dispersed core particle powder. The dispersion promoting means separates the low-dispersion core particle powder particles / gas mixture in the mixture of the core particle powder particles and the gas, and the core particle powder particles are present in the air mainly in a single particle state. A transporting step of transporting through one or more types of high-dispersion core particle powder particle / gas mixture selecting means for selecting a particle / gas mixture of high-dispersion core particle powder;
(C) The particles of the highly dispersed core particle powder and the particles of the core particle powder of the gas mixture conveyed in this conveyance step are
When the average particle diameter is more than 10 μm and 20 μm or less, the degree of dispersion β is 80% or more,
When it exceeds 20 μm and is 50 μm or less, the degree of dispersion β is 90% or more,
When it exceeds 50 μm and is 300 μm or less, the degree of dispersion β is 95% or more,
When it exceeds 300 μm and is 800 μm or less, the degree of dispersion β is 97% or more,
When it exceeds 800 μm, the degree of dispersion β is 99% or more,
In a dispersed state of, a coating step of starting coating by contacting and / or colliding with a coating forming substance precursor in a coating starting area of a coating space,
Coating method provided with.
[0103]
As described above, in all of 1 to V, preferably, the average particle diameter in the volume-based frequency distribution is more than 10 μm particles of the quasi-fine particle core particle powder of 20 μm or less or particles of the core particle powder mainly consisting of quasi-fine particles. A spatial region in which the degree of dispersion β of the particles of the core particle powder of the highly dispersed core particle powder / gas mixture dispersed by the quasi-fine particle high dispersion processing means group is 80% or more;
Particles of a quasi-fine particle core particle powder having an average particle diameter of more than 20 μm and not more than 50 μm in a volume-based frequency distribution or particles of a core particle powder mainly composed of quasi-fine particles are dispersed by a quasi-fine particle high dispersion treatment means group. A spatial region in which the degree of dispersion β of the particles of the dispersed core particle powder and the particles of the core particle powder of the gas mixture achieves 90% or more,
Particles of a quasi-fine particle core particle powder having an average particle diameter of more than 50 μm and not more than 300 μm in a volume-based frequency distribution or particles of a core particle powder mainly composed of quasi-fine particles are dispersed by a quasi-fine particle high dispersion treatment means group. A spatial region in which the degree of dispersion β of the particles of the dispersed core particle powder / particles of the core particle powder of the gas mixture is 95% or more;
Particles of a quasi-fine particle core particle powder having an average particle diameter of more than 300 μm and 800 μm or less in a volume-based frequency distribution or particles of a core particle powder mainly composed of quasi-fine particles are dispersed by a quasi-fine particle high dispersion treatment means group. A spatial region in which the degree of dispersion β of the particles of the dispersed core particle powder and the particles of the core particle powder of the gas mixture is 97% or more,
Highly dispersed core particles obtained by dispersing particles of a quasi-fine particle core particle powder having an average particle diameter exceeding 800 μm in a volume-based frequency distribution or particles of a core particle powder mainly consisting of quasi-fine particles by a quasi-fine particle high dispersion treatment means group Powder particles / core particles of gas mixture Particles of highly dispersed core particles / core particles in the gas mixture within the space region where the degree of dispersion β of the particles of the powder is 99% or more is realized. In the space area including the surface through which all the particles pass, the coating start area of the coating space is located, or
Particles of a quasi-fine particle core particle powder having an average particle diameter of more than 10 μm and not more than 20 μm in a volume-based frequency distribution or particles of a core particle powder mainly composed of quasi-fine particles are dispersed by a quasi-fine particle high dispersion treatment means group. A spatial region in which the degree of dispersion β of the particles of the core particle powder of the dispersed core particle powder / gas mixture realizes 80% or more,
Particles of a quasi-fine particle core particle powder having an average particle diameter of more than 20 μm and not more than 50 μm in a volume-based frequency distribution or particles of a core particle powder mainly composed of quasi-fine particles are dispersed by a quasi-fine particle high dispersion treatment means group. A spatial region in which the degree of dispersion β of the particles of the dispersed core particle powder and the particles of the core particle powder of the gas mixture achieves 90% or more,
Particles of a quasi-fine particle core particle powder having an average particle diameter of more than 50 μm and not more than 300 μm in a volume-based frequency distribution or particles of a core particle powder mainly composed of quasi-fine particles are dispersed by a quasi-fine particle high dispersion treatment means group. A spatial region in which the degree of dispersion β of the particles of the dispersed core particle powder / particles of the core particle powder of the gas mixture is 95% or more;
Particles of a quasi-fine particle core particle powder having an average particle diameter of more than 300 μm and 800 μm or less in a volume-based frequency distribution or particles of a core particle powder mainly composed of quasi-fine particles are dispersed by a quasi-fine particle high dispersion treatment means group. A spatial region in which the degree of dispersion β of the particles of the dispersed core particle powder and the particles of the core particle powder of the gas mixture is 97% or more,
Highly dispersed core particles obtained by dispersing particles of a quasi-fine particle core particle powder having an average particle diameter exceeding 800 μm in a volume-based frequency distribution or particles of a core particle powder mainly consisting of quasi-fine particles by a quasi-fine particle high dispersion treatment means group Spatial region in which the degree of dispersion β of the particles of the powder particles and the core particles of the gas mixture is 99% or more.
