JP2002266002A - Metallic fine particle-containing composition and producing method therefor - Google Patents
Metallic fine particle-containing composition and producing method thereforInfo
- Publication number
- JP2002266002A JP2002266002A JP2001069491A JP2001069491A JP2002266002A JP 2002266002 A JP2002266002 A JP 2002266002A JP 2001069491 A JP2001069491 A JP 2001069491A JP 2001069491 A JP2001069491 A JP 2001069491A JP 2002266002 A JP2002266002 A JP 2002266002A
- Authority
- JP
- Japan
- Prior art keywords
- metal
- fine particles
- copper
- containing composition
- fine particle
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、表面部分を高分子
化合物（樹脂）で被覆した金属微粒子を含有する組成物
およびその製造方法に関する。The present invention relates to a composition containing fine metal particles whose surface is coated with a polymer compound (resin) and a method for producing the same.
【０００２】この金属微粒子含有組成物は、電子材料、
光学材料、磁性材料や触媒などとして利用される。電子
材料としては、プリント配線板の回路パターン形成、各
種ビアホールの導体形成や微細部品の接合などの際に用
いられる。[0002] The composition containing fine metal particles comprises an electronic material,
It is used as an optical material, a magnetic material, a catalyst, and the like. As an electronic material, it is used for forming a circuit pattern of a printed wiring board, forming conductors for various via holes, joining fine parts, and the like.
【０００３】[0003]
【従来の技術】従来、蒸発室および回収室を備えた装置
で、次の手順により金属微粒子含有組成物を製造してい
る。 （１）装置内部（蒸発室および回収室）を１０-6torrま
で減圧する。 （２）ヘリウムガスを蒸発室に導入してそのガス圧を１
torrに保持する。 （３）α−テルピネオールの蒸気を回収室に導入しなが
ら、蒸発室のるつぼ内の例えば銅を高周波誘導加熱手段
で加熱して銅蒸気を発生させる。この銅蒸気は真空ポン
プの排気作用によって回収室に移送される。 （４）回収室の冷却板上に銅微粒子を沈積させる。2. Description of the Related Art Conventionally, an apparatus having an evaporation chamber and a recovery chamber has been used to produce a composition containing fine metal particles according to the following procedure. (1) The pressure inside the apparatus (evaporation chamber and recovery chamber) is reduced to 10 -6 torr. (2) Helium gas is introduced into the evaporation chamber and the gas pressure is reduced to 1
Hold in torr. (3) While introducing α-terpineol vapor into the recovery chamber, for example, copper in the crucible in the evaporation chamber is heated by high-frequency induction heating means to generate copper vapor. This copper vapor is transferred to the recovery chamber by the evacuation action of the vacuum pump. (4) deposit copper fine particles on the cooling plate of the collection chamber;
【０００４】蒸発室から回収室へと進んだ銅蒸気は、α
−テルピネオールの蒸気と混合した状態で冷やされて冷
却板上に銅微粒子ペースト（銅微粒子含有組成物）のか
たちで回収される。[0004] The copper vapor that has progressed from the evaporation chamber to the recovery chamber is α
-Cooled while mixed with terpineol vapor and collected on a cooling plate in the form of a copper fine particle paste (copper fine particle-containing composition).
【０００５】この銅微粒子含有組成物は、銅微粒子がα
−テルピネオールの有機溶媒で捕集された状態になって
いる。[0005] In the composition containing copper fine particles, the copper fine particles have α
It is trapped in the organic solvent of terpineol.
【０００６】[0006]
【発明が解決しようとする課題】従来の金属微粒子含有
組成物の場合、有機化合物（有機溶媒）の中に金属微粒
子がいわば分散しているだけにすぎず、当該組成物の高
濃度化や長期的保存の点で安定性に欠けるという問題点
があった。In the case of the conventional composition containing fine metal particles, the fine metal particles are merely dispersed in an organic compound (organic solvent), so to speak. There is a problem that stability is lacking in terms of preservation.
【０００７】そこで、本発明では、金属微粒子の表面を
高分子化合物で安定的に被覆し、この被覆部分から酸素
が入り込みにくいようにして、金属微粒子同士の凝集が
ほとんど生じず、酸化に対してより安定な金属微粒子含
有組成物を提供することを目的とする。Therefore, in the present invention, the surface of the metal fine particles is stably coated with a polymer compound so that oxygen does not easily enter from the coated portion, so that aggregation of the metal fine particles hardly occurs and oxidation is prevented. It is an object of the present invention to provide a more stable composition containing metal fine particles.
