JPWO2012168993A1 - オニオンライクカーボンの作製方法 - Google Patents
オニオンライクカーボンの作製方法 Download PDFInfo
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 68
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 23
- 239000007789 gas Substances 0.000 claims abstract description 150
- 239000000843 powder Substances 0.000 claims abstract description 136
- 238000000034 method Methods 0.000 claims abstract description 69
- 238000006243 chemical reaction Methods 0.000 claims abstract description 37
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 30
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 30
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 30
- 239000011261 inert gas Substances 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 11
- 238000005268 plasma chemical vapour deposition Methods 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims description 46
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 25
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 25
- 238000002360 preparation method Methods 0.000 claims description 22
- 239000007858 starting material Substances 0.000 abstract description 9
- 229910021385 hard carbon Inorganic materials 0.000 abstract description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 27
- 238000004458 analytical method Methods 0.000 description 23
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 21
- 229910052786 argon Inorganic materials 0.000 description 14
- -1 hydrogen radicals Chemical class 0.000 description 7
- 238000000354 decomposition reaction Methods 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 3
- 239000005977 Ethylene Substances 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 description 3
- 229910003460 diamond Inorganic materials 0.000 description 3
- 239000010432 diamond Substances 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 239000011733 molybdenum Substances 0.000 description 3
- 238000012805 post-processing Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 229910052754 neon Inorganic materials 0.000 description 2
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 2
- 238000004611 spectroscopical analysis Methods 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 241000234282 Allium Species 0.000 description 1
- 235000002732 Allium cepa var. cepa Nutrition 0.000 description 1
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 150000001485 argon Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 150000001723 carbon free-radicals Chemical class 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000007670 carcinogenicity Effects 0.000 description 1
- 231100000260 carcinogenicity Toxicity 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000009931 harmful effect Effects 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000026683 transduction Effects 0.000 description 1
- 238000010361 transduction Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/18—Nanoonions; Nanoscrolls; Nanohorns; Nanocones; Nanowalls
