JP5847996B2 - 複合粒子の製造方法 - Google Patents
複合粒子の製造方法 Download PDFInfo
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- 238000004519 manufacturing process Methods 0.000 title claims description 29
- 239000011246 composite particle Substances 0.000 title claims description 18
- 239000002243 precursor Substances 0.000 claims description 122
- 239000000463 material Substances 0.000 claims description 109
- 239000002245 particle Substances 0.000 claims description 100
- 239000007789 gas Substances 0.000 claims description 77
- 239000000443 aerosol Substances 0.000 claims description 33
- 238000000034 method Methods 0.000 claims description 30
- 239000000843 powder Substances 0.000 claims description 22
- 239000011258 core-shell material Substances 0.000 claims description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 14
- 229910052799 carbon Inorganic materials 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 150000002642 lithium compounds Chemical class 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 229910000733 Li alloy Inorganic materials 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 239000001989 lithium alloy Substances 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims 1
- 239000002184 metal Substances 0.000 claims 1
- 239000011162 core material Substances 0.000 description 23
- 239000007788 liquid Substances 0.000 description 18
- 239000011257 shell material Substances 0.000 description 18
- 239000002105 nanoparticle Substances 0.000 description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 14
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 description 10
- 239000010936 titanium Substances 0.000 description 9
- 229910006404 SnO 2 Inorganic materials 0.000 description 7
- 229910052786 argon Inorganic materials 0.000 description 7
- 238000000354 decomposition reaction Methods 0.000 description 7
- 238000010586 diagram Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 4
- 239000005977 Ethylene Substances 0.000 description 4
- 238000003917 TEM image Methods 0.000 description 4
- 239000012705 liquid precursor Substances 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 150000003254 radicals Chemical class 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000003574 free electron Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 150000002902 organometallic compounds Chemical group 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 239000011263 electroactive material Substances 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 238000000386 microscopy Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000011236 particulate material Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C16/50—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 using electric discharges
- C23C16/513—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 using electric discharges using plasma jets
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C16/22—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 deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C16/4417—Methods specially adapted for coating powder
Description
乾燥前駆体粉末であり、第一材料を含有する第一前駆体を用意する工程、
第一ガスを用意する工程、
高強度場ゾーンと高強度場ゾーンの下流である残照領域とを有するプラズマを用意する工程、
第一ガスおよび第一前駆体をプラズマの高強度場ゾーンを通す工程、
プラズマの高強度場ゾーン内で第一前駆体中の第一材料の少なくとも一部を分解する工程、
乾燥前駆体粉末であり、第二材料を含有する第二前駆体を用意する工程、
第二前駆体を第二ガス中に懸濁させてエアロゾルを製造する工程、
残照領域中にエアロゾルを通し、その際にエアロゾルに高強度場ゾーンを迂回させる工程、
分解した第一材料をプラズマの高強度場ゾーンから除く工程、および
分解した第一材料の少なくとも一部をエアロゾル中の第二材料上に凝縮させて、複合粒子を製造する工程、
を含む、前記方法に関する。
前記の方法は、第一材料を含有する第一前駆体およびプラズマ領域を発生させる働きをするプラズマトーチを用意する工程を含む。乾燥前駆体粉末で存在し得る第一前駆体を、プラズマトーチによって発生されるプラズマの高強度場ゾーンに通して第一前駆体の少なくとも一部が分解する。第一前駆体が乾燥前駆体粉末を含む場合、それは第一ガス中に懸濁され得て、プラズマの高強度場ゾーンを通る前に第一エアロゾルを製造し得る。