【０００８】[0008]
【課題を解決するための手段】本発明はこの課題を次の
ようにして解決する。 （１）減圧した不活性ガス雰囲気下で、金属を蒸発させ
て、この金属蒸気にモノマーの蒸気を混合することによ
り、当該金属の微粒子表面に付着する当該モノマーが重
合して高分子被膜を形成した金属微粒子からなる組成物
（金属微粒子含有組成物）を製造する。 （２）上記（１）において、金、銀、銅、白金、パラジ
ウム、ロジウム、オスミウム、ルテニウム、イリジウ
ム、鉄、錫、亜鉛、コバルト、ニッケル、クロム、チタ
ン、タンタル、タングステン、インジウム、ケイ素の中
の少なくとも１種類の金属、または２種類以上の金属か
らなる合金を用いる。The present invention solves this problem as follows. (1) In a reduced pressure inert gas atmosphere, the metal is evaporated, and the metal vapor is mixed with the vapor of the monomer, whereby the monomer adhering to the fine particle surface of the metal is polymerized to form a polymer film. A composition (metal-particle-containing composition) composed of the thus-prepared metal fine particles is produced. (2) In the above (1), gold, silver, copper, platinum, palladium, rhodium, osmium, ruthenium, iridium, iron, tin, zinc, cobalt, nickel, chromium, titanium, tantalum, tungsten, indium, and silicon Of at least one metal or an alloy composed of two or more metals.
【０００９】本発明によれば、金、銀、銅などの上記金
属またはこれらの合金の蒸気と、モノマー（有機化合
物）の蒸気とを混合し、当該金属微粒子の表面で当該モ
ノマーの重合反応を進行させて、当該表面を高分子化合
物（樹脂）で安定的に被覆している。According to the present invention, the vapor of the above metal such as gold, silver, copper or the like or the alloy of these metals and the vapor of the monomer (organic compound) are mixed, and the polymerization reaction of the monomer is carried out on the surface of the metal fine particles. By proceeding, the surface is stably covered with the polymer compound (resin).
【００１０】この高分子被膜で表面を被覆された金属微
粒子は、互いに凝集せずに、安定な微粒子の状態で捕集
される。The fine metal particles whose surfaces are coated with the polymer film are collected in a stable fine particle state without aggregating with each other.
【００１１】[0011]
【発明の実施の形態】以下、本発明の実施の形態を説明
する。図１は、金属微粒子含有組成物の製造装置を示す
説明図である。Embodiments of the present invention will be described below. FIG. 1 is an explanatory diagram showing an apparatus for producing a metal fine particle-containing composition.
【００１２】ここで、１は蒸発室，２は処理対象金属を
入れるためのるつぼ，３はるつぼ２を加熱するための高
周波誘導加熱手段，４は不活性ガスを蒸発室１に導入す
るためのバルブ，５は回収室，６は冷却装置（図示省
略）で低温に保持した冷却部，７はモノマー類の蒸気
と、不活性ガスとを回収室５に導入するためのバルブ，
８は蒸発室１および回収室５を真空ポンプ（図示省略）
により排気するためのバルブ，９は冷却部６に捕集され
た金属微粒子含有組成物，をそれぞれ示している。Here, 1 is an evaporation chamber, 2 is a crucible for containing a metal to be treated, 3 is a high-frequency induction heating means for heating the crucible 2, and 4 is a gas for introducing an inert gas into the evaporation chamber 1. A valve 5 for a recovery chamber, 6 a cooling unit maintained at a low temperature by a cooling device (not shown), 7 a valve for introducing vapors of monomers and an inert gas into the recovery chamber 5,
Reference numeral 8 denotes a vacuum pump (not shown) for the evaporation chamber 1 and the recovery chamber 5
The reference numeral 9 denotes a metal particle-containing composition collected in the cooling unit 6.
