JP2009538745A - ナノメータ粒子を製造するための気相法 - Google Patents
ナノメータ粒子を製造するための気相法 Download PDFInfo
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Abstract
−該リアクター(11)と気体の塩化物(12)を製造するための装置を連結する工程
−粉末の形態の塩基前駆物質(20)から気体の塩化物を製造する工程、及び
−前記反応流(14)をリアクター(11)内に注入する工程。
Description
ナノ粒子を製造するための数多くの方法が存在し(プラズマ、レーザー熱分解、燃焼、蒸発凝縮、超臨海流体、ゲル−ソル、共沈殿、熱水合成)、あるものは酸化物の製造により適しており(燃焼、蒸発凝縮、超臨海流体、ゲル−ソル、共沈殿、熱水合成)、他のものは気相における非酸化物粒子の合成に適している(非特許文献1に記載のレーザー熱分解、プラズマ、蒸発凝縮)。
本発明の目的は、低コストで、高い純度を有するナノ粒子を製造するための気相法を提案することでこの技術的問題を解決することである。
−該リアクターと気体の塩化物を製造するための装置を連結する工程
−粉末の形態の塩基前駆物質から気体の塩化物を製造する工程、及び
−前記反応流をリアクター内に注入する工程
を含むことを特徴とする気相法に関する。
ナノメータ粒子は金属粒子であってもよい。
ナノメーター粒子は、炭化物、窒化物、酸化物、ケイ化物及び混合物の粒子、例えば純粋なMAXフェーズであってもよい。
ナノメーター粒子は、高融点を有する耐火性金属要素、例えばZr、W、Mo、…、であってもよい。
好ましくは、気体の金属塩化物は、塩化物製造用装置で、1000℃より下の温度、さらには500℃より下の温度で、金属粉末を熱し、それらを塩酸と反応させることによって製造される。
この方法は、好適には、形成したいとナノメーター粒子の全ての構成成分の別々の注入及び多元素粒子の製造の促進を可能にし、それらの化学組成は、各前駆物質の流速を独立に変化させることによって任意に変化させてもよい。
また、この方法は、気体の塩素化分子として、市販の耐火性金属粉末及び塩酸(HCl)を使用することのみによって、最適化されたコストで、大量の耐火性金属(Zr、W、Mo、…)の生成及び注入を可能にする。
この方法は、市販の粉末の使用を可能にし、それは他の知られている前駆物質に等しい純度レベルを有する最も安価な前駆物質であるので、非常に高価にはならない利点を有する。ナノ粒子を合成するためのこの方法では、そのままで市販の粉末を塩素化することによって、市販の塩化物の使用に比べて、製造コスト上10倍の利益を獲得しうる。
この実施例において、レーザー熱分解リアクター(11)が使用され、塩素発生装置(12)に接続され、粉末の空気との接触における自然発火効果を避けるために不活性雰囲気下で、ジルコニウム粉末(20)(塩基前駆物質)が塩素発生装置(12)中に導入される。
粉末は450℃より高く熱され、その蒸気を塩素処理するために、塩素ガス(HCl)の流れによって流される。その後、これらの蒸気は注入ノズル(22)を介して、レーザー熱分解リアクター)中に運ばれる。ノズル(22)は、ZrCl4の凝集を避けるための300℃より高く熱される。気体の前駆物質(13)はエチレン(C2H4)である。それは、注入ノズル(22)に導入され、ZrCl4と混合される。それはレーザーの赤外線放射(15)の10.6ミクロン(CO2レーザーの波長)を吸収し、そのエネルギーを試薬に再分配するため炎色反応がおきるので、選択された。この反応は、ナノメータ粒子の発芽に続いて前駆物質の分解を起こし、その成長はクエンチング効果によって止められる。エネルギー流(15)の源は5kWのCO2レーザーである。
得られた純度は、出発の粉末のそれである。すなわち、後に記載する表に記載したジルコニウムの純度であり、99.7%のオーダーである。
Claims (12)
- 反応流(14)とエネルギー流(15)の間の相互作用がある気相中で、粒子製造用リアクター(11)内でナノメータ粒子(10)を製造する気相法であって、
−該リアクター(11)と気体の塩化物を製造するための装置(12)を連結する工程
−粉末の形態の塩基前駆物質(20)から気体の塩化物を製造する工程、及び
−前記反応流(14)をリアクター(11)内に注入する工程
を含むことを特徴とする気相法。 - ナノメーター粒子が金属粒子である請求項1に記載の方法。
- 反応流(14)を形成するために、気体の塩化物(16)と少なくとも1つの他の前駆物質(13)を組合わせる工程を更に含む請求項1に記載の方法。
- ナノメータ粒子が炭化物粒子、窒化物粒子、酸化物粒子、ケイ化物粒子又は混合物粒子である請求項3に記載の方法。
- 混合物粒子が純粋なMAXフェーズである請求項4に記載の方法。
- ナノメータ粒子が高融点を有する耐火性金属を含む請求項1から5の何れか一項に記載の方法。
- 耐火性金属がW、Zr又はCoから選択される金属である請求項6に記載の方法。
- 塩化物を製造するための装置内で、1000℃より下の温度で粉末を熱し塩酸と反応させることによって、気体の金属塩化物が製造される、請求項1に記載の方法。
- 温度が500℃より下である請求項8に記載の方法。
- 前記ナノメーター粒子の全ての構成成分が別々に注入される請求項1に記載の方法。
- エネルギー流がCO2又はCOレーザー、又はプラズマトーチにより放出される請求項1に記載の方法。
- 前記少なくとも1つの他の前駆物質(13)がエチレンを含む請求項1に記載の方法。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR0651959A FR2901714B1 (fr) | 2006-05-30 | 2006-05-30 | Procede en phase gazeuse pour la production de particules nanometriques |
FR0651959 | 2006-05-30 | ||
PCT/EP2007/055161 WO2007138034A1 (fr) | 2006-05-30 | 2007-05-29 | Procede en phase gazeuse pour la production de particules nanometriques |
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JP2009538745A true JP2009538745A (ja) | 2009-11-12 |
JP5290161B2 JP5290161B2 (ja) | 2013-09-18 |
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JP2009512566A Active JP5290161B2 (ja) | 2006-05-30 | 2007-05-29 | ナノメータ粒子を製造するための気相法 |
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US (1) | US8241392B2 (ja) |
EP (1) | EP2021123B1 (ja) |
JP (1) | JP5290161B2 (ja) |
KR (1) | KR101410802B1 (ja) |
AT (1) | ATE441475T1 (ja) |
CA (1) | CA2653680C (ja) |
DE (1) | DE602007002298D1 (ja) |
ES (1) | ES2333066T3 (ja) |
FR (1) | FR2901714B1 (ja) |
PL (1) | PL2021123T3 (ja) |
WO (1) | WO2007138034A1 (ja) |
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FR2901721B1 (fr) * | 2006-05-30 | 2008-08-22 | Commissariat Energie Atomique | Poudres de phase max et procede de fabrication des dites poudres |
