JP2006347807A - 酸化物焼結体、酸化物透明導電膜、およびこれらの製造方法 - Google Patents
酸化物焼結体、酸化物透明導電膜、およびこれらの製造方法 Download PDFInfo
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- JP2006347807A JP2006347807A JP2005175794A JP2005175794A JP2006347807A JP 2006347807 A JP2006347807 A JP 2006347807A JP 2005175794 A JP2005175794 A JP 2005175794A JP 2005175794 A JP2005175794 A JP 2005175794A JP 2006347807 A JP2006347807 A JP 2006347807A
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- Prior art keywords
- oxide
- sintered body
- oxide sintered
- indium
- film
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- 238000000034 method Methods 0.000 title claims abstract description 102
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 35
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 65
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 63
- 239000010937 tungsten Substances 0.000 claims abstract description 63
- 229910003437 indium oxide Inorganic materials 0.000 claims abstract description 54
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229910052738 indium Inorganic materials 0.000 claims abstract description 43
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000000203 mixture Substances 0.000 claims description 91
- 238000005245 sintering Methods 0.000 claims description 86
- 239000013078 crystal Substances 0.000 claims description 80
- 239000000843 powder Substances 0.000 claims description 68
- 239000011701 zinc Substances 0.000 claims description 47
- 238000002834 transmittance Methods 0.000 claims description 38
- 239000000758 substrate Substances 0.000 claims description 29
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 28
- 229910052725 zinc Inorganic materials 0.000 claims description 28
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 26
- 229910052751 metal Inorganic materials 0.000 claims description 24
- 239000002184 metal Substances 0.000 claims description 24
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 20
- 239000001301 oxygen Substances 0.000 claims description 20
- 229910052760 oxygen Inorganic materials 0.000 claims description 20
- 238000001771 vacuum deposition Methods 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 13
- 239000012298 atmosphere Substances 0.000 claims description 12
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 8
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- 238000007731 hot pressing Methods 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 4
- 238000007733 ion plating Methods 0.000 abstract description 18
- 238000007740 vapor deposition Methods 0.000 abstract description 18
- 238000005336 cracking Methods 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 212
- 238000010894 electron beam technology Methods 0.000 description 62
- 238000005259 measurement Methods 0.000 description 41
- 230000015572 biosynthetic process Effects 0.000 description 38
- 238000002360 preparation method Methods 0.000 description 35
- 238000004458 analytical method Methods 0.000 description 32
- 239000010409 thin film Substances 0.000 description 31
- 239000002994 raw material Substances 0.000 description 28
- 239000002245 particle Substances 0.000 description 19
- 238000012360 testing method Methods 0.000 description 19
- 238000009826 distribution Methods 0.000 description 16
- 238000004453 electron probe microanalysis Methods 0.000 description 16
- 239000004570 mortar (masonry) Substances 0.000 description 16
- 238000000634 powder X-ray diffraction Methods 0.000 description 16
- 238000005211 surface analysis Methods 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 15
- 229910007541 Zn O Inorganic materials 0.000 description 13
- 238000000151 deposition Methods 0.000 description 12
- 239000011521 glass Substances 0.000 description 12
- 238000001704 evaporation Methods 0.000 description 10