チタン酸リチウム(Li4Ti5O12)のコアおよび炭素のシェルを有するコア/シェルナノ粒子を、図2A又は図2Cに示す装置および上記の製造法を用いて製造した。特に、アントラセンおよび/又はエチレンの第一前駆体を提供し、そして1.47標準L/分(SLPM)の流速でアルゴンの第一ガスを用いてプラズマトーチを通した。また、加えて、2.89SLPMの流速のアルゴンのプラズマガスを用意した。第二前駆体として、38nm未満の平均径を有するLi4Ti5O12の粒子が、1.83SLPMの流速を有するアルゴンの第二ガスを用いて高強度場ゾーンとプラズマ装置の残照領域との間の位置に用意された。900ワットのマイクロ波エネルギー源および+10トールの全圧がプラズマトーチ内でプラズマを発生させるために用いられ、そしてある場合には、アントラセンおよび/又はエチレンおよびLi4Ti5O12がプラズマ工程の間、超音波振動に供された。
複数の酸化スズ(SnO2)/炭素コア−シェルナノ粒子を図2Aに示す装置を用いて製造した。特に、アントラセンの第一前駆体を1.47SLPMの流速を有するアルゴンの第一ガスを用いてプラズマの高強度場ゾーンに用意した。加えて、アルゴンのプラズマガスを2.89SLPMの流速を用いて用意した。SnO2の第二前駆体を1.83SLPMの流速を有するアルゴンの第二ガスを用いて残照の底端部/高強度場ゾーン領域の頂部に用意した。プラズマトーチ内でプラズマを発生させるために、900ワットのマイクロ波エネルギーと全圧+10トールを用い、そしてある場合には、プラズマ工程の間、アントラセンおよびSnO2を入れた1つ又は両方のビーカーに超音波振動を供した。SnO2/炭素コア−シェルナノ粒子のTEM画像を図6に示し、そして内部のSnO2コア上の外部炭素シェルを示すHR−TEM画像を図7に示す。
Claims (16)
- 乾燥前駆体粉末であり、第一材料を含有する第一前駆体を用意する工程、
第一ガスを用意する工程、
高強度場ゾーンと高強度場ゾーンの下流である残照領域とを有するプラズマを用意する工程、
第一ガスおよび第一前駆体をプラズマの高強度場ゾーンを通す工程、
プラズマの高強度場ゾーン内で第一前駆体中の第一材料の少なくとも一部を分解する工程、
乾燥前駆体粉末であり、第二材料を含有する第二前駆体を用意する工程、
第二前駆体を第二ガス中に懸濁させてエアロゾルを製造する工程、
残照領域中にエアロゾルを通し、その際にエアロゾルに高強度場ゾーンを迂回させる工程、
分解した第一材料をプラズマの高強度場ゾーンから除く工程、および
分解した第一材料の少なくとも一部をエアロゾル中の第二材料上に凝縮させて、複合粒子を製造する工程、
を含み、
前記複合粒子を第二前駆体内の第二材料として用い、そして第一前駆体の一部であって且つプラズマの高強度場ゾーンで分解した第三材料をエアロゾル中の複合粒子上に凝縮させて、さらなる複合粒子を製造する工程をさらに含み、
前記さらなる複合粒子を第二前駆体内の第二材料として用い、そして第一前駆体の一部であって且つプラズマの高強度場ゾーンで分解した第四材料をエアロゾル中のさらなる複合粒子上に凝縮させて、よりさらなる複合粒子を製造する工程をさらに含む、
前記よりさらなる複合粒子の製造方法。 - 前記第一前駆体が複数の材料を含有する請求項1に記載の製造方法。
- 前記第一ガス中に前記第一前駆体を懸濁させて、プラズマの高強度場ゾーンを通る第一エアロゾルを製造する工程をさらに含む、請求項1に記載の製造方法。
- 前記第一材料の少なくとも一部を分解する工程が、前記第一材料の少なくとも一部を蒸発させる工程である請求項1に記載の製造方法。
- 前記よりさらなる複合粒子が、ミクロンサイズの粒子、サブミクロンサイズの粒子およびナノメートルサイズの粒子からなる群から選択される粒子である請求項1に記載の製造方法。
[但し、ミクロンサイズの粒子とは1〜1000μmの、サブミクロンサイズの粒子とは200〜1000nmの、そしてナノメートルサイズの粒子とは1〜200nmの平均外径を有する粒子をいう。] - 前記よりさらなる複合粒子が、コア−シェル構造の1〜200nmの平均外径を有する粒子である請求項1に記載の製造方法。
- 前記よりさらなる複合粒子が、分解した第一材料によって部分的に被覆された第二材料で製造されたコアを有する請求項1に記載の製造方法。
- 前記第一材料が、金属、炭素、窒素及び酸素からなる群から選択される1種以上の元素を含有する請求項1に記載の製造方法。
- 前記第二材料が、1〜200nmの平均径を有する粒子状である請求項1に記載の製造方法。
- 前記第二材料が、リチウム化合物である請求項1に記載の製造方法。
- 前記第二材料が、リチウム合金材料である請求項1に記載の製造方法。
- 前記エアロゾルがプラズマの高強度場ゾーン内で終了する管を通る請求項1に記載の製造方法。
- 前記プラズマの高強度場ゾーンを通るプラズマガスを供給する工程をさらに含む、請求項1に記載の製造方法。
- 前記プラズマが、非酸化性のプラズマである請求項1に記載の製造方法。
- 前記よりさらなる複合粒子が、1000nm未満の平均外径を有する請求項1に記載の製造方法。
- 前記よりさらなる複合粒子が、500nm未満の平均外径を有する請求項1に記載の製造方法。
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US12/480,812 US8642139B2 (en) | 2009-06-09 | 2009-06-09 | Process to make structured particles |
US12/480,812 | 2009-06-09 |
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JP2010284646A5 JP2010284646A5 (ja) | 2015-11-19 |
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US20110006254A1 (en) * | 2009-07-07 | 2011-01-13 | Toyota Motor Engineering & Manufacturing North America, Inc. | Process to make electrochemically active/inactive nanocomposite material |
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EP3072582A1 (en) * | 2015-03-27 | 2016-09-28 | Max-Planck-Gesellschaft zur Förderung der Wissenschaften e.V. | Method for encapsulating a nanostructure, coated nanostructure and use of a coated nanostructure |
US20180025889A1 (en) * | 2016-07-22 | 2018-01-25 | Regents Of The University Of Minnesota | Nonthermal plasma synthesis |
US10543534B2 (en) * | 2016-11-09 | 2020-01-28 | Amastan Technologies Inc. | Apparatus and method for the production of quantum particles |
KR101887788B1 (ko) * | 2016-12-19 | 2018-08-10 | 인하대학교 산학협력단 | 타이타늄 및 탄소나노섬유를 포함하는 복합 나노 분말의 제조방법 및 이를 제조하기 위한 플라즈마 장치 |
KR102311541B1 (ko) * | 2017-12-13 | 2021-10-13 | 엘티메탈 주식회사 | 은-카본 나노 복합 입자, 이의 제조방법 및 상기 은-카본 나노 복합 입자를 포함하는 전기 접점 재료 |
CN108193107B (zh) * | 2017-12-21 | 2020-04-10 | 陕西科技大学 | 一种有机包覆核-壳纳米复合储氢材料的制备方法 |
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