JP6042405B2 - 積層複合体 - Google Patents
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- JP6042405B2 JP6042405B2 JP2014502330A JP2014502330A JP6042405B2 JP 6042405 B2 JP6042405 B2 JP 6042405B2 JP 2014502330 A JP2014502330 A JP 2014502330A JP 2014502330 A JP2014502330 A JP 2014502330A JP 6042405 B2 JP6042405 B2 JP 6042405B2
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- 229910021389 graphene Inorganic materials 0.000 claims description 93
- 239000000758 substrate Substances 0.000 claims description 79
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- 239000007787 solid Substances 0.000 description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910001868 water Inorganic materials 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Natural products CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
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- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
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- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 239000011214 refractory ceramic Substances 0.000 description 1
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- 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
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
- H01L29/16—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, only elements of Group IV of the Periodic Table
- H01L29/1606—Graphene
-
- 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
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02367—Substrates
- H01L21/0237—Materials
- H01L21/0242—Crystalline insulating materials
-
- 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
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02524—Group 14 semiconducting materials
- H01L21/02527—Carbon, e.g. diamond-like carbon
-
- 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
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
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- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
Description
[1] α−酸化アルミニウム単結晶からなるサファイア基板と、該サファイア基板に接して形成されたグラフェン層とを有する積層複合体であって、該サファイア基板が、r面(01−12)で該グラフェン層と接している、積層複合体。
[2] 上記[1]に記載の積層複合体の製造方法であって、該サファイア基板上に、気相成長によって該グラフェン層を形成することを含む、方法。
ID:Dバンドのピーク強度
IG:Gバンドのピーク強度
に従って結晶子サイズLaを算出する。すなわち、測定した装置の条件(λlaser:532nm)およびDバンド/Gバンドの比から、上式に従って結晶子サイズを算出する。結晶子サイズが15nm以上であることは、グラフェンの二次元シートが大きいことを意味し、グラフェンのキャリア移動度が大きくなるという利点を与える。
表面形状は、AFM(NanoscopeIII(Digital Instruments社製)又はXE−100(Park社製))を用いて評価した。表面の形状像が取得され、平滑性は4μm×4μmの観察範囲における形状像の粗度Ra(平均偏差、表面粗度)にて評価した。
(2)結晶子サイズ
ラマンスペクトル測定により、2Dバンド、Gバンド、及びDバンドの強度比から算出した。
ホール効果測定装置:ResiTest8310(東陽テクニカ社製)を用い、van der Pauw法によるホール測定によって、積層複合体を構成するグラフェン層のキャリア移動度、及びシートキャリア濃度を測定した。
積層複合体表面を低エネルギー低速電子線回折(LEED)装置(Omicron社製)にて測定し、グラフェン層及びサファイア基板の結晶方位を取得した。
サファイア単結晶基板を研磨後、洗浄・乾燥させた。乾燥後の基板は、(01−12)から[0001]方向に0.00°、[11−20]方向に0.05°傾斜した面(これは本開示におけるr面に包含される)を有していた。この基板を大気中1200℃で15分間加熱した。上記基板の表面の構造をAFMで確認した。図1は、実施例1で用いたサファイア基板の表面AFM形状像を示す図である。AFM形状像のフルスケールは、x及びy:各4μm、z:2nmである。基板は、その傾斜方向と垂直方向に高さ約0.35nmの段差を有する、幅400〜500nmの直線的なステップ・テラス構造を有していた。表面の粗度Ra=0.09nmであった。基板表面の結晶方位は500/(0.35+500)×100=99.9(%)であり、基板の大部分が面方位(01−12)であることを確認した。
