JP4507598B2 - 表面に無機薄膜を有する非凝集粒子を製造するための方法 - Google Patents
表面に無機薄膜を有する非凝集粒子を製造するための方法 Download PDFInfo
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- JP4507598B2 JP4507598B2 JP2003513771A JP2003513771A JP4507598B2 JP 4507598 B2 JP4507598 B2 JP 4507598B2 JP 2003513771 A JP2003513771 A JP 2003513771A JP 2003513771 A JP2003513771 A JP 2003513771A JP 4507598 B2 JP4507598 B2 JP 4507598B2
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
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- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/006—Coating of the granules without description of the process or the device by which the granules are obtained
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- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
- B01J21/04—Alumina
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
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- B01J37/0201—Impregnation
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/086—Decomposition of an organometallic compound, a metal complex or a metal salt of a carboxylic acid
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- B22—CASTING; POWDER METALLURGY
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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- B22F1/18—Non-metallic particles coated with metal
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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Description
例えば、周囲環境から攻撃を受けたり、そうでなければ望ましくない反応に関与する表面を粒子が有する場合がある。この場合、その反応表面を不動態化してこれらの反応の発生を阻止することが好ましい。
従って、粒子材料のバルク特性を著しく変えずに粒子の表面特性を改質できる方法を提供することが望ましい。
別の態様において、本発明は、粒子の表面に結合した超薄膜無機材料を形成するために、粒子の表面において2回以上の自己停止反応工程を行うことから成る、粒子上に超薄膜の無機材料を成膜させる方法である。
第三の態様において、本発明は、無機材料の粒子で充填された樹脂マトリックスであり、この場合粒子はその表面上に超薄膜無機材料を有する。
第四の態様において、本発明は、表面に超薄膜のコンフォーマル金属皮膜を有する複数の焼結可能な無機材料粒子から成形された集塊を形成し、次いで、この粒子を焼結するのに十分な条件にこの集塊を曝して、成形された部品を作製することから成るサーメット部品の製造方法である。
第五の態様において、本発明は、表面に超薄膜のコンフォーマル金属皮膜を有する複数の焼結可能な無機材料粒子から成形された集塊を形成し、次いで、この粒子を焼結するのに十分な条件にこの集塊を曝して、成形された部品を作製することから成るセラミック部品の製造方法である。
第六の態様において、本発明は、500ミクロン以下の平均粒径を有し、表面に化学反応のための触媒である金属の超薄膜成膜を有する粒子の存在下で、化学反応を行うことから成る、化学反応に触媒作用を及ぼす方法である。
電子機器実装用の高熱伝導性充填材として有用な無機材料は、約3W/mK以上、好ましくは5W/mK以上、より好ましくは10W/mK以上、更に更に好ましくは15W/mK以上、最も好ましくは200W/mK以上のバルク熱伝導率を有することが望ましい。適切なものとしては、例えば、二酸化ケイ素、アルミナ、3族、13族、14族元素の窒化物及び、4族、6族、13族、14族元素の炭化物が含まれる。充填材用途に好ましい窒化物は、窒化アルミニウム(AIN)、窒化ホウ素(BN)(特に、六方型のBN)、窒化ケイ素(Si3N4)などである。好ましい炭化物は炭化タングステン(WC)である。
サーメット用途に有用な無機材料には、窒化ケイ素、窒化アルミニウム、窒化ホウ素、炭化タングステン、炭化ホウ素、炭化チタンが含まれる。