FR2984766B1 (fr) * | 2011-12-23 | 2014-02-14 | Commissariat Energie Atomique | Buse d'injection en materiau composite pour la production de poudres par pyrolyse laser. |
FR2984758B1 (fr) * | 2011-12-23 | 2014-02-14 | Commissariat Energie Atomique | Methode de production de poudres en flux continu par pyrolyse laser utilisant une buse d'injection en materiau composite. |
CN109396456B (zh) * | 2018-12-28 | 2024-02-13 | 西安赛隆金属材料有限责任公司 | 一种球形钨粉末的制备装置及方法 |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0388709A (ja) * | 1989-08-31 | 1991-04-15 | Canon Inc | 炭化物微粒子の製造方法 |
WO2006009881A2 (en) * | 2004-06-18 | 2006-01-26 | Innovalight, Inc. | Process and apparatus for forming nanoparticles using radiofrequency plasmas |
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IT1281338B1 (it) * | 1995-11-24 | 1998-02-18 | Cise Spa | Processo per produrre polveri nanometriche di ossidi metallici da cloruri metallici |
US20020155059A1 (en) * | 2001-04-24 | 2002-10-24 | Tekna Plasma Systems Inc. | Plasma synthesis of titanium dioxide nanopowder and powder doping and surface modification process |
US6994837B2 (en) * | 2001-04-24 | 2006-02-07 | Tekna Plasma Systems, Inc. | Plasma synthesis of metal oxide nanopowder and apparatus therefor |
US20040065170A1 (en) * | 2002-10-07 | 2004-04-08 | L. W. Wu | Method for producing nano-structured materials |
US20050119398A1 (en) * | 2003-09-11 | 2005-06-02 | Lu Zhang | Plasma synthesis of metal oxide nanoparticles |
US7828999B2 (en) | 2004-09-07 | 2010-11-09 | Nisshin Seifun Group Inc. | Process and apparatus for producing fine particles |
-
2006
- 2006-05-30 FR FR0651959A patent/FR2901714B1/fr not_active Expired - Fee Related
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2007
- 2007-05-29 AT AT07729584T patent/ATE441475T1/de active
- 2007-05-29 ES ES07729584T patent/ES2333066T3/es active Active
- 2007-05-29 WO PCT/EP2007/055161 patent/WO2007138034A1/fr active Application Filing
- 2007-05-29 EP EP07729584A patent/EP2021123B1/fr active Active
- 2007-05-29 PL PL07729584T patent/PL2021123T3/pl unknown
- 2007-05-29 DE DE602007002298T patent/DE602007002298D1/de active Active
- 2007-05-29 KR KR1020087028410A patent/KR101410802B1/ko active IP Right Grant
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- 2007-05-29 CA CA2653680A patent/CA2653680C/en active Active
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Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0388709A (ja) * | 1989-08-31 | 1991-04-15 | Canon Inc | 炭化物微粒子の製造方法 |
WO2006009881A2 (en) * | 2004-06-18 | 2006-01-26 | Innovalight, Inc. | Process and apparatus for forming nanoparticles using radiofrequency plasmas |
Non-Patent Citations (2)
Title |
---|
JPN6013004644; Guozhen Shen et.al.: '"Synthesis of ZrC hollow nanospheres at low temperature"' Journal of Crystal Growth 262, 20040215, pp.277-280 * |
JPN6013004644; Guozhen Shen: 'Synthesis of ZrC hollow nanospheres at low temperature' Journal of Crystal Growth 262, 20040215, pp.277-280 * |
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KR20090012334A (ko) | 2009-02-03 |
CA2653680C (en) | 2014-08-05 |
WO2007138034A1 (fr) | 2007-12-06 |
FR2901714A1 (fr) | 2007-12-07 |
ES2333066T3 (es) | 2010-02-16 |
EP2021123B1 (fr) | 2009-09-02 |
ATE441475T1 (de) | 2009-09-15 |
KR101410802B1 (ko) | 2014-07-01 |
US8241392B2 (en) | 2012-08-14 |
FR2901714B1 (fr) | 2008-09-05 |
EP2021123A1 (fr) | 2009-02-11 |
PL2021123T3 (pl) | 2010-01-29 |
CA2653680A1 (en) | 2007-12-06 |
US20090294274A1 (en) | 2009-12-03 |
DE602007002298D1 (de) | 2009-10-15 |
JP5290161B2 (ja) | 2013-09-18 |
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