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S977/00—Nanotechnology
- Y10S977/70—Nanostructure
- Y10S977/773—Nanoparticle, i.e. structure having three dimensions of 100 nm or less
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- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
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- Composite Materials (AREA)
- Manufacturing & Machinery (AREA)
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- Carbon And Carbon Compounds (AREA)
Abstract
Description
Electron Microscope;TEM)で観察したところ、図4に示すような画像が得られた。この図4において、白の破線丸印で囲まれた部分がOLCを示す。即ち、この図4から、OLCの存在が認められる。なお、この図4に示すOLCは、その直前原料としてのDLC粉末100が作製される際に(つまり第1ステップとしてのDLC粉末作製処理において)、当該DLC粉末100の作製温度が200℃とされた以外は、上述の図3に係るのと同じ条件とされたものである。
Claims (12)
- 材料ガスとして炭化水素系ガスを用いたプラズマCVD法によってDLC粉末を作製するDLC粉末作製過程と、
上記DLC粉末作成過程において作製された上記DLC粉末を真空中または不活性ガス雰囲気中で加熱することによって該DLC粉末をオニオンライクカーボンに変換する変換過程と、
を具備する、オニオンライクカーボンの作製方法。 - 上記炭化水素系ガスはアセチレンガスである、
請求項1に記載のオニオンライクカーボンの作製方法。 - 上記DLC粉末作製過程は、
基準電位に接続された真空槽と該真空槽内に設置された開口形状の容器とを一対の電極として該真空槽と該容器とに交流の放電用電力を供給することによって該容器内を含む該真空槽内にプラズマを発生させるプラズマ発生過程と、
上記真空槽内に上記炭化水素系ガスを導入するガス導入過程と、
上記容器内の温度が300℃よりも高くならないように該容器内の温度を制御する温度制御過程と、
を含む、
請求項1または2に記載のオニオンライクカーボンの作製方法。 - 上記ガス導入過程において上記真空槽と絶縁された状態にあるガス導入管を介して上記炭化水素系ガスを該真空槽内に導入すると共に該ガス導入管の該真空槽内への該炭化水素系ガスの噴出口を上記容器の開口部の近傍に位置させ、
上記DLC粉末作製過程は上記ガス導入管に対して上記基準電位を基準とする正電位の直流電力を供給する直流電力供給過程をさらに含む、
請求項3に記載のオニオンライクカーボンの作製方法。 - 上記DLC粉末作製過程は上記容器内に上記プラズマを閉じ込めるための磁場を上記真空槽内に形成する磁場形成過程をさらに含む、
請求項3または4に記載のオニオンライクカーボンの作成方法。 - 上記変換過程は、
上記真空槽内を上記真空または上記不活性ガス雰囲気とする変換環境形成過程と、
上記真空または上記不活性ガス雰囲気とされた上記真空槽内において上記DLC粉末を700℃〜2000℃で加熱する加熱過程と、
を含む、
請求項3ないし5のいずれかに記載のオニオンライクカーボンの作製方法。 - 材料ガスとして炭化水素系ガスを用いたプラズマCVD法によってDLC粉末を作製するDLC粉末作製手段と、
上記DLC粉末作製手段によって作製された上記DLC粉末を真空中または不活性ガス雰囲気中で加熱することによって該DLC粉末をオニオンライクカーボンに変換する変換手段と、
を具備する、オニオンライクカーボンの作製装置。 - 上記炭化水素系ガスはアセチレンガスである、
請求項7に記載のオニオンライクカーボンの作製装置。 - 基準電位に接続された真空槽と、
上記真空槽内に設置された開口形状の容器と、
を具備し、
上記DLC粉末作製手段は、
上記真空槽と上記容器とを一対の電極として該真空槽と該容器とに交流の放電用電力を供給することによって該容器内を含む該真空槽内にプラズマを発生させるプラズマ発生手段と、
上記真空槽内に上記炭化水素系ガスを導入するガス導入手段と、
上記容器内の温度が300℃よりも高くならないように該容器内の温度を制御する温度制御手段と、
を含む、
請求項7または8に記載のオニオンライクカーボンの作製装置。 - 上記ガス導入手段は上記真空槽と絶縁された状態にあるガス導入管を含み、
上記炭化水素系ガスは上記ガス導入管を介して上記真空槽内に導入され、
上記ガス導入管は上記真空槽内への上記炭化水素系ガスの噴出口を上記容器の開口部の近傍に位置させるように設けられ、
上記DLC粉末作製手段は上記ガス導入管に対して上記基準電位を基準とする正電位の直流電力を供給する直流電力供給手段をさらに含む、
請求項9に記載のオニオンライクカーボンの作製装置。 - 上記DLC粉末作製手段は上記容器内に上記プラズマを閉じ込めるための磁場を上記真空槽内に形成する磁場形成手段をさらに含む、
請求項9または10に記載のオニオンライクカーボンの作製装置。 - 上記変換手段は、
上記真空槽内を上記真空または上記不活性ガス雰囲気とする変換環境形成手段と、
上記真空または上記不活性ガス雰囲気とされた上記真空槽内において上記DLC粉末を700℃〜2000℃で加熱する加熱手段と、
を含む、
請求項9ないし11のいずれかに記載のオニオンライクカーボンの作製装置。
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PCT/JP2011/062923 WO2012168993A1 (ja) | 2011-06-06 | 2011-06-06 | オニオンライクカーボンの作製方法 |
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JPWO2012168993A1 true JPWO2012168993A1 (ja) | 2015-02-23 |
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US (1) | US8992880B2 (ja) |
EP (1) | EP2573047B1 (ja) |