【００１３】図２は、金属微粒子含有組成物の製造手順
を示す説明図であり、その内容は次のようになってい
る。 （ｓ１１）るつぼの中に銅を入れる。 （ｓ１２）バルブ４，７を閉じ、バルブ８を開いて真空
ポンプを作動させ、蒸発室１および回収室５の圧力を１
×１０-3〜１×１０-6torrまで下げる。 （ｓ１３）バルブ４を開き、アルゴンガスを蒸発室１に
導入してその圧力を１〜１００torrに保つ。 （ｓ１４）バルブ７を開いてアルゴンガスとアクリロニ
トリルモノマーとの混合蒸気を回収室５に導入しなが
ら、るつぼ２を高周波誘導加熱手段３で加熱して、銅の
蒸気を発生させる。 （ｓ１５）銅微粒子含有組成物９を冷却部６に捕集す
る。FIG. 2 is an explanatory view showing the procedure for producing the metal fine particle-containing composition, and the contents are as follows. (S11) Put copper in the crucible. (S12) The valves 4 and 7 are closed, the valve 8 is opened, and the vacuum pump is operated to reduce the pressure in the evaporation chamber 1 and the recovery chamber 5 to 1
× 10 -3 to 1 × 10 -6 torr. (S13) The valve 4 is opened, and argon gas is introduced into the evaporation chamber 1 to maintain the pressure at 1 to 100 torr. (S14) The crucible 2 is heated by the high frequency induction heating means 3 while the mixed gas of the argon gas and the acrylonitrile monomer is introduced into the recovery chamber 5 by opening the valve 7 to generate copper vapor. (S15) The copper fine particle-containing composition 9 is collected in the cooling unit 6.
【００１４】るつぼ２の加熱温度は約１０００〜１８０
０℃に設定し、冷却部６の温度は約０〜２０℃に設定す
る。また、上記（ｓ１３）〜（ｓ１５）の間も真空ポン
プで回収室５および蒸発室１を排気する。The heating temperature of the crucible 2 is about 1000 to 180
The temperature is set to 0 ° C., and the temperature of the cooling unit 6 is set to about 0 to 20 ° C. In addition, the collection chamber 5 and the evaporating chamber 1 are evacuated by the vacuum pump during the above (s13) to (s15).
【００１５】蒸発室１のるつぼ２で発生した銅蒸気は、
バルブ８を介したこの排気作用により回収室５へと進ん
でアクリロニトリルモノマーの蒸気（およびアルゴンガ
ス）との混合ガスとなる。The copper vapor generated in the crucible 2 of the evaporation chamber 1 is
This exhaust action via the valve 8 leads to the recovery chamber 5 where it becomes a mixed gas with acrylonitrile monomer vapor (and argon gas).
【００１６】この混合ガスは冷却部６に到達し、このと
きの冷却部近傍を含む空間領域での冷却作用によって、
銅微粒子が冷却部６に析出する。This mixed gas reaches the cooling unit 6 and at this time, by the cooling action in the space region including the vicinity of the cooling unit,
Copper fine particles precipitate in the cooling unit 6.
【００１７】析出した銅微粒子の表面に、アクリロニト
リルが付着する。当該表面を被覆したアクリロニトリル
モノマーは銅の触媒作用を受け、また析出した銅微粒子
の温度が高いので、当該モノマーの重合が進行する。Acrylonitrile adheres to the surface of the precipitated copper fine particles. The acrylonitrile monomer coated on the surface is catalyzed by copper, and the temperature of the precipitated copper fine particles is high, so that the polymerization of the monomer proceeds.
【００１８】この重合作用によって、銅微粒子の表面
は、ガスバリア性を有する高分子化合物（ポリアクリロ
ニトリル）で被覆される。By this polymerization action, the surface of the copper fine particles is coated with a polymer compound having a gas barrier property (polyacrylonitrile).
【００１９】冷却部６において銅微粒子を回収する際、
予め冷却部６に有機溶剤を添加しておくことにより銅微
粒子含有組成物分散液として回収することが好ましい。When recovering the copper fine particles in the cooling section 6,
It is preferable that an organic solvent is added to the cooling section 6 in advance to recover the composition as a dispersion liquid containing fine copper particles.
【００２０】上記の有機溶剤としてはヘキサン、イソオ
クタンなどの脂肪族炭化水素、トルエン、キシレンなど
の芳香族炭化水素、オクタノール、ドデシルアルコー
ル、ターピネオールなどのアルコール類、オクチルアミ
ン、ドデシルアミンなどのアミン類などが挙げられる。Examples of the organic solvent include aliphatic hydrocarbons such as hexane and isooctane, aromatic hydrocarbons such as toluene and xylene, alcohols such as octanol, dodecyl alcohol and terpineol, and amines such as octylamine and dodecylamine. Is mentioned.