有用な担持材料である無機材料には、例えば、アルミナ、シリカ、ジルコニア、及び様々な天然及び合成ゼオライト材料などが含まれる。
鉄、ニッケル、及び又は、ネオジミウム‐鉄‐ホウ素(Nd−Fe−B)常時勢磁石材料などの磁性又は常磁性材料。
ALD法において形成された無機成膜は、個別の粒子又は連続若しくは半連続薄膜の形態を取ってもよい。この成膜の物理的形状は、基質の物理的形状及び反応工程の反復回数などの因子に依存する。
無機材料は成膜後に粒子が凝集化しないことが好ましい。"凝集化しない"とは、基質粒子を無機材料で被覆する工程の間、粒子が著しい量の凝集体を形成しないという意味である。(a)皮膜が成膜した結果、平均粒径が約5%未満、好ましくは約2%未満、より好ましくは約1%未満だけ増大した(粒径の増大とは別に皮膜そのものに起因する)場合に、又は、(b)無機材料の成膜工程中に、粒子の2重量%だけ、好ましくは1重量%だけが凝集化した場合に、粒子は凝集化していないものと見なされる。
1.シリカ又はアルミナで被膜された、AIN、BN、Si3N4粒子などの3属、13属、14属の窒化物粒子。これらは、熱可塑性及び熱硬化性樹脂、特に電子部品実装用途に使用されるエポキシ樹脂のための充填材として有用である。
4.アルミナ、シリカ又は酸化イットリウムのような酸化物皮膜有する金属粒子、AIN、BN、Si3N4のような窒化物皮膜を有する金属粒子、硫化ガリウムなどの硫化物皮膜を有する金属粒子。このような皮膜は金属粒子を酸化環境から絶縁できるので、酸化しやすい金属については特に重要である。これら被覆された金属粒子は、様々な用途において充填材として使用可能である。特に重要な例としては、IR放射に対して透過性のシリカなどの材料で被膜した鉄粒子である。また、焼結助剤で被膜されサーメット用途に金属相として有用な金属も特に重要である。
6.大気に曝されると容易に酸化される金属又はセラミック材料のナノサイズ粒子であり、酸化から粒子を保護する層で被膜されているもの。具体例としては、炭化チタン、炭化ホウ素、炭化ケイ素、炭化タングステン、窒化アルミニウム、窒化ホウ素又は窒化ケイ素のような鉄及び非酸化物系セラミック材料粒子で、例えば、シリカ又はアルミナで被膜されているもの。
M-Z-H* + M1Xn → M-Z-M1X* + HX (A1)
M-Z-M1X* + H2O → M-Z-M1OH* + HX (B1)
Al-(CH3)* + H2O → Al-OH* + CH4 (A1A)
Al-OH* + Al(CH3)3 → Al-O-Al(CH3)2 * + CH4 (B1A)
この特定の反応順序は、反応が350°Kを下回る温度で進行するため、アルミナの成膜に特に好ましい。この特定の反応工程はABサイクルごとに〜1.2オングストロームの速度でAl2O3を成膜させる傾向がある。トリエチルアルミニウム(TEM)は、この反応工程においてTMAの代わりに使用することができる。
M-Z-H* + M1Xn → M-Z-M1X* + HX (A2)
M-Z-M1X* + NH3 → M-Z-M1NH* + HX (B2)
アンモニアを除去して層内または層間にM1−N−M1結合を形成することができる。必要に応じて、例えば、高温及び/又は減圧下で焼きなましを行いこの反応を促進することができる。
M-Z-H* + M1Xn → M-Z-M1X* + HX (A3)
M-Z-M1X* + H2S → M-Z-M1SH* + HX (B3)
硫化水素を除去して層内または層間M1−S−M1結合を形成することができる。上記と同様に、高温及び/又は減圧下で焼きなましを行いこの反応を促進することができる。
無機リン化物成膜の被覆に適した二元反応体系はIshii等のCrystal. Growth 180(1997)15に開示されている。
M-F1 + C1 → M-F1---C1 (A4a)
M-F1---C1 + F2-M1-F2 → M-M1-F2 + F1-F2 + C1 (A4b)
M-M1-F2 + C2 → M-M1-F1---C2 (B4a)
M-M1-F1---C2 + F1-M-F1 → M-M1-M-F1+ F1-F2 + C2 (B4b)
Si-OH* (粒子) + C5H5N → Si-OH---C5H5N*
Si-OH---C5H5N* + SiCl4 → Si-O-SiCl3 * + C5H5N + HCl
Si-O-SiCl3 * + C5H5N → Si-O-SiCl3---C5H5N*
Si-O-SiCl3 *---C5H5N + H2O → Si-O-SiOH* + C5H5N + HCl
金属の成膜に適した二元反応体系は2000年3月10日出願の共係属出願"A Solid material Comprising a Thin Metal Film on its Surface and Methods for Producing the Same"に開示されている。そこに開示の具体的な反応体系には、基質表面がハロゲン化金属に続きハロゲン化金属還元剤と逐次的に反応することが包含される。ハロゲン化金属の金属は、好ましくはタングステン、レニウム、モリブデン、アンチモン、セレン、テルル、白金、ルテニウム及びイリジウムなどの遷移金属又は半金属元素である。ハロゲン化物は、好ましくはフッ化物である。還元剤は、シラン、ジシラン、トリシラン及びそれらの混合物などの好適なシリル化剤である。その他の好適な還元剤とはジボランなどのハロゲン化ホウ素である。タングステン成膜のための反応工程は次のように表わされる。
M-OH* (粒子) + Si2H6 → M-Si* 2H5 (前駆体反応)
