JP4909105B2 - Boron nitride containing slurry - Google Patents
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Description
本発明は、例えば真空蒸着室の内面にダミー壁を形成させるのに好適な、窒化硼素含有スラリーに関する。 The present invention relates to a boron nitride-containing slurry suitable for forming a dummy wall on the inner surface of a vacuum deposition chamber, for example.
窒化硼素と導電性物質（例えば硼化ジルコニウム）を含むセラミックス焼結体で構成された金属蒸発発熱体（ボート）は、例えばアルミニウム等の金属をプラスチックなどのフィルムに蒸着するのに用いられている。蒸着操作は、金属線材をボートに供給し、高真空下、３００〜４００℃に加熱して蒸発させ、それをボートの上方に置かれたフィルムに蒸着させることによって行われる。この蒸着操作によって、真空蒸着室の内面にも金属が沈着するのでほぼ毎回の蒸着ごとに除去される。しかし、金属が強固に付着しているので除去作業に多くの手間をとり蒸着フィルムの生産性を低下させていた。 A metal evaporation heating element (boat) composed of a ceramic sintered body containing boron nitride and a conductive material (for example, zirconium boride) is used to deposit a metal such as aluminum on a film such as plastic. . The vapor deposition operation is performed by supplying a metal wire to a boat, evaporating by heating to 300-400 ° C. under high vacuum, and depositing it on a film placed above the boat. By this vapor deposition operation, metal is deposited also on the inner surface of the vacuum vapor deposition chamber, so that it is removed almost every vapor deposition. However, since the metal is firmly attached, much work is required for the removal work, and the productivity of the deposited film is lowered.
そこで、真空蒸着室の内面に窒化硼素と増粘剤を含有するスラリーを塗布することが提案されたが（特許文献１）、増粘剤が強固に付着した。増粘剤を使用せずに、窒化硼素粉末の結晶性の違いによる増粘作用を利用したスラリー（特許文献２）では、今度は窒化硼素が強固に付着することがあった。このように、これまでのスラリーでは、金属か、増粘剤か、窒化硼素が真空蒸着室の内面に付着する場合があり改善の余地があった。
本発明の目的は、真空蒸着室内に、電気絶縁性に優れ、一段と剥離の容易なダミー壁を形成するのに好適なスラリーを提供することである。 An object of the present invention is to provide a slurry suitable for forming a dummy wall that is excellent in electrical insulation and is more easily peeled off in a vacuum deposition chamber.
本発明は、窒化硼素粉末を５〜３０質量％含有するラリーであって、窒化硼素粉末が、黒鉛化指数が３〜１５、酸化硼素含有量が０．５質量％未満、平均粒径が２０μｍ以下である窒化硼素粉末含有スラリーである。 The present invention is a rally containing 5 to 30% by mass of boron nitride powder, wherein the boron nitride powder has a graphitization index of 3 to 15, a boron oxide content of less than 0.5% by mass, and an average particle size of 20 μm. The following is a slurry containing boron nitride powder.
本発明においては、窒化硼素粉末が、（ａ）黒鉛化指数が５〜３０、酸化硼素含有率が０．５〜５質量％、比表面積が２０ｍ２／ｇ以上、平均粒径が１０μｍ以下、最大粒径が４０μｍ以下である窒化硼素粉末ａと、（ｂ）黒鉛化指数が５未満、酸化硼素含有率が０．５質量％未満、平均粒径が５〜３０μｍである窒化硼素粉末ｂとの混合窒化硼素粉末であり、（窒化硼素粉末ａ）／（窒化硼素粉末ｂ）の質量比が１〜２５であることが好ましい。また、真空蒸着室の内面にダミー壁を形成させるための窒化硼素含有スラリーであることが好ましい。 In the present invention, the boron nitride powder has (a) a graphitization index of 5 to 30, a boron oxide content of 0.5 to 5% by mass, a specific surface area of 20 m 2 / g or more, an average particle size of 10 μm or less, Boron nitride powder a having a maximum particle size of 40 μm or less; and (b) boron nitride powder b having a graphitization index of less than 5, boron oxide content of less than 0.5 mass%, and an average particle size of 5 to 30 μm. It is preferable that the mass ratio of (boron nitride powder a) / (boron nitride powder b) is 1 to 25. Moreover, it is preferable that it is a boron nitride containing slurry for forming a dummy wall in the inner surface of a vacuum evaporation chamber.
