JP4970619B2 - グラフェン膜の製造方法、電子素子の製造方法および基板へのグラフェン膜の転写方法 - Google Patents
グラフェン膜の製造方法、電子素子の製造方法および基板へのグラフェン膜の転写方法 Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 170
- 229910021389 graphene Inorganic materials 0.000 title claims description 154
- 239000000758 substrate Substances 0.000 title claims description 61
- 238000000034 method Methods 0.000 title claims description 46
- 238000004519 manufacturing process Methods 0.000 title claims description 20
- 229910003481 amorphous carbon Inorganic materials 0.000 claims description 89
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 62
- 229910052733 gallium Inorganic materials 0.000 claims description 61
- 239000007788 liquid Substances 0.000 claims description 42
- 238000010438 heat treatment Methods 0.000 claims description 34
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- 238000012546 transfer Methods 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 3
- 238000010000 carbonizing Methods 0.000 claims description 3
- 238000000151 deposition Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 2
- 239000010408 film Substances 0.000 description 217
- 239000010410 layer Substances 0.000 description 15
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 11
- 239000011347 resin Substances 0.000 description 11
- 229920005989 resin Polymers 0.000 description 11
- 229910052710 silicon Inorganic materials 0.000 description 11
- 239000010703 silicon Substances 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 10
- 229910052799 carbon Inorganic materials 0.000 description 8
- 239000000919 ceramic Substances 0.000 description 8
- 239000013078 crystal Substances 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 6
- 239000004205 dimethyl polysiloxane Substances 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 238000010894 electron beam technology Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 238000005087 graphitization Methods 0.000 description 3
- 229910001338 liquidmetal Inorganic materials 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 2
- 238000002679 ablation Methods 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
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- 238000010586 diagram Methods 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
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- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 2
- 239000004926 polymethyl methacrylate Substances 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 238000002230 thermal chemical vapour deposition Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229920002120 photoresistant polymer Polymers 0.000 description 1
- -1 polydimethylsiloxane Polymers 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 238000013518 transcription Methods 0.000 description 1
- 230000035897 transcription Effects 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
Classifications
-
- 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
- C01B32/182—Graphene
- C01B32/184—Preparation
-
- 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
- C01B32/182—Graphene
- C01B32/194—After-treatment
-
- 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
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/20—Deposition of semiconductor materials on a substrate, e.g. epitaxial growth solid phase epitaxy
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
Description
Novoselov, K. S. et al. "Electric field effect in atomically thin carbon films" Science 306 (2004) 666-669. Meyer JC, et al, "The structure of suspended graphene sheets" Nature. 446(7131) (2007) 60-63. A. J. van Bommel, et al. "A. LEED and Auger electron observations of the SiC(0001) surface" Surf. Sci. 48 (1975) 463-472. I. Forbeaux et al. "Heteroepitaxial graphite on 6H-SiC(0001): Interface formation through conduction-band electronic structure" Phys. Rev. B 58 (1998) 16396-16406. Berger, C. et al. "Ultrathin epitaxial graphite: 2D electron gas properties and a route toward graphene-based nanoelectronics" J. Phys. Chem. B, 108, (2004) 19912-19916. Berger, C. et al. "Electronic confinement and coherence in patterned epitaxial grapheme", Science 312, (2006) 1191-1196. Ohta, T. et al. "Controlling the electronic structure of bilayer grapheme",Science 313 (2006) 951 - 954. T. A. Land, et al. "STM investigation of single layer graphite structures produced on Pt(111) by hydrocarbon decomposition", Sur. Sci. 264 (1992) 261-270. A. Nagashima et al. "Electronic states of monolayer graphite formed on TiC(111) surface", Surf. Sci. 291 (1993) 93-98.