【００２１】冷却部６の銅微粒子含有組成物９は、この
被覆された銅微粒子が互いに凝集せずに、安定な微粒子
の状態になっている。冷却部６で得られる銅微粒子は球
状でその平均粒径は0.1〜10nmであった。The copper fine particle-containing composition 9 in the cooling section 6 is in a state of stable fine particles without the coated copper fine particles aggregating with each other. The copper fine particles obtained in the cooling section 6 were spherical and had an average particle diameter of 0.1 to 10 nm.
【００２２】本発明が銅以外の上述の各種金属や合金も
対象とすることは勿論である。回収室５に導入するモノ
マーは重合を起こしやすい有機化合物であればよく、例
えば、アクリル酸、アクリル酸エステル、メタクリル
酸、メタクリル酸エステル、エチレン、プロピレン、ス
チレン、塩化ビニル、塩化ビニリデン、アクリロニトリ
ル、アクリルアミド、酢酸ビニル、ビニルピロリドンな
どの中から選ばれる１種または２種以上を用いることが
できる。また、ヘリウム、窒素などアルゴン以外の不活
性ガスを用いてもよい。It goes without saying that the present invention covers the above-mentioned various metals and alloys other than copper. The monomer to be introduced into the recovery chamber 5 may be any organic compound that easily undergoes polymerization, for example, acrylic acid, acrylic acid ester, methacrylic acid, methacrylic acid ester, ethylene, propylene, styrene, vinyl chloride, vinylidene chloride, acrylonitrile, acrylamide , Vinyl acetate, vinyl pyrrolidone and the like. Further, an inert gas other than argon, such as helium or nitrogen, may be used.
【００２３】また、排気用バルブ８や冷却部６の設置場
所・個数は図示のものに限定されず、例えば回収室５の
内面を冷却部として用いるようにしてもよい。The location and number of the exhaust valve 8 and the cooling unit 6 are not limited to those shown in the figure. For example, the inner surface of the collection chamber 5 may be used as a cooling unit.
【００２４】また、回収室５を設けずに、蒸発室１に有
機化合物を導入してこの室内で銅微粒子含有組成物９を
回収するようにしてもよい。Alternatively, without providing the recovery chamber 5, an organic compound may be introduced into the evaporation chamber 1 and the copper fine particle-containing composition 9 may be recovered in this chamber.
【００２５】[0025]
【発明の効果】本発明は、金属微粒子の表面を高分子化
合物（樹脂）で安定的に被覆し、この被覆部分から酸素
が入り込みにくいようにしているので、金属微粒子同士
の凝集がほとんど生じず、酸化に対してより安定な金属
微粒子含有組成物を提供することができる。According to the present invention, since the surface of the metal fine particles is stably coated with the polymer compound (resin) so that oxygen does not easily enter from the coated portion, aggregation of the metal fine particles hardly occurs. Thus, a composition containing fine metal particles that is more stable against oxidation can be provided.
【００２６】また、この金属微粒子含有組成物を、プリ
ント配線板の回路パターン形成、各種ビアホールの導体
形成や微細部品の接合などに用いることにより、微細回
路の描画性能、および当該回路パターンなどの導電率特
性、光学（透過）特性や接合強度特性などを改善するこ
とができる。The composition containing fine metal particles is used for forming a circuit pattern on a printed wiring board, forming conductors for various via holes, joining fine parts, and the like, thereby providing a fine circuit drawing performance and a conductive property for the circuit pattern. The ratio characteristics, optical (transmission) characteristics, bonding strength characteristics, and the like can be improved.
【図１】本発明の、金属微粒子含有組成物の製造装置を
示す説明図である。FIG. 1 is an explanatory view showing an apparatus for producing a metal fine particle-containing composition of the present invention.
【図２】本発明の、金属微粒子含有組成物の製造手順を
示す説明図である。FIG. 2 is an explanatory view showing a production procedure of a metal fine particle-containing composition of the present invention.