本発明のスラリーは、塗布作業が簡単でしかも塗布物は自然乾燥によって固化するので、真空蒸着室の内面にダミー壁等を容易に形成させることができる。このダミー壁等は、真空蒸着後に例えばハンマーで軽く叩く等の衝撃を加えることによって容易に剥離するので蒸着フィルムの生産性が向上する。 Since the slurry of the present invention is easy to apply and the applied material is solidified by natural drying, a dummy wall or the like can be easily formed on the inner surface of the vacuum deposition chamber. Since the dummy wall and the like are easily peeled off by applying an impact such as tapping with a hammer after vacuum deposition, productivity of the deposited film is improved.
本発明のスラリーは、増粘剤を用いないこと、窒化硼素粉末として黒鉛化指数が３〜１５、酸化硼素含有量が０．５質量％未満、平均粒径が２０μｍ以下のものを用いたこと、特に酸化硼素含有量が０．５質量％未満のものを用いたことが特徴である。増粘剤を用いると、増粘剤の成分が真空蒸着室の内面に強固に付着することがある。 The slurry of the present invention does not use a thickener, and uses boron nitride powder having a graphitization index of 3 to 15, boron oxide content of less than 0.5% by mass, and an average particle size of 20 μm or less. In particular, it is characterized in that the boron oxide content is less than 0.5% by mass. When a thickener is used, the thickener component may adhere firmly to the inner surface of the vacuum deposition chamber.
窒化硼素粉末の黒鉛化指数が３未満ではスラリーの粘度及びチクソ性の適正化が困難となり、１５をこえると、ダミー壁等を形成してもひび割れ、亀裂が生じやすくなる。好ましい黒鉛化指数は５〜１０ある。黒鉛化指数（ＧＩ）は、窒化硼素粉末のＸ線回折図の（１００）、（１０１）及び（１０２）回折線の積分強度比（つまり面積比)より、式、ＧＩ＝［面積｛（１００）＋（１０１）｝］／［面積（１０２）］、により算出できる（Ｊ．Ｔｈｏｍａｓ．ｅｔ．ａｌ，Ｊ．Ａｍ．Ｃｈｅｍ．Ｓｏｃ．，８４，４６１９［１９６２］）。 If the graphitization index of the boron nitride powder is less than 3, it is difficult to optimize the viscosity and thixotropy of the slurry, and if it exceeds 15, cracks and cracks are likely to occur even if a dummy wall or the like is formed. A preferred graphitization index is 5-10. The graphitization index (GI) is calculated from the integral intensity ratio (that is, area ratio) of (100), (101), and (102) diffraction lines in the X-ray diffraction diagram of boron nitride powder: GI = [area {(100 ) + (101)}] / [area (102)] (J. Thomas. Et.al, J. Am. Chem. Soc., 84, 4619 [1962]).
窒化硼素粉末の酸化硼素含有量が０．５質量％をこえるとダミー壁等からの剥離性が悪化する。好ましい酸化硼素含有量は０．４質量％以下である。酸化硼素含有率の測定は以下のようにして行う。精秤した試料５ｇ（Ａｇ）とメタノール１５ｍｌを５０ｍｌのガラス製ビーカーに採取し、液温５５〜５８℃に保ちながら３０秒間、ガラス棒を用い分析技術の常識範囲内でゆっくり攪拌する。得られた混合溶液を１２０℃で蒸発乾固して質量（Ｂｇ）を測定し、（Ａ−Ｂ）×１００／Ａ、により算出する。 When the boron oxide content of the boron nitride powder exceeds 0.5% by mass, the peelability from the dummy wall and the like deteriorates. A preferable boron oxide content is 0.4 mass% or less. The boron oxide content is measured as follows. Precisely weighed 5 g (Ag) of the sample and 15 ml of methanol are collected in a 50 ml glass beaker and slowly stirred for 30 seconds within a common sense of analytical techniques using a glass rod while maintaining the liquid temperature at 55-58 ° C. The obtained mixed solution is evaporated to dryness at 120 ° C., the mass (Bg) is measured, and it is calculated by (A−B) × 100 / A.
窒化硼素粉末の平均粒径が２０μｍをこえると、スラリー粘度の適正化が困難である。好ましい平均粒径は２〜１０μｍである。 When the average particle size of the boron nitride powder exceeds 20 μm, it is difficult to optimize the slurry viscosity. A preferable average particle diameter is 2 to 10 μm.
