JPWO2011105530A1 - 炭素膜積層体 - Google Patents
炭素膜積層体 Download PDFInfo
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- JPWO2011105530A1 JPWO2011105530A1 JP2012501871A JP2012501871A JPWO2011105530A1 JP WO2011105530 A1 JPWO2011105530 A1 JP WO2011105530A1 JP 2012501871 A JP2012501871 A JP 2012501871A JP 2012501871 A JP2012501871 A JP 2012501871A JP WO2011105530 A1 JPWO2011105530 A1 JP WO2011105530A1
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 118
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 39
- 239000013078 crystal Substances 0.000 claims abstract description 138
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 137
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 80
- 239000000758 substrate Substances 0.000 claims abstract description 79
- 239000010949 copper Substances 0.000 claims abstract description 74
- 229910052802 copper Inorganic materials 0.000 claims abstract description 72
- 239000010408 film Substances 0.000 claims abstract description 56
- 239000010409 thin film Substances 0.000 claims abstract description 56
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 34
- 239000010980 sapphire Substances 0.000 claims abstract description 34
- 238000002230 thermal chemical vapour deposition Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims description 18
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 229910003460 diamond Inorganic materials 0.000 claims description 5
- 239000010432 diamond Substances 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 15
- 239000011889 copper foil Substances 0.000 abstract description 13
- 239000010410 layer Substances 0.000 description 21
- 238000005259 measurement Methods 0.000 description 21
- 238000010438 heat treatment Methods 0.000 description 14
- 239000000463 material Substances 0.000 description 12
- 238000001069 Raman spectroscopy Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000003841 Raman measurement Methods 0.000 description 3
- 238000001530 Raman microscopy Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000002356 single layer Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-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
- 238000000089 atomic force micrograph Methods 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 150000001879 copper Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 238000004590 computer program Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- -1 nickel Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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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
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/186—Preparation by chemical vapour deposition [CVD]
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- C01B32/00—Carbon; Compounds thereof
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- C01B32/182—Graphene
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- C01B32/19—Preparation by exfoliation
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- 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
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
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- 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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Abstract