１：蒸発室 ２：るつぼ ３：高周波誘導加熱手段 ４：不活性ガス導入用のバルブ ５：回収室 ６：冷却部 ７：モノマー類の蒸気および不活性ガス導入用のバルブ ８：排気用のバルブ ９：冷却部に捕集された金属微粒子含有組成物 1: Evaporation chamber 2: Crucible 3: High frequency induction heating means 4: Valve for introducing inert gas 5: Recovery chamber 6: Cooling unit 7: Valve for introducing vapor of monomer and inert gas 8: Valve for exhaust 9: Composition containing fine metal particles collected in the cooling section
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｈ０１Ｂ 13/00 ５０１ Ｈ０１Ｂ 13/00 ５０１Ｚ (72)発明者 松葉 頼重 茨城県つくば市東光台五丁目９番の３ ハ リマ化成株式会社筑波研究所内 (72)発明者 山口 智彦 茨城県つくば市東１−１ 経済産業省産業 技術総合研究所物質工学工業技術研究所内 Ｆターム(参考） 4J037 AA04 AA06 CB01 CB04 CB16 CC12 CC13 CC14 CC15 CC16 EE03 EE23 FF02 FF11 4K018 BA01 BA02 BA03 BA04 BA09 BA13 BA20 BC30 BD04 BD10 5G301 DA03 DA05 DA06 DA07 DA10 DA11 DA12 DA13 DA14 DA15 DA42 DD10 ──────────────────────────────────────────────────の Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat ゛ (Reference) H01B 13/00 501 H01B 13/00 501Z (72) Inventor Yorige Matsuba 5-9 Tokodai, Tokodai, Tsukuba City, Ibaraki Prefecture No. 3 Harima Chemicals Co., Ltd. Tsukuba Research Laboratory (72) Inventor Tomohiko Yamaguchi 1-1 East Higashi, Tsukuba, Ibaraki Prefecture F-term in Material Engineering Industrial Technology Research Institute, AIST CC12 CC13 CC14 CC15 CC16 EE03 EE23 FF02 FF11 4K018 BA01 BA02 BA03 BA04 BA09 BA13 BA20 BC30 BD04 BD10 5G301 DA03 DA05 DA06 DA07 DA10 DA11 DA12 DA13 DA14 DA15 DA42 DD10
Claims (4)
合物で被覆した態様により分散している金属微粒子含有
組成物。1. A metal fine particle-containing composition in which metal fine particles are dispersed in a form in which the surface is coated with a polymer compound.
ウム、ロジウム、オスミウム、ルテニウム、イリジウ
ム、鉄、錫、亜鉛、コバルト、ニッケル、クロム、チタ
ン、タンタル、タングステン、インジウム、ケイ素の中
の少なくとも１種類の金属、または２種類以上の金属か
らなる合金である、ことを特徴とする請求項１記載の金
属微粒子含有組成物。2. The method according to claim 1, wherein the metal is gold, silver, copper, platinum, palladium, rhodium, osmium, ruthenium, iridium, iron, tin, zinc, cobalt, nickel, chromium, titanium, tantalum, tungsten, indium, or silicon. The metal fine particle-containing composition according to claim 1, wherein the composition is at least one kind of metal or an alloy composed of two or more kinds of metals.
蒸発させて、この金属蒸気に有機化合物の蒸気を混合す
ることにより、表面部分が当該有機化合物で被覆された
金属微粒子からなる組成物を製造する方法において、 前記混合の際の有機化合物としてアクリロニトリルなど
のモノマーを用い、前記金属の微粒子表面に付着した前
記有機化合物が重合して当該表面部分の高分子被膜を形
成する、ことを特徴とする金属微粒子含有組成物の製造
方法。3. A composition comprising metal fine particles having a surface portion coated with an organic compound by evaporating a metal under a reduced pressure inert gas atmosphere and mixing the metal vapor with an organic compound vapor. In the method for producing, using a monomer such as acrylonitrile as the organic compound at the time of the mixing, the organic compound attached to the surface of the metal fine particles is polymerized to form a polymer film on the surface portion. Method for producing a metal fine particle-containing composition to be used.
ラジウム、ロジウム、オスミウム、ルテニウム、イリジ
ウム、鉄、錫、亜鉛、コバルト、ニッケル、クロム、チ
タン、タンタル、タングステン、インジウム、ケイ素の
中の少なくとも１種類の金属、または２種類以上の金属
からなる合金を用いる、ことを特徴とする請求項３記載
の金属微粒子含有組成物の製造方法。4. The metal includes gold, silver, copper, platinum, palladium, rhodium, osmium, ruthenium, iridium, iron, tin, zinc, cobalt, nickel, chromium, titanium, tantalum, tungsten, indium, and silicon. The method for producing a metal fine particle-containing composition according to claim 3, wherein an alloy comprising at least one kind of metal or two or more kinds of metals is used.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001069491A JP2002266002A (en) | 2001-03-12 | 2001-03-12 | Metallic fine particle-containing composition and producing method therefor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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