スラリー粘度を適正化し、かつダミー壁等の剥離性を向上させるためには、一種類の窒化硼素粉末では困難である。そこで物性の異なる窒化硼素粉末ａと窒化硼素粉末ｂとを、（窒化硼素粉末ａ）／（窒化硼素粉末ｂ）の質量比を１〜２５、特に５〜２３にして混合し、上記物性を満たす窒化硼素粉末を調達することが好ましい。 In order to optimize the slurry viscosity and improve the peelability of the dummy wall and the like, it is difficult to use one kind of boron nitride powder. Therefore, boron nitride powder a and boron nitride powder b having different physical properties are mixed at a mass ratio of (boron nitride powder a) / (boron nitride powder b) of 1 to 25, particularly 5 to 23, to satisfy the above physical properties. It is preferable to procure boron nitride powder.
窒化硼素粉末ａは主としてスラリー粘度の適正化を担う成分である。窒化硼素粉末ａの黒鉛化指数は５〜３０であることが好ましい。黒鉛化指数が３０よりも高いと、粉末同士のファンデルワールス力による結合が弱いのでスラリーの固化物が脆くなる。その結果、ダミー壁等を形成してもひび割れ、亀裂が生じやすくなる。一方、黒鉛化指数が５よりも低いと、スラリーのチクソ性が低く、塗工後のタレが発生し易くなる。特に好ましい黒鉛化指数は１０〜２０である。 The boron nitride powder a is a component mainly responsible for optimizing the slurry viscosity. The boron nitride powder a preferably has a graphitization index of 5 to 30. When the graphitization index is higher than 30, the solidified product of the slurry becomes brittle because the bonding between the powders by van der Waals force is weak. As a result, even if a dummy wall or the like is formed, cracks and cracks are likely to occur. On the other hand, if the graphitization index is lower than 5, the thixotropy of the slurry is low, and sagging after coating tends to occur. A particularly preferred graphitization index is 10-20.
窒化硼素粉末ａの酸化硼素含有率は０．５〜５質量％であることが好ましい。０．５質量％未満であると、スラリーのチクソ性が低く、塗工後のタレが発生し易くなり、５質量％をこえると、ダミー壁等の電気絶縁性が低下し蒸着時間が短くなる。特に好ましい酸化硼素含有率は０．５〜１．０質量％である。 The boron oxide content of the boron nitride powder a is preferably 0.5 to 5% by mass. If it is less than 0.5% by mass, the thixotropy of the slurry is low, and sagging after coating tends to occur. If it exceeds 5% by mass, the electrical insulation properties of the dummy walls and the like are reduced and the deposition time is shortened. . A particularly preferable boron oxide content is 0.5 to 1.0% by mass.
窒化硼素粉末ａの比表面積、平均粒径、粒度分布の極限値は、塗工性の良いスラリーを調製する観点から、比表面積が２０ｍ２／ｇ以上、平均粒径が１０μｍ以下、最大粒径が４０μｍ以下であることが好ましい。とくに、比表面積が３０〜７０ｍ２／ｇ、平均粒径が５μｍ以下、最大粒径が３０μｍ以下であることが好ましい。 The specific values of the specific surface area, average particle size, and particle size distribution of the boron nitride powder a are such that the specific surface area is 20 m 2 / g or more, the average particle size is 10 μm or less, and the maximum particle size from the viewpoint of preparing a slurry with good coatability. Is preferably 40 μm or less. In particular, the specific surface area is preferably 30 to 70 m 2 / g, the average particle size is 5 μm or less, and the maximum particle size is 30 μm or less.
窒化硼素粉末ｂはダミー壁等の剥離性の向上を担う成分である。窒化硼素粉末ｂの黒鉛化指数が５未満、酸化硼素含有率が０．５質量％以下、平均粒径が５〜５０μｍであることが好ましい。黒鉛化指数が５以上であると、結晶性が低いためダミー壁等の剥離性が低下する。特に好ましい黒鉛化指数は１．５未満である。酸化硼素含有率が０．５質量％をこえると、ダミー壁等の剥離性が不十分となる。特に好ましい酸化硼素含有率は０．３質量％以下である。平均粒径が５μｍ未満であると、一次粒子が小さすぎるため剥離性が不十分となり、３０μｍをこえると、粒子の大半が一次粒子の凝集体で構成されるため、これまた剥離性が低下する。好ましい平均粒径は５〜２０μｍである。 Boron nitride powder b is a component responsible for improving the peelability of dummy walls and the like. It is preferable that the boron nitride powder b has a graphitization index of less than 5, a boron oxide content of 0.5% by mass or less, and an average particle size of 5 to 50 μm. If the graphitization index is 5 or more, the crystallinity is low, so that the peelability of the dummy walls and the like is lowered. A particularly preferred graphitization index is less than 1.5. When the boron oxide content exceeds 0.5% by mass, the peelability of the dummy walls and the like becomes insufficient. A particularly preferable boron oxide content is 0.3% by mass or less. If the average particle size is less than 5 μm, the primary particles are too small and the releasability is insufficient, and if it exceeds 30 μm, the majority of the particles are composed of aggregates of primary particles, which also reduces the releasability. . A preferable average particle diameter is 5 to 20 μm.