M-Si* 2H5 +WF6 → M-W-F* + Si* 2H6 (A5)
M-W-F* + Si2Hy Fz → M-W-Si* 2H5 + H2 + Si2H6Fb (B5)
また、次の二元反応体系も表面ヒドロキシル又はアミノ基をもつ粒子の上に金属(M2)を成膜する際に適している。
M*-Z-H + M2Xn → M-Z-M2Xn + HX (前駆体反応 )
M-Z-M2X* + H2 → M-Z-M2-H* + HX (B6 )
M-Z-M2-H* + M2 (acac) → M-Z-M2-M2*(acac) (A6 )
上記の触媒反応体系を除き、二元反応は一般に高温で、好ましくは約300〜1000Kで行われる。反応と反応の間に、粒子を十分な所定条件下にさらし反応生成物と未反応試薬を除去する。これは、各反応ステップ後、例えば、約10-5Torr(約133×10-5Pa)以下の高真空に粒子をさらすことで達成できる。また、もう一つの達成方法は、各反応段階の間に粒子を不活性パージガスでスウィープするもので、産業用途で用いられている方法である。このパージガスは粒子の流動化媒体及び試薬の担体として機能することもできる。
同様に、本発明による金属成膜を有するセラミック材料は、サーメットを形成するために形を形成し焼結可能である。このため焼結前に形成された形状の全体に金属相を微細に分布できる。これは最終部品内の金属の分布を向上し、結果としてより均一な組成の部品が形成される。このような金属成膜を有する金属セラミック材料の使用により、必要な金属粉末量を減少又は全くゼロにすることができる。特に重要な系は炭化タングステン系サーメットである。従来のサーメット製造法では靭性と焼結性を向上するために、金属相としてコバルトが使用されているが、コバルトの存在は最終部品の硬度を減少させる傾向があり望ましくない。超薄膜コバルト成膜を有する炭化タングステン粒子の使用は、炭化タングステンの硬度を保持する高品質の炭化タングステンサーメット材料の製造方法を潜在的に提供するものである。
また、別の用途においては、サブミクロン鉄粒子をシリカのような赤外線透過超薄膜で被覆する。得られる粒子は防錆かつレーダー吸収体である。この粒子は結合剤と併用して航空機及びその他の車輌のコーティング材を形成でき、車輌から反射されるレーダー量を軽減する。
微小な分子、放射性核種、生物製剤、造影剤、遺伝ベクターなど広範な種類の薬剤を使用することができる。薬剤の例としては、ドクソルビシン、パクリタキセル、99Tc、186Te、188Re、メトトレキセート、サリドマイド、FUDR、マイトマイシンC、ブレオマイシン、ビンブラスチンがあげられる。
もう一つの用途では、反射粒子を形成して、例えば、ガラス又はその他基質に反射皮膜を適用する。本発明による被膜粒子の例は、タングステン、アルミニウム、銀若しくはその他金属で被膜されたシリカ又は発煙性シリカ基質粒子である。粒子は、例えば、UV線などの電磁放射線を反射する皮膜を提供するために、ガラス又はその他の基質に被覆されるか又は導入される。粒子は、(1)大部分又は全ての可視光が基質を通じて透過される濃度、(2)UVなどの反射放射線がランダム反射する濃度で使用されることが好ましい。
次に、実施例を参照して本発明を説明するが、これらの実施例は発明の範囲を制限するものではない。特に示されない限り、部及びパーセンテージはすべて重量に基づくものである。
生体内透過FTIR振動分光法用に設計された真空装置の中で、アルミナ(Al2O3)をBN粒子に成膜する。この装置は、Dillon等のSurface Science 139:537-543 (1992)及び共に係属中の出願第08/442,907号(1995年5月17日出願)に詳細に記載されている。BN窒化物粒子はAdvanced Ceramics Corporation製HCVグレードBN粒子である。これは、全表面積約40m2/g、約0.1〜0.5ミクロン(μm)のターボ成薄膜結晶を主成分とする約10ミクロンの凝集体である。
その後、粒子を連続的に450°KでAl(CH3)3と水に50サイクル曝し、粒子表面に90オングストロームの皮膜を成膜する。各反応ステップで反応が完了するように、各反応とも、反応物の露出は1.8×108ラングミュア(L, = 10-6 Torr(約133×10-6 Pa)・秒)とする。低圧露出は1×10-4 〜1×10-3 Torr(約133×10-4 〜133×10-3 Pa)の範囲の反応圧力とし、ゲート弁で上側チェンバーと下側チェンバーを開いておく。高圧露出は、0.01〜10Torr(約1.33〜1330 Pa)で曝すために、上側チェンバーは機械式ポンプにより封じ込められた液体N2で排出する。次に上側チェンバーを下側チェンバーとターボ分子ポンプに開き、露出と露出の間に2×10-6Torr(約266×10-6 Pa)以下の圧力をかける。各反応サイクル毎に、約1.8オングストロームのAl2O3形成が見られる。
生成物のTEM像から BN粒子のベース面はSiO2で無作為に被覆され、端面はかなり均一に被覆されていることが分かる。
粒子表面のXPS分析から、約72-77eVの結合エネルギー値でスペクトルにAl 2pのピークが出現したことから実証されるように、表面がアルミナで被膜されることがわかる。
Claims (2)
- シリカ又はアルミナの無機薄膜を表面に有し、平均粒径が500μm以下の窒化物粒子又は金属粒子である基質粒子から成る非凝集粒子を製造するための方法であって、基質粒子の表面で2回以上の自己停止反応工程を連続して行い、前記基質粒子の表面に結合する厚さが100nm以下の無機薄膜を有する被膜粒子を形成することから成り、該反応が該基質粒子を含んだ流動層で行われることを特徴とする方法。