In this method, the coating start area of the coating space is located in a space area including a surface through which all the particles pass through the collection section of the collection means.
[0104]
Or, in the above I and II, preferably
Particles of a quasi-fine particle core particle powder having an average particle diameter of more than 10 μm and not more than 20 μm in a volume-based frequency distribution or particles of a core particle powder mainly composed of quasi-fine particles are dispersed by a quasi-fine particle high dispersion treatment means group. A group of quasi-fine particle high dispersion processing means for achieving a dispersion degree β of 80% or more of the particles of the core particle powder of the dispersed core particle powder / gas mixture,
Particles of a quasi-fine particle core particle powder having an average particle diameter of more than 20 μm and not more than 50 μm in a volume-based frequency distribution or particles of a core particle powder mainly composed of quasi-fine particles are dispersed by a quasi-fine particle high dispersion treatment means group. A group of quasi-fine particle high dispersion processing means for realizing a degree of dispersion β of 90% or more of the particles of the core particle powder of the dispersed core particle powder and the gas mixture,
Particles of a quasi-fine particle core particle powder having an average particle diameter of more than 50 μm and not more than 300 μm in a volume-based frequency distribution or particles of a core particle powder mainly composed of quasi-fine particles are dispersed by a quasi-fine particle high dispersion treatment means group. A group of quasi-fine particle high dispersion processing means for realizing a degree of dispersion β of 95% or more of the particles of the core particle powder of the dispersed core particle powder / gas mixture,
Particles of a quasi-fine particle core particle powder having an average particle diameter of more than 300 μm and 800 μm or less in a volume-based frequency distribution or particles of a core particle powder mainly composed of quasi-fine particles are dispersed by a quasi-fine particle high dispersion treatment means group. A group of quasi-fine particle high dispersion processing means for realizing a degree of dispersion β of 97% or more of particles of the core particle powder of the dispersed core particle powder / gas mixture,
Highly dispersed core particles obtained by dispersing particles of a quasi-fine particle core particle powder having an average particle diameter exceeding 800 μm in a volume-based frequency distribution or particles of a core particle powder mainly consisting of quasi-fine particles by a quasi-fine particle high dispersion treatment means group A group of quasi-fine particle high dispersion processing means for realizing a dispersion degree β of 99% or more of the particles of the powder particles / core particles of the gas mixture,
In this case, at least a part of the dispersing step of dispersing in the air to form a particle / gas mixture of the highly dispersed core particle powder and at least a part of the coating step are performed by sharing at least a part of the space.
[0105]
The invention will now be described in more detail by way of examples.
[0106]
Example 1
Hereinafter, a detailed description will be given based on FIG. 6 as a specific example of the device having the configuration shown in FIG. 5A and the embodiment of the present invention shown in FIG. 7 which is a partially enlarged view of FIG.
[0107]
The apparatus of this example includes a plasma torch 3-A, a plasma chamber 3-a, a cooling tank 3-B for a coating-forming substance precursor generation chamber, a coating-forming substance precursor generation chamber 3-b, and a coating
[0108]
The quasi-fine particle high dispersion processing means group α is composed of a
[0109]
The plasma torch 3-A is mainly composed of, for example, a quartz tube having an inner diameter of 44 mm and a length of 200 mm, a coil for high-frequency oscillation is mounted on the outside, and a jacket tube for cooling is provided on the outside. A
The lower portion of the plasma torch 3-A is provided with a
[0110]
The coating-forming substance precursor generation chamber 3-b includes a quartz tube having an inner diameter of 120 mm and a length of 200 mm, and a cooling jacket tube 3-B outside the quartz tube.
The coating chamber 3-c in a narrow sense includes an inner tube having an inner diameter of 120 mm and a length of 100 mm, and a cooling outer tube 3-C outside the inner tube. In the coating chamber 3-c in a narrow sense, the core particles supplied from the
The coated quasi-fine particle cooling chamber 3-d includes a tube 116 having an inner diameter of 440 mm and a length of 800 mm, and a cooling outer tube 3-D outside the tube 116.
