JP2016034888A - 酸化物焼結体、スパッタリング用ターゲット、及びそれを用いて得られる酸化物半導体薄膜 - Google Patents
酸化物焼結体、スパッタリング用ターゲット、及びそれを用いて得られる酸化物半導体薄膜 Download PDFInfo
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- 239000010409 thin film Substances 0.000 title claims abstract description 93
- 239000004065 semiconductor Substances 0.000 title claims abstract description 58
- 238000005477 sputtering target Methods 0.000 title claims abstract description 18
- 239000011701 zinc Substances 0.000 claims abstract description 85
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 63
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 49
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 45
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229910052738 indium Inorganic materials 0.000 claims abstract description 34
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000004544 sputter deposition Methods 0.000 claims abstract description 20
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 claims description 24
- 239000000758 substrate Substances 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000002441 X-ray diffraction Methods 0.000 claims description 9
- 238000012545 processing Methods 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 239000012071 phase Substances 0.000 description 104
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 60
- 238000005245 sintering Methods 0.000 description 30
- 239000000843 powder Substances 0.000 description 29
- 239000011787 zinc oxide Substances 0.000 description 28
- 239000010408 film Substances 0.000 description 24
- 229910052760 oxygen Inorganic materials 0.000 description 21
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 19
- 239000001301 oxygen Substances 0.000 description 19
- 230000015572 biosynthetic process Effects 0.000 description 17
- 238000000034 method Methods 0.000 description 16
- 239000002994 raw material Substances 0.000 description 16
- 229910003437 indium oxide Inorganic materials 0.000 description 13
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 13
- 238000002425 crystallisation Methods 0.000 description 12
- 230000008025 crystallization Effects 0.000 description 12
- 239000000203 mixture Substances 0.000 description 11
- 239000002245 particle Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 7
- 239000004973 liquid crystal related substance Substances 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 description 6
- 229910001195 gallium oxide Inorganic materials 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000001039 wet etching Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 238000001312 dry etching Methods 0.000 description 3
- 238000004993 emission spectroscopy Methods 0.000 description 3
- 230000001747 exhibiting effect Effects 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 230000031700 light absorption Effects 0.000 description 3
- 108091006149 Electron carriers Proteins 0.000 description 2
- 230000005355 Hall effect Effects 0.000 description 2
- 229910021417 amorphous silicon Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000007733 ion plating Methods 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000002250 progressing effect Effects 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 206010021143 Hypoxia Diseases 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- -1 argon and oxygen Chemical compound 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000009694 cold isostatic pressing Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