1)サファイアのr面由来の、格子定数4.84Å×5.22Åの面心長方格子による回折スポット。
2)1)の(2 1)点又は(−2 1)点に重なって現れている、グラフェン格子定数2.46Åの六方格子による六角形回折スポット。
3)グラフェンの格子定数2.46Åの無秩序に回転した結晶による薄い円形の回折像。
ここで、1)と相関のある2)の回折像が存在することから、積層複合体において、サファイア基板r面結晶面にグラフェンが直接接して形成されていることが確認された。
洗浄後の、(0001);c面から[11−20]方向に0.02°、[1−100]方向に0.0°傾斜した概略c面を表面とするサファイア単結晶基板を用い、該概略c面の上にグラフェン層を形成したこと以外は、実施例1と同様の工程で積層複合体を作製した。作製した積層複合体は、目視でやや黒かった。積層複合体のグラフェン側の表面を、実施例1と同様に光学顕微鏡で倍率:100倍にて観察した。図5は、比較例1で作製した積層複合体におけるグラフェン側の表面の光学顕微鏡反射像を示す図である。スケールは図2と同じである。反射像では粒状の異物が見られた。
比較例1と同様のc面基板を準備し、グラフェンを気相化学成長させるための原料ガスとして、エチレンガスに代えてエチレン/アルゴン体積濃度比=0.00017%のガスを用い(すなわち、エチレンガスを5分の1に希釈し)、原料ガス導入時間を15分と、実施例1の5倍にしたこと以外は実施例1と同様の手順で、積層複合体を作製した。図6は、比較例2で作製した積層複合体におけるグラフェン側の表面のAFM形状像を示す図である。AFM形状像のフルスケールはx及びy:各4μm、z:50nmである。AFM形状像では、深さ20nmの六角形のへこみが見られたり、高さ数nm以上の粒子凝集体とみられる突起が多く生成していることが確認された。また表面は非常に荒れておりRa=8.0nmであった。
(0001);c面から[11−20]方向に0.05°、[1−100]方向に0.00°傾斜した概略c面を表面とするサファイア単結晶基板の、該概略c面上に、通電加熱した黒鉛からの炭素を全圧1×10-6Paで供給したMBEによって気相成長にてグラフェン層を形成した。基板温度1100℃で20分間気相成長を行ったところ、得られた積層複合体の、2Dバンド/Gバンドの比は0.2、Dバンド/Gバンドの比は1.9であり、2Dバンド半値幅68cm-1、2Dバンド位置2687cm-1であった。これらの値から算出される結晶子サイズは10nmであり、多層グラフェン、すなわちナノグラフェンであった。この積層複合体は電気伝導性を示さず、ホール測定も不可能であった。
Claims (2)
- α−酸化アルミニウム単結晶からなるサファイア基板と、該サファイア基板に接して形成されたグラフェン層とを有する積層複合体であって、該サファイア基板が、r面(01−12)で該グラフェン層と接しており、前記グラフェン層の結晶子サイズが30nm以上200mm以下である、積層複合体。
- 請求項1に記載の積層複合体の製造方法であって、該サファイア基板上に、気相成長によって該グラフェン層を形成することを含む、方法。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2012041836 | 2012-02-28 | ||
JP2012041836 | 2012-02-28 | ||
PCT/JP2013/055215 WO2013129514A1 (ja) | 2012-02-28 | 2013-02-27 | 積層複合体 |
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JPWO2013129514A1 JPWO2013129514A1 (ja) | 2015-07-30 |
JP6042405B2 true JP6042405B2 (ja) | 2016-12-14 |
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JP2014502330A Expired - Fee Related JP6042405B2 (ja) | 2012-02-28 | 2013-02-27 | 積層複合体 |
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JP (1) | JP6042405B2 (ja) |
CN (1) | CN104144875B (ja) |
WO (1) | WO2013129514A1 (ja) |
Families Citing this family (7)
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JP6485868B2 (ja) * | 2015-07-21 | 2019-03-20 | 昭和電工株式会社 | 垂直磁気記録媒体及び磁気記録再生装置 |
JP6485867B2 (ja) * | 2015-07-21 | 2019-03-20 | 昭和電工株式会社 | 垂直磁気記録媒体及び磁気記録再生装置 |
JP6485866B2 (ja) * | 2015-07-21 | 2019-03-20 | 昭和電工株式会社 | 垂直磁気記録媒体の製造方法及び磁気記録再生装置 |
CN105576086B (zh) * | 2015-12-21 | 2017-11-07 | 曹胜伟 | 一种生长氮化镓晶体的复合衬底及其制备方法 |
CN107481913B (zh) | 2016-06-08 | 2019-04-02 | 清华大学 | 一种电子束加工系统 |
CN107473179B (zh) | 2016-06-08 | 2019-04-23 | 清华大学 | 一种表征二维纳米材料的方法 |
CN107479330B (zh) | 2016-06-08 | 2019-02-05 | 清华大学 | 一种采用电子束的光刻方法 |
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JP3920555B2 (ja) * | 2000-10-27 | 2007-05-30 | 株式会社山武 | 接合剤および接合方法 |
JP2010109037A (ja) * | 2008-10-29 | 2010-05-13 | Nec Corp | グラファイト薄膜の切断方法、グラファイト薄膜を備える積層基板、およびこれを用いる電界効果トランジスタ |
US8697230B2 (en) * | 2009-08-31 | 2014-04-15 | Kyushu University | Graphene sheet and method for producing the same |
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