2 蒸留水
3 有機膜
4 セラミックスリング
5 アブレーション用炭素原料
6 YAGレーザー
7 アモルファスカーボン膜
8 液体ガリウム
9 液体ガリウム表面に転写されたアモルファスカーボン膜
10 合成されたグラフェン膜
11 未反応のアモルファスカーボン膜
12 有機シリコン樹脂
13 有機シリコン樹脂表面に転写されたグラフェン膜
14 電子素子基板
<実施例1>
次の手順でグラフェン膜を作製した。まず、蒸留水の上に5%コロジオン液を滴下し、水面上に極薄のコロジオン膜を得た。このコロジオン膜をアルミナセラミックスリングですくい取り、リングの上に膜厚約30nmコロジオン膜を形成した。
<実施例2>
実施例1の手順によりガリウム表面に作製したグラフェン膜の転写を行った。ガリウム表面のグラフェン膜に対してPDMSシートを接触させると、グラフェン膜は一部のガリウムと共にPDMSシート表面に張り付いた(図9(a))。グラフェン膜と共に付着したガリウムを希塩酸中で処理すると、ガリウムが剥がれ、図9(b)の写真に示すようにガリウムを除去した膜がPDMSシート表面に残存した。
<実施例3>アモルファスカーボン膜厚による結晶性の変化
実施例1と同様にして得たアモルファスカーボン膜と液体ガリウムとを接触させ、5×10-4Paの真空中において1000℃または1100℃で30分間熱処理し、アモルファスカーボンと液体ガリウムの接触界面において4〜6層の多層グラフェンを形成した。
<実施例4> グラフェンフィルムの電界効果特性
実施例3において得たグラフェンを300 nmの酸化膜付Si基板に転写し、ステンシルマスクを用いてTi/Au電極を作製し、バックゲート構造を作製した。
<実施例5> Si基板上でのレジストパターンのグラファイト化
図14に示す工程によりグラフェンFETを作製した。シリコン酸化膜上にレジスト(化学増幅法NEBネガレジスト)を薄く(約10nm程度)塗布し、電子線描画でFETチャネルパターン、さらに電子回路パターンを形成した。
Claims (9)
- アモルファスカーボン膜とガリウムとを接触させ、接触界面にグラフェン膜を形成する工程を含むことを特徴とするグラフェン膜の製造方法。
- アモルファスカーボン膜は、有機膜を真空熱処理することによりアモルファス状に炭化させて得たものであることを特徴とする請求項1に記載のグラフェン膜の製造方法。
- アモルファスカーボン膜は、有機膜にアモルファスカーボンを蒸着し、次いで真空熱処理することにより有機膜をアモルファス状に炭化させて得たものであることを特徴とする請求項1に記載のグラフェン膜の製造方法。
- アモルファスカーボン膜を液体ガリウムの表面に転写し、次いで真空熱処理することによりグラフェン膜を形成することを特徴とする請求項1から3のいずれかに記載のグラフェン膜の製造方法。
- 電子素子基板上にレジストを塗布し、電子回路に対応するレジストパターンを形成した後、このレジストパターンに液体ガリウムを接触させ、次いで真空熱処理することにより、レジストパターンをグラフェン化して電子回路を形成する工程を含むことを特徴とする電子素子の製造方法。
- 請求項1から4のいずれかの方法によりアモルファスカーボン膜と金属との接触界面にグラフェン膜を形成した後、アモルファスカーボン膜を基板表面に接触させてグラフェン膜を基板に転写する工程を含むことを特徴とする基板へのグラフェン膜の転写方法。
- 基板が電子素子基板であることを特徴とする請求項6に記載の基板へのグラフェン膜の転写方法。
- 請求項1から4のいずれかの方法によりアモルファスカーボン膜と金属との接触界面にグラフェン膜を形成した後、アモルファスカーボン膜を中間媒体表面に接触させてグラフェン膜を中間媒体に転写する工程と、中間媒体に転写されたグラフェン膜を基板表面に接触させてグラフェン膜を基板に転写する工程とを含むことを特徴とする基板へのグラフェン膜の転写方法。
- 基板および/または中間媒体に転写されたグラフェン膜上に残る金属を酸で洗浄除去する工程をさらに含むことを特徴とする請求項6から8のいずれかに記載の基板へのグラフェン膜の転写方法。
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PCT/JP2010/054602 WO2010110153A1 (ja) | 2009-03-27 | 2010-03-17 | グラフェン膜の製造方法、電子素子の製造方法および基板へのグラフェン膜の転写方法 |
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US (1) | US20120082787A1 (ja) |
EP (1) | EP2412670B1 (ja) |
JP (1) | JP4970619B2 (ja) |
KR (1) | KR101357060B1 (ja) |
CN (1) | CN102438944B (ja) |
WO (1) | WO2010110153A1 (ja) |
Cited By (1)
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WO2012086387A1 (ja) * | 2010-12-21 | 2012-06-28 | 日本電気株式会社 | グラフェン基板の製造方法およびグラフェン基板 |
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KR102225590B1 (ko) * | 2017-09-26 | 2021-03-10 | 고려대학교 산학협력단 | 박막성장방법 및 박막의 결정상태를 바꾸는 방법 |
WO2019070872A1 (en) * | 2017-10-03 | 2019-04-11 | Northwestern University | INTERFACIAL BARRIERS IN GRAPHIC CONDUCTOR FOR ELECTRONIC DEVICES BASED ON LIQUID METAL |
KR102234101B1 (ko) * | 2018-09-21 | 2021-04-01 | 고려대학교 산학협력단 | 박막성장구조, 박막성장방법 및 박막열처리방법 |
CN110963486A (zh) * | 2018-09-28 | 2020-04-07 | 浙江大学 | 一种基于方华层增强石墨烯与柔性基底界面的方法 |
CN116216705A (zh) * | 2022-12-30 | 2023-06-06 | 苏州大学 | 一种碳氢化合物催化制备氧化石墨烯的方法 |
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KR101357060B1 (ko) | 2014-02-03 |
WO2010110153A1 (ja) | 2010-09-30 |
KR20110131225A (ko) | 2011-12-06 |
CN102438944A (zh) | 2012-05-02 |
EP2412670B1 (en) | 2016-06-01 |
CN102438944B (zh) | 2014-07-16 |
US20120082787A1 (en) | 2012-04-05 |
EP2412670A4 (en) | 2014-09-10 |
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JPWO2010110153A1 (ja) | 2012-09-27 |
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