- 前記反応工程が、前記基質粒子に第一の反応物と第二の反応物を交互に接触させることから成り、該第一の反応物と第二の反応物は、これらが反応して無機薄膜を形成するものである、請求項1に記載の方法。
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US10221637B2 (en) | 2015-08-11 | 2019-03-05 | Baker Hughes, A Ge Company, Llc | Methods of manufacturing dissolvable tools via liquid-solid state molding |
US10016810B2 (en) | 2015-12-14 | 2018-07-10 | Baker Hughes, A Ge Company, Llc | Methods of manufacturing degradable tools using a galvanic carrier and tools manufactured thereof |
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WO2018192885A1 (fr) * | 2017-04-20 | 2018-10-25 | Rolex Sa | Fabrication d'un composant en céramique |
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KR102584736B1 (ko) | 2018-10-02 | 2023-10-05 | 로저스코포레이션 | 코팅된 질화 붕소를 포함하는 인쇄회로기판 서브스트레이트 |
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DE3546113A1 (de) * | 1985-12-24 | 1987-06-25 | Santrade Ltd | Verbundpulverteilchen, verbundkoerper und verfahren zu deren herstellung |
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US5273942A (en) * | 1990-10-19 | 1993-12-28 | Rutgers University | Ceramic powder useful in the manufacture of green and densified fired ceramic articles |
US5935889A (en) * | 1996-10-04 | 1999-08-10 | Abb Lummus Global Inc. | Catalyst and method of preparation |
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US6811813B1 (en) * | 1999-05-19 | 2004-11-02 | Sarnoff Corporation | Method of coating micrometer sized inorganic particles |
US6613383B1 (en) * | 1999-06-21 | 2003-09-02 | Regents Of The University Of Colorado | Atomic layer controlled deposition on particle surfaces |
JP2002308716A (ja) * | 2001-04-06 | 2002-10-23 | Isi:Kk | 単分散超薄膜で包接された微粒子とそれを用いた化粧料 |
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- 2002-07-16 AU AU2002320588A patent/AU2002320588A1/en not_active Abandoned
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US11887781B2 (en) | 2014-04-01 | 2024-01-30 | Forge Nano, Inc. | Energy storage devices having coated passive particles |
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CA2452531C (en) | 2010-11-02 |
WO2003008186A1 (en) | 2003-01-30 |
CA2452531A1 (en) | 2003-01-30 |
DE60232884D1 (de) | 2009-08-20 |
JP2005501176A (ja) | 2005-01-13 |
ATE435740T1 (de) | 2009-07-15 |
EP1412175B1 (en) | 2009-07-08 |
EP1412175A4 (en) | 2006-03-01 |
EP1412175A1 (en) | 2004-04-28 |
AU2002320588A1 (en) | 2003-03-03 |
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