Description
この銅箔を基材とする手法では銅の表面の特性を利用し、従来のニッケルなど他の金属を用いる手法と比較して、グラフェンを制御性よく合成することが可能である。一方、銅箔を基材として用いた合成手法で得られるグラフェンの結晶サイズは今のところ数十μmが最大である。グラフェンを高性能電子デバイスなどの材料として利用するためには、できるだけ大きな結晶サイズのグラフェンが求められており、結晶サイズの拡大が課題となっている。
[1]単結晶基板と、該基板上にエピタキシャル成長させて形成された銅(111)単結晶薄膜と、該銅(111)単結晶薄膜上に堆積されたグラフェンとを備える炭素膜積層体。
[2]前記単結晶基板は、サファイア(0001)単結晶基板又はダイヤモンド(111)単結晶基板であることを特徴とする上記[1]の炭素膜積層体。
[3]前記単結晶基板は、原子レベルで平坦なテラス面と原子層ステップからなる表面を有するサファイア(0001)単結晶基板又は原子レベルで平坦なテラス面と原子層ステップからなる表面を有するダイヤモンド(111)単結晶基板であることを特徴とする上記[1]の炭素膜積層体。
[4]前記グラフェンは、減圧下で水素ガス及びメタンガスを用いて熱CVD法により形成したものであることを特徴とする上記[1]〜[3]のいずれかの炭素膜積層体。
[5]単結晶基板にエピタキシャル成長させて形成された銅(111)単結晶薄膜上に堆積されたものであることを特徴とするグラフェン。
[6]減圧下で水素ガス及びメタンガスを用いて熱CVD法により形成されたものであることを特徴とする上記[5]のグラフェン。
[7]前記銅(111)単結晶薄膜から剥離して得られる上記[5]又は[6]に記載のグラフェン。
12:サファイア(0001)単結晶基板
14:銅(111)単結晶薄膜
16:グラフェン
以上の結果から、結晶サイズの大きなグラフェンを作成するためには、銅(111)面の領域をもつ銅表面を成膜の基材として使用する。したがって、大面積のグラフェンの成膜には、結晶学的な(111)面をもつ単結晶の銅を用いることが好ましい。
きわめて良好な表面平坦性が出現すると、図2−2、図2−3に示すように、原子レベルで平坦なテラスと原子層の高さの段差、すなわち原子層ステップが周期的に表れる。テラスは結晶学的な表面の結晶方位(−・−・−)と実際の表面の傾斜(−−−)とのなす角度θによって決まる幅をもつ。このような表面を原子間力顕微鏡で観察すると図1のような縞模様のコントラストを得る。
以下に実施例の詳細について述べるが、本発明はこの実施例に限定されるものではない。
サファイア(0001)単結晶基板の詳細なスペックは以下のとおりである。
製造・販売元:株式会社信光社(http://www.shinkosha.com/index.html)
品名:サファイアSTEP基板
材質:Al2O3(サファイア)
面方位:(0001)
大きさ:10mm×10mm×厚さ0.5mm
研磨:片面
面方位公差:0.3°以下
平行度:幅10mmの基材の端と端で0.020mm以下
平坦度:光学的な測定限界以下
表面形状:原子レベルで平坦なテラス面と原子層ステップ(図1参照)
蒸着材料:銅(純度99.99%以上)
予備排気:2.0×10−4Pa
放電気体:アルゴン(純度99.999%)
放電電力:100W(定電力モード)
放電電流:370〜380mA
放電電圧:338〜340V
放電気体圧力:1.3×10−1Pa
放電時間:28分6秒
設定膜厚:1000nm
基板温度:約100℃(成膜時基板ホルダー実測値で106〜113℃)
熱CVDに必要な加熱装置には、試料の急速加熱冷却と温度の精密制御を行うことが可能な、赤外線ゴールドイメージ炉を用いた(以下、加熱炉という)。使用した加熱炉はアルバック理工株式会社製MINI-LAMP-ANNEALER「MILA3000-P-N」であった。
成膜は以下の手順で行った。
(1)サファイア(0001)単結晶基板にエピタキシャル成長させて作成した銅(111)単結晶薄膜(以下、「基材」と呼ぶ)をサファイア基板ごと加熱炉の石英製サンプルステージに乗せた。
(2)加熱炉を閉め、3×10−4Pa以下まで予備真空排気した。
(3)水素ガスを2SCCM流し、加熱炉内の圧力を5.3Paに保った。
(4)この状態で加熱を開始し、基材の温度を室温から1000℃まで5分間かけて上昇させた。
(5)基材の温度が1000℃に達したと同時に、温度を1000℃に保ちながら、水素ガス2SCCMに加えてメタンガス35SCCM流し、圧力を5.3Paから66.5Paに上昇させた。圧力を上昇するのに1分20秒ほど時間を要した。
(6)温度1000℃、水素ガス2SCCM、メタンガス35SCCM、圧力66.5Paを維持し、グラフェンの成膜を行った。成膜時間は20分間であった。
(7)上記状態を20分間保って成膜を行った後、成膜を終了した。終了の手順は、メタンガスを止める→水素ガスを止める→真空排気をスタート→加熱ストップ、で行った。終了手順に要した時間は10秒以下であった。
(8)加熱炉内を真空排気して1×10−3Pa以下の圧力に保ちながら、成膜済みの基材を冷却した。加熱を終了してから300℃まで冷却するのに要した時間はおよそ6分、100℃まで冷却するのに要した時間はおよそ19分であった。
(9)成膜済みの基材が100℃以下に冷却されたのを確認し、真空排気を停止、その後加熱炉に空気を導入して成膜済みの基材を取り出した。
図5の2DバンドとGバンドのピークをそれぞれのバックグラウンドを差し引いてフィッティングし、ピークの面積を算出して強度比を求めたところ、I(2D)/I(G)=3.27であった。したがって、このラマン測定を行った領域(測定用レーザービームのスポットサイズである直径1ミクロンの領域)はグラフェンであることがわかった。
また、本発明の炭素膜積層体において、銅(111)単結晶薄膜の表面に堆積されたグラフェンを、該銅(111)単結晶薄膜から剥離することにより、結晶サイズの大きなグラフェンを得ることができる。
Claims (7)
- 単結晶基板と、該基板上にエピタキシャル成長させて形成された銅(111)単結晶薄膜と、該銅(111)単結晶薄膜上に形成されたグラフェンとを備える炭素膜積層体。
- 前記単結晶基板は、サファイア(0001)単結晶基板又はダイヤモンド(111)単結晶基板であることを特徴とする請求項1に記載の炭素膜積層体。
- 前記単結晶基板は、原子レベルで平坦なテラス面と原子層ステップからなる表面を有するサファイア(0001)単結晶基板又は原子レベルで平坦なテラス面と原子層ステップからなる表面を有するダイヤモンド(111)単結晶基板であることを特徴とする請求項1に記載の炭素膜積層体。
- 前記グラフェンは、減圧下で水素ガス及びメタンガスを用いて熱CVD法により形成したものであることを特徴とする請求項1〜3のいずれか1項に記載の炭素膜積層体。
- 単結晶基板にエピタキシャル成長させて形成された銅(111)単結晶薄膜上に堆積されたものであることを特徴とするグラフェン。
- 減圧下で水素ガス及びメタンガスを用いて熱CVD法により形成されたものであることを特徴とする請求項5に記載のグラフェン。
- 前記銅(111)単結晶薄膜から剥離して得られる請求項5又は6に記載のグラフェン。
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