JP (1) | JP5159960B2 (ja) |
KR (1) | KR101373640B1 (ja) |
CN (1) | CN102933490B (ja) |
TW (1) | TWI457275B (ja) |
WO (1) | WO2012168993A1 (ja) |
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CN104209062B (zh) * | 2013-05-20 | 2016-07-06 | 燕山大学 | 超高硬度纳米孪晶金刚石块体材料及其制备方法 |
US10160654B2 (en) | 2014-11-13 | 2018-12-25 | Yanshan University | Ultrahard nanotwinned diamond bulk material and method for preparing the same |
US10428197B2 (en) | 2017-03-16 | 2019-10-01 | Lyten, Inc. | Carbon and elastomer integration |
US10920035B2 (en) | 2017-03-16 | 2021-02-16 | Lyten, Inc. | Tuning deformation hysteresis in tires using graphene |
US9862606B1 (en) | 2017-03-27 | 2018-01-09 | Lyten, Inc. | Carbon allotropes |
CN109112330B (zh) * | 2018-08-20 | 2020-10-16 | 东南大学 | 一种纳米洋葱碳增强钛基复合材料及其制备方法 |
CN109207835A (zh) * | 2018-10-12 | 2019-01-15 | 燕山大学 | 一种Fe基宽应用温度自润滑复合材料及其制备方法 |
CN109321849B (zh) * | 2018-10-12 | 2021-04-02 | 燕山大学 | 一种适用于高低温的Fe基自润滑复合材料及其制备方法 |
WO2021040931A1 (en) | 2019-08-29 | 2021-03-04 | Novonix Battery Testing Services Inc. | Lithium transition metal oxide and precursor particulates and methods |
US11309545B2 (en) | 2019-10-25 | 2022-04-19 | Lyten, Inc. | Carbonaceous materials for lithium-sulfur batteries |
US11398622B2 (en) | 2019-10-25 | 2022-07-26 | Lyten, Inc. | Protective layer including tin fluoride disposed on a lithium anode in a lithium-sulfur battery |
US11489161B2 (en) | 2019-10-25 | 2022-11-01 | Lyten, Inc. | Powdered materials including carbonaceous structures for lithium-sulfur battery cathodes |
US11342561B2 (en) | 2019-10-25 | 2022-05-24 | Lyten, Inc. | Protective polymeric lattices for lithium anodes in lithium-sulfur batteries |
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KR900008505B1 (ko) * | 1987-02-24 | 1990-11-24 | 세미콘덕터 에너지 라보라터리 캄파니 리미티드 | 탄소 석출을 위한 마이크로파 강화 cvd 방법 |
JPH11157818A (ja) | 1997-11-21 | 1999-06-15 | Masanori Yoshikawa | オニオングラファイト作製方法およびそのグラファイト製品 |
JP2000109310A (ja) | 1998-08-03 | 2000-04-18 | Osaka Gas Co Ltd | 機能性炭素材料の製法 |
WO2000078674A1 (de) | 1999-06-18 | 2000-12-28 | Carbo-Tec Gesellschaft Für Nano-Und Biotechnische Produkte Mbh | Verfahren zur dynamisch-chemischen herstellung von diamantartigen kohlenstoffstrukturen, diamantartige kohlenstoffstrukturen und verwendungen von diamantartigen kohlenstoffstrukturen |
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JP5375197B2 (ja) * | 2009-02-28 | 2013-12-25 | 伸夫 大前 | オニオンライクカーボンの作製方法 |
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KR101373640B1 (ko) | 2014-03-12 |
EP2573047A4 (en) | 2015-04-15 |
TW201249741A (en) | 2012-12-16 |
EP2573047A1 (en) | 2013-03-27 |
KR20130029762A (ko) | 2013-03-25 |
JP5159960B2 (ja) | 2013-03-13 |
TWI457275B (zh) | 2014-10-21 |
CN102933490B (zh) | 2015-02-11 |
WO2012168993A1 (ja) | 2012-12-13 |
US8992880B2 (en) | 2015-03-31 |
EP2573047B1 (en) | 2018-10-31 |
CN102933490A (zh) | 2013-02-13 |
US20130189178A1 (en) | 2013-07-25 |
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