The
[0111]
According to the apparatus for producing coated quasi-fine particles of the example of the present invention, DM= 40 μm ([DM/ 5, 5DM], ≧ 90%) distribution of diamond quasi-fine particles were coated with silicon oxide as a coating-forming substance.
Argon gas is supplied at a rate of 20 liters / minute from a
[0112]
The silicon oxide powder, which is a raw material of the coating forming material, supplied from the
[0113]
The diamond core particles supplied at 1.5 g / min from the
[0114]
The quasi-fine particle high dispersion processing means group α composed of the
[0115]
The coated quasi-fine particles, the surface of which is coated with the coating forming substance, generated in this manner, descend along with the gas in the coating quasi-fine particle cooling chamber 3-d, and reach the coating quasi-fine particle recovery unit 3-G. The product composed of the coated quasi-fine particles is separated from the gas by the
[0116]
Observation of the obtained coated quasi-fine particles, diamond quasi-fine particles, the surface of which was coated with silicon oxide, was observed with a scanning electron microscope. As shown in FIG. It was coated in the form of ultrafine particles.
[0117]
Comparative example
This embodiment uses an apparatus having the same configuration as the apparatus used in this embodiment except that the dispersion means is not provided and the quasi-fine particle powder is directly introduced from the
[0118]
Example 2
The device shown in FIG. 10 and FIG. 11, which is a partially enlarged view thereof, is one specific example of the device having the configuration shown in FIG.
[0119]
The configuration of the apparatus for generating the coating forming substance precursor of this example is the same as that of the first embodiment. The quasi-fine particle high dispersion processing means group α is composed of a
[0120]
With the apparatus for producing coated quasi-fine particles of this example, volume-based average particle diameter DM= 200 μm ([DM/ 5, 5DM], ≧ 90%) distribution of aluminum oxide quasi-fine particles were coated with metallic aluminum as a coating-forming substance.
A
[0121]
Metal aluminum powder, which is a raw material of the coating forming material and is supplied at a rate of 0.5 g / min from a
[0122]
The core particles of aluminum oxide supplied at 2.0 g / min from the
The coated quasi-fine particles, the surface of which is coated with the coating forming substance, generated in this manner, descend with the gas in the coating quasi-fine particle cooling chamber 5-d, and reach the coated quasi-fine particle recovery unit 5-G. The product composed of the coated quasi-fine particles is separated from the gas by the
[0123]
The obtained coated quasi-fine particles, the aluminum oxide quasi-fine particles whose surface was coated with metallic aluminum, were observed by a scanning electron microscope, and were obtained by coating the individual aluminum oxide quasi-fine particles as primary particles with metallic aluminum. . The coating configuration was similar to that obtained in Example 1.
[0124]
Example 3
The device shown in FIG. 12 and FIG. 13 which is a partially enlarged view thereof is a specific example of the device having the configuration shown in FIG. 5B.
[0125]
The configuration of the apparatus for generating the coating forming substance precursor of this example is the same as that of the first embodiment. The quasi-fine particle high dispersion processing means group α includes a
[0126]
With the apparatus for producing coated quasi-fine particles of this example, DM= 15 μm ([DM/ 5, 5DM], ≧ 90%). The particles of the quasi-fine particle powder of cubic boron nitride having a distribution were coated with metallic aluminum as a coating-forming substance.
Argon gas is supplied at a rate of 20 liters / minute from a
[0127]
Metal aluminum powder, which is a raw material of the coating forming material and supplied at a rate of 0.5 g / min from a
[0128]
Core particles of cubic boron nitride supplied at 1.7 g / min from a
The coated quasi-fine particles, the surface of which is coated with the coating forming substance, generated in this manner, descend along with the gas in the coating quasi-fine particle cooling chamber 6-d, and reach the coated quasi-fine particle recovery unit 6-G. The product composed of the coated quasi-fine particles is separated from the gas by the
[0129]
The obtained quasi-fine particles, cubic boron nitride quasi-fine particles whose surface was coated with metallic aluminum, were observed with a scanning electron microscope. As a result, individual cubic boron nitride quasi-fine particles as primary particles were coated with metallic aluminum. It was done. The coating form was the same as in Example 1.
[0130]
【The invention's effect】
According to the method and apparatus for producing coated quasi-fine particles of the present invention, even if the particles are quasi-fine particle core particles or particles of core particle powder mainly composed of quasi-fine particles, it is possible to coat the individual particles with the coating forming substance. In addition, the generation of uncoated particles or particles having uncoated by forming a coated aggregate in which the surface of the aggregate is coated with the coating forming substance is eliminated. As a result, uncoated core particles or core particles having an uncoated portion do not exist, and the merit in industrial production is extremely large.