Description
100×I[In2Ga2ZnO7相(0010)]/{I[In2O3相(400)]+I[In2Ga2ZnO7相(0010)]} [%]・・・・式1
(式中、I[In2O3相(400)]は、ビックスバイト型構造のIn2O3相の(400)ピーク強度であり、[In2Ga2ZnO7相(0010)]は、Yb2Fe3O7型構造のIn2Ga2ZnO7相(0010)ピーク強度を示す。)
本発明の酸化物焼結体は、主にビックスバイト型構造のIn2O3相及びβ−Ga2O3型構造のGaInO3相によって構成されることが好ましい。ここでガリウムはIn2O3相に固溶する、あるいはGaInO3相を構成することが好ましい。ガリウムは、In2O3相に固溶する場合には、正三価イオンであるインジウムの格子位置を置換する。焼結が進行しないなどの理由によって、ガリウムがIn2O3相に固溶しにくい、あるいはβ−Ga2O3型構造のGaInO3相が生成しにくくなり、その結果として、β−Ga2O3型構造のGa2O3相を形成することは好ましくない。Ga2O3相は導電性に乏しいため、異常放電の原因となる。
(式中、I[In2O3相(400)]は、ビックスバイト型構造のIn2O3相の(400)ピーク強度であり、[In2Ga2ZnO7相(0010)]は、Yb2Fe3O7型構造のIn2Ga2ZnO7相(0010)ピーク強度を示す。)
本発明の酸化物焼結体は、酸化インジウム粉末と酸化ガリウム粉末からなる酸化物粉末、ならびに酸化亜鉛粉末を原料粉末とする。
本発明のターゲットは、上記酸化物焼結体を所定の大きさに切断加工することで得られる。ターゲットとして用いる場合には、さらに表面を研磨加工し、バッキングプレートに接着して得ることができる。ターゲット形状は、平板形が好ましいが、円筒形でもよい。円筒形ターゲットを用いる場合には、ターゲット回転によるパーティクル発生を抑制することが好ましい。また、上記酸化物焼結体を、例えば円柱形状に加工してタブレットとし、蒸着法やイオンプレーティング法による成膜に使用することができる。
本発明の結晶質の酸化物半導体薄膜は、主に前記のスパッタリング用ターゲットを用いて、スパッタリング法で基板上に一旦非晶質の酸化物薄膜を形成し、次いで熱処理を施すことによって得られる。
得られた酸化物焼結体の金属元素の組成をICP発光分光法によって調べた。得られた酸化物焼結体の端材を用いて、X線回折装置(フィリップス製)を用いて粉末法による生成相の同定を行った。
得られた酸化物薄膜の組成をICP発光分光法によって調べた。酸化物薄膜の膜厚は表面粗さ計(テンコール社製)で測定した。成膜速度は、膜厚と成膜時間から算出した。酸化物薄膜のキャリア濃度及び移動度は、ホール効果測定装置(東陽テクニカ製)によって求めた。膜の生成相はX線回折測定によって同定した。
酸化インジウム粉末と酸化ガリウム粉末、ならびに酸化亜鉛粉末を平均粒径1.0μm以下となるよう調整して原料粉末とした。これらの原料粉末を、表1の実施例及び比較例のGa/(In+Ga)原子数比、Zn/(In+Ga+Zn)原子数比の通りになるように調合し、水とともに樹脂製ポットに入れ、湿式ボールミルで混合した。この際、硬質ZrO2ボールを用い、混合時間を18時間とした。混合後、スラリーを取り出し、濾過、乾燥、造粒した。造粒物を、冷間静水圧プレスで3ton/cm2の圧力をかけて成形した。
(式中、I[In2O3相(400)]は、ビックスバイト型構造のIn2O3相の(400)ピーク強度であり、[In2Ga2ZnO7相(0010)]は、Yb2Fe3O7型構造のIn2Ga2ZnO7相(0010)ピーク強度を示す。)
表1の結果より、実施例1〜14では、ガリウム含有量がGa/(In+Ga)原子数比で0.08以上0.20未満であり、亜鉛の含有量がZn/(In+Ga+Zn)原子量比で0.0001以上0.08未満の場合には、ビックスバイト型構造のIn2O3相とGaInO3相、あるいはビックスバイト型構造のIn2O3相とβ−Ga2O3型構造のGaInO3相と(Ga,In)2O3相、あるいはビックスバイト型構造のIn2O3相とβ−Ga2O3型構造のGaInO3相とYb2Fe3O7型構造のIn2Ga2ZnO7相によって構成されていた。
Claims (11)
- インジウム、ガリウム及び亜鉛を酸化物として含有し、
前記ガリウムの含有量がGa/(In+Ga)原子数比で0.08以上0.20未満であり、
前記亜鉛の含有量がZn/(In+Ga+Zn)原子数比で0.0001以上0.08未満であることを特徴とする酸化物焼結体。 - 前記亜鉛の含有量がZn/(In+Ga+Zn)原子数比で0.01以上0.05以下である請求項1に記載の酸化物焼結体。
- 前記ガリウムの含有量がGa/(In+Ga)原子数比で0.08以上0.15以下である請求項1又は2に記載の酸化物焼結体。
- 亜鉛以外の正二価元素、及び、インジウムとガリウム以外の正三価から正六価の元素、を実質的に含有しない請求項1から3のいずれかに記載の酸化物焼結体。
- ビックスバイト型構造のIn2O3相と、In2O3相以外の生成相がβ−Ga2O3型構造のGaInO3相、β−Ga2O3型構造のGaInO3相と(Ga,In)2O3相、β−Ga2O3型構造のGaInO3相とYb2Fe3O7型構造のIn2Ga2ZnO7相、(Ga,In)2O3相とYb2Fe3O7型構造のIn2Ga2ZnO7相、及びβ−Ga2O3型構造のGaInO3相と(Ga,In)2O3相とYb2Fe3O7型構造のIn2Ga2ZnO7相からなる群より選ばれた生成相によって構成される請求項1から4のいずれかに記載の酸化物焼結体。
- 下記の式1で定義されるYb2Fe3O7型構造のIn2Ga2ZnO7相のX線回折ピーク強度比が43%以下の範囲である請求項5に記載の酸化物焼結体。
100×I[In2Ga2ZnO7相(0010)]/{I[In2O3相(400)]+I[In2Ga2ZnO7相(0010)]} [%]・・・・式1
(式中、I[In2O3相(400)]は、ビックスバイト型構造のIn2O3相の(400)ピーク強度であり、[In2Ga2ZnO7相(0010)]は、Yb2Fe3O7型構造のIn2Ga2ZnO7相(0010)ピーク強度を示す。) - 請求項1から6のいずれかに記載の酸化物焼結体を加工して得られるスパッタリング用ターゲット。
- 請求項7に記載のスパッタリング用ターゲットを用いてスパッタリング法によって基板上に形成された後、酸化性雰囲気における熱処理によって結晶化させた結晶質の酸化物半導体薄膜。
- キャリア移動度が10cm2/V・s以上である請求項8に記載の酸化物半導体薄膜。
- キャリア移動度が15cm2/V・s以上である請求項8に記載の酸化物半導体薄膜。
- キャリア濃度が8.0×1017cm−3以下である請求項8から10のいずれかに記載の酸化物半導体薄膜。
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