JP5290161B2 - 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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- 239000002245 particle Substances 0.000 title claims description 34
- 238000004519 manufacturing process Methods 0.000 title claims description 14
- 238000000034 method Methods 0.000 claims description 33
- 239000002243 precursor Substances 0.000 claims description 31
- 239000000843 powder Substances 0.000 claims description 23
- 229910052751 metal Inorganic materials 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 150000004767 nitrides Chemical class 0.000 claims description 12
- 239000003870 refractory metal Substances 0.000 claims description 10
- 229910052726 zirconium Inorganic materials 0.000 claims description 10
- 229910021332 silicide Inorganic materials 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 7
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 claims description 6
- 150000001805 chlorine compounds Chemical class 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 229910052721 tungsten Inorganic materials 0.000 claims description 5
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 4
- 239000005977 Ethylene Substances 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 230000003993 interaction Effects 0.000 claims description 3
- 229910001510 metal chloride Inorganic materials 0.000 claims description 2
- 239000002923 metal particle Substances 0.000 claims description 2
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- 239000012071 phase Substances 0.000 description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
- 230000015572 biosynthetic process Effects 0.000 description 13
- 239000007789 gas Substances 0.000 description 10
- 238000003786 synthesis reaction Methods 0.000 description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 8
- 239000000460 chlorine Substances 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 229910052760 oxygen Inorganic materials 0.000 description 8
- 239000001301 oxygen Substances 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 238000001725 laser pyrolysis Methods 0.000 description 7
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical group [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 6
- 229910052801 chlorine Inorganic materials 0.000 description 6
- 125000002524 organometallic group Chemical group 0.000 description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 5
- 125000004429 atom Chemical group 0.000 description 5
- 229910052750 molybdenum Inorganic materials 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
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- 239000000463 material Substances 0.000 description 4
- 150000001247 metal acetylides Chemical class 0.000 description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
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- 239000010936 titanium Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910007926 ZrCl Inorganic materials 0.000 description 2
- 239000007833 carbon precursor Substances 0.000 description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 2
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- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
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- 229910052719 titanium Inorganic materials 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical class C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical class CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
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- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000013626 chemical specie Substances 0.000 description 1
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- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 229910003480 inorganic solid Inorganic materials 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- -1 metallocenes Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
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- 230000005855 radiation Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 238000002626 targeted therapy Methods 0.000 description 1
- 238000003856 thermoforming Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 description 1
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- C01B9/00—General methods of preparing halides
- C01B9/02—Chlorides
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- B22F9/00—Making metallic powder or suspensions thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C01B32/00—Carbon; Compounds thereof
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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)
- 反応の流れ(14)とエネルギーの流れ(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、
−塩化物を製造するための装置内で、金属粉末の形態の塩基前駆物質(20)を熱すること及びそれらを塩酸と反応させることによって、気体の塩化物を製造する工程、及び
−その結果形成された反応の流れ(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。 - ナノメータ粒子が金属粒子である請求項1に記載の方法。
- 反応の流れ(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℃より下の温度で粉体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。
- エネルギーの流れがCO 2 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。
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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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