[Brief description of the drawings]
FIG. 1 is a distribution diagram of powder particles, wherein (a) represents the original degree of dispersion β, and (b) represents the particle diameter D.1~ DTwoRepresents the particle size of powder occupying 90% by volume of particles in the range vs. frequency based on volume.
FIGS. 2A to 2C are block diagrams showing a basic configuration of a group of quasi-fine particle high dispersion processing means.
FIGS. 3A to 3G are block diagrams for explaining the configuration of a quasi-fine particle high dispersion processing means group in more detail.
FIGS. 4 (a) to 4 (e) are views showing a mode in which coating of core particle powder is started.
FIGS. 5A to 5G are block diagrams illustrating the configuration of an apparatus according to the present invention.
FIG. 6 is a diagram showing an apparatus according to the first embodiment.
FIG. 7 is a partially enlarged view of the apparatus according to the first embodiment.
FIG. 8 is a scanning electron micrograph of the coated quasi-fine particles obtained by the apparatus of Example 1.
FIG. 9 is a scanning electron micrograph of the coated quasi-fine particles obtained in Comparative Example.
FIG. 10 is a diagram showing an apparatus according to a second embodiment.
FIG. 11 is a partially enlarged view of the device of the second embodiment.
FIG. 12 is a diagram showing an apparatus according to a third embodiment.
FIG. 13 is a partially enlarged view of the device according to the third embodiment.
Claims (7)
前記高分散粒子・気体混合物を被覆空間に投入し、気相を経て生成する被覆形成物質前駆体及び／又は気相状態の被覆形成物質前駆体と接触及び／又は衝突させて前記芯粒子粉体の粒子表面を被覆する被覆工程とからなることを特徴とする、被覆準微粒子の製造方法。Core particle powder having an average particle diameter of more than 10 μm and 20 μm or less in a volume-based frequency distribution composed of quasi-fine particles is dispersed in the air, and the degree of dispersion β present in the air mainly in a single particle state is 80% or more. A dispersing step of forming a highly dispersed particle / gas mixture of
Charging the high-dispersion particles / gas mixture into a coating space, and contacting and / or colliding with a coating-forming substance precursor generated via a gaseous phase and / or a coating-forming substance precursor in a gaseous state to form the core particle powder; A method for producing coated quasi-fine particles, characterized by comprising a coating step of coating the surface of the particles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21926993A JP3545784B2 (en) | 1993-08-12 | 1993-08-12 | Method for producing coated quasi-fine particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21926993A JP3545784B2 (en) | 1993-08-12 | 1993-08-12 | Method for producing coated quasi-fine particles |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0754006A JPH0754006A (en) | 1995-02-28 |
| JP3545784B2 true JP3545784B2 (en) | 2004-07-21 |
Family
ID=16732882
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP21926993A Expired - Fee Related JP3545784B2 (en) | 1993-08-12 | 1993-08-12 | Method for producing coated quasi-fine particles |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3545784B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20200179821A1 (en) * | 2015-04-13 | 2020-06-11 | Virginia Tech Intellectual Properties, Inc. | Apparatus for Dewatering and Demineralization of Fine Particles |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20080032083A (en) * | 2005-06-10 | 2008-04-14 | 시바 스페셜티 케미칼스 홀딩 인크. | Process for the treatment of particles using a plasma torch |
| US8642139B2 (en) * | 2009-06-09 | 2014-02-04 | Toyota Motor Engineering & Manufacturing North America, Inc. | Process to make structured particles |
| JP2014185382A (en) * | 2013-03-25 | 2014-10-02 | Atsumi Tec:Kk | Nano particle discriminating apparatus |
| DE102015116351A1 (en) | 2015-09-28 | 2017-03-30 | Von Ardenne Gmbh | Method for substrate coating with particles and apparatus for carrying out the method |
| JP7013062B1 (en) * | 2021-10-14 | 2022-01-31 | 株式会社クリエイティブコーティングス | Powder film formation method and equipment |
-
1993
- 1993-08-12 JP JP21926993A patent/JP3545784B2/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20200179821A1 (en) * | 2015-04-13 | 2020-06-11 | Virginia Tech Intellectual Properties, Inc. | Apparatus for Dewatering and Demineralization of Fine Particles |
| US11752451B2 (en) * | 2015-04-13 | 2023-09-12 | Virginia Tech Intellectual Properties, Inc. | Method for dewatering and demineralization of fine particles |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0754006A (en) | 1995-02-28 |
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