本発明のスラリーの媒体は水及び有機媒体の少なくとも一方である。有機媒体としては、アルコール、直鎖炭化水素、芳香族炭化水素などが用いられる。スラリー中の窒化硼素粉末の含有率は５〜３０質量％が好ましく、特に１０〜２０質量％が好ましい。窒化硼素粉末の含有率が５質量％未満であると、沢山の重ね塗りをしないとダミー壁等を形成させることが容易でなく、またダミー壁等の電気絶縁性も小さくなる傾向がある。一方、３０質量％をこえると、塗工性が悪化し、またダミー壁等にひび割れが発生する恐れがある。スラリーの調製には、例えばスリーワンモーター、ボールミル、振動ミル、アトライターミル等の混合機が使用される。 The medium of the slurry of the present invention is at least one of water and an organic medium. As the organic medium, alcohol, linear hydrocarbon, aromatic hydrocarbon and the like are used. The content of boron nitride powder in the slurry is preferably 5 to 30% by mass, particularly preferably 10 to 20% by mass. If the content of boron nitride powder is less than 5% by mass, it is not easy to form dummy walls or the like unless a large amount of overcoating is performed, and the electrical insulation properties of the dummy walls and the like tend to be reduced. On the other hand, if it exceeds 30% by mass, the coatability deteriorates, and cracks may occur in the dummy wall and the like. For the preparation of the slurry, for example, a mixer such as a three-one motor, a ball mill, a vibration mill, or an attritor mill is used.
スラリーの粘度としては、真空蒸着室の側壁や天井等への塗工性の点から、１０〜１０００Ｐａ・ｓが好ましく、特に１００〜５００Ｐａ・ｓであることが好ましい。このような粘度は、ポリエチレングリコール等の有機物を積極的に添加することによって実現できる。 The viscosity of the slurry is preferably 10 to 1000 Pa · s, and particularly preferably 100 to 500 Pa · s, from the viewpoint of coating properties on the side wall or ceiling of the vacuum deposition chamber. Such a viscosity can be realized by positively adding an organic substance such as polyethylene glycol.
スラリーの塗工は、例えば刷毛塗り、へら塗り、スプレー塗布等によって行われ、塗布後の固化は、自然乾燥、２００℃以下の熱風をあてる強制乾燥のいずれでも可能である。 The slurry is applied by, for example, brush coating, spatula coating, spray coating, or the like. Solidification after coating can be performed by either natural drying or forced drying by applying hot air of 200 ° C. or less.
実施例１〜８ 比較例１〜7
黒鉛化指数、酸化硼素含有率、比表面積、平均粒径及び最大粒径が異なる３種の窒化硼素粉末（電気化学工業社製商品名「ＳＰ−２」、「ＳＧＰ」、「ＧＰ」）を所定量配合して混合窒化硼素粉末となし、アトライターミルを用い、蒸留水と３時間混合してスラリーを調製した。得られたスラリーの塗工性、タレ性及びダミー壁の剥離性を以下に従い評価した。それらの結果を表１に示す。
Examples 1-8 Comparative Examples 1-7
Three types of boron nitride powders (trade names “SP-2”, “SGP”, “GP” manufactured by Denki Kagaku Kogyo Co., Ltd.) having different graphitization indexes, boron oxide contents, specific surface areas, average particle diameters and maximum particle diameters A predetermined amount was mixed to form a boron nitride powder, and an attritor mill was used to mix with distilled water for 3 hours to prepare a slurry. The coating property, sagging property and peelability of the dummy wall of the obtained slurry were evaluated as follows. The results are shown in Table 1.
（１）塗工性
アルミニウム真空蒸着室の内壁の側壁に約１０ｍｍの厚さにスラリーを刷毛塗りし、塗布面積あたりの塗布量（塗布速度）を測定した。
（２）タレ性
アルミニウム真空蒸着室の天井面に５ｋｇ／ｍ２のスラリーを刷毛塗りし、１分間放置した際のタレ量を測定し、「優」：タレがない、「良」：タレ量が１０ｇ／ｍ２未満である、「不可」：タレ量が１０ｇ／ｍ２以上である、で評価した。
（３）剥離性
アルミニウム真空蒸着室の内側壁と天井面にスラリーを塗布した後、２時間自然乾燥させてダミー壁（厚み１０ｍｍ）を形成させた後、０．０１Ｐａに真空排気し、５ｇ／分の速度で５分間、アルミニウムを蒸発させた。この時、真空蒸着室の内側壁と天井面の温度は１３０〜１７０℃となった。その後、真空蒸着室を室温まで冷却し、内側壁に形成させたダミー壁をハンマーで１〜２ｋｇ・ｍ／ｓの衝撃力を与えた。このとき、ダミー壁の剥離率（真空蒸着室の内側壁の面積に対する剥がれたダミー壁面積の比率）を測定し、更に剥離率が１００％のときには、剥離に要した時間を測定し、式、剥離時間（秒／ｍ２）＝（剥離に要した時間／真空蒸着室の内側壁の面積）、により単位面積当たりの剥離所要時間を算出した。
(1) Coating property The slurry was brush-coated to a thickness of about 10 mm on the side wall of the inner wall of the aluminum vacuum deposition chamber, and the coating amount per coating area (coating speed) was measured.
(2) Sagging properties Brushing 5 kg / m 2 of slurry on the ceiling surface of the aluminum vacuum deposition chamber, measuring the sagging amount when left for 1 minute, “excellent”: no sagging, “good”: sagging amount Is less than 10 g / m 2 , “impossible”: the sagging amount is 10 g / m 2 or more.
(3) Peelability After applying the slurry to the inner wall and ceiling surface of the aluminum vacuum deposition chamber, the slurry was naturally dried for 2 hours to form a dummy wall (thickness 10 mm), then evacuated to 0.01 Pa, and 5 g / The aluminum was evaporated for 5 minutes at a rate of minutes. At this time, the temperature of the inner wall and the ceiling surface of the vacuum deposition chamber was 130 to 170 ° C. Thereafter, the vacuum deposition chamber was cooled to room temperature, and an impact force of 1 to 2 kg · m / s was applied to the dummy wall formed on the inner wall with a hammer. At this time, the peeling rate of the dummy wall (ratio of the peeled dummy wall area to the area of the inner wall of the vacuum evaporation chamber) was measured. When the peeling rate was 100%, the time required for peeling was measured, Peeling time per unit area was calculated from peeling time (second / m 2 ) = (time required for peeling / area of inner wall of vacuum deposition chamber).
本発明のスラリーは、例えば金属の真空蒸着室内にダミー壁を形成させるのに使用される。 The slurry of the present invention is used, for example, to form a dummy wall in a metal vacuum deposition chamber.
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| JP5530318B2 (en) * | 2010-09-10 | 2014-06-25 | 電気化学工業株式会社 | Hexagonal boron nitride powder and high thermal conductivity and high moisture resistance heat dissipation sheet using the same |
| JP6588731B2 (en) * | 2015-05-07 | 2019-10-09 | キヤノン株式会社 | Electrophotographic photosensitive member, process cartridge, and electrophotographic apparatus |
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| JP3644713B2 (en) * | 1995-02-10 | 2005-05-11 | 電気化学工業株式会社 | Method for producing hexagonal boron nitride powder |
| JP4014445B2 (en) * | 2002-05-22 | 2007-11-28 | 電気化学工業株式会社 | Engine oil additive and engine oil |
| JP3818992B2 (en) * | 2003-08-22 | 2006-09-06 | 電気化学工業株式会社 | Boron nitride composition |
| JP4278531B2 (en) * | 2004-02-13 | 2009-06-17 | 電気化学工業株式会社 | Release agent |
| JP4241424B2 (en) * | 2004-02-18 | 2009-03-18 | 電気化学工業株式会社 | Boron nitride powder and mold release agent |
| JP4331140B2 (en) * | 2005-04-21 | 2009-09-16 | 電気化学工業株式会社 | Boron nitride containing slurry |
| JP4916687B2 (en) * | 2005-08-19 | 2012-04-18 | 電気化学工業株式会社 | engine oil |
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