- 239000007789 gas Substances 0.000 description 10
- 239000011787 zinc oxide Substances 0.000 description 10
- 238000005566 electron beam evaporation Methods 0.000 description 9
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 230000003746 surface roughness Effects 0.000 description 8
- 238000000313 electron-beam-induced deposition Methods 0.000 description 7
- 230000008020 evaporation Effects 0.000 description 7
- 230000008021 deposition Effects 0.000 description 6
- 239000012535 impurity Substances 0.000 description 5
- 239000000470 constituent Substances 0.000 description 4
- 239000002019 doping agent Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 150000002894 organic compounds Chemical class 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- 229910052718 tin Inorganic materials 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000004973 liquid crystal related substance Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000010891 electric arc Methods 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 238000005401 electroluminescence Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- 229920001903 high density polyethylene Polymers 0.000 description 2
- 239000004700 high-density polyethylene Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 229910052741 iridium Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 229910052762 osmium Inorganic materials 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 229910052702 rhenium Inorganic materials 0.000 description 2
- 229910052707 ruthenium Inorganic materials 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 229910004613 CdTe Inorganic materials 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 235000010724 Wisteria floribunda Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 238000000137 annealing 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
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009694 cold isostatic pressing Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 230000005525 hole transport Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 238000004969 ion scattering spectroscopy Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000007916 tablet composition Substances 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
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Abstract
【解決手段】タングステンを固溶したインジウム酸化物を含有し、タングステンがインジウムに対する原子数比で0.001以上0.034以下含まれ、密度が4.0g/cm3以上6.5g/cm3以下である酸化物焼結体とする。
【選択図】 なし
Description
本発明に係るIn−W−O系酸化物焼結体は、タングステンがW/In原子数比で0.001以上0.034以下の割合で含まれ、密度が4.0g/cm3以上6.5g/cm3以下である。
In−W−O系の酸化物透明導電膜は、前述のように太陽電池や表示デバイスの透明電極用として有用であるが、その理由は、以下の通りである。
平均粒径が1μm以下のIn2O3粉末、および平均粒径が1μm以下のWO3粉末を原料粉末とし、In2O3粉末とWO3粉末を、W/Inの原子数比が0.006となるような割合で調合した。これらの原料を乾式ボールミル、Vブレンダーなどで均一に混合し、カーボン製容器中に給粉して各条件でホットプレス法を用いて焼結した。焼結温度は700〜900℃、圧力は2.45MPa(25kgf/cm2)〜29.40MPa(300kgf/cm2)の範囲から選択し、焼結時間は1時間で一定とした。雰囲気は不活性ガス(Arガス)中で行った。
焼結温度を700℃、焼結時間を0.5時間、焼結圧力を4.91MPaとした以外は、実施例1〜6と同じ条件でホットプレス焼結法で酸化物焼結体タブレットを作製したところ、密度は3.8g/cm3であった。測定結果を表1に示す。
焼結温度を900℃、焼結時間を3時間、焼結圧力を29.40MPaとした以外は、実施例1〜6と同じ条件でホットプレス焼結法で酸化物焼結体タブレットを作製したところ、密度は6.7g/cm3であった。測定結果を表1に示す。
焼結温度を1000℃、焼結時間を1時間、焼結圧力を14.70MPaとした以外は、実施例1〜6と同じ条件でホットプレス焼結法で酸化物焼結体タブレットを作製したところ、密度は6.6g/cm3であった。測定結果を表1に示す。
平均粒径が1μm以下のIn2O3粉末、および平均粒径が1μm以下のWO3粉末、さらに平均粒径が1μm以下のZnO粉末を原料粉末とし、In2O3粉末とWO3粉末を、W/Inの原子数比が0.006、Zn/Inの原子数比が0.00018〜0.017となるような割合で調合し、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。
原料粉末の調合におけるZnO粉末の量をZn/Inの原子数比で0.00015とした以外は、実施例7〜11と同じ条件で常圧焼結法による酸化物焼結体タブレットを作製したところ、密度は3.7g/cm3であった。測定結果を表2に示す。
平均粒径が1μm以下のIn2O3粉末、および平均粒径が1μm以下のWO3粉末を原料粉末とし、In2O3粉末とWO3粉末を、W/Inの原子数比が0.006となるような割合で調合し、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。
焼結温度を1150〜1250℃とし、焼結時間を1〜5時間とした以外は、比較例5と同じ条件で常圧焼結法で酸化物焼結体タブレットを作製したところ、密度は3.4〜3.8g/cm3であった。測定結果を表2に示す。
焼結温度を1300℃とし、焼結時間を5時間とした以外は、比較例5と同じ条件で常圧焼結法で酸化物焼結体タブレットの作製をしたところ、密度は4.1g/cm3であった。測定結果を表2に示す。
平均粒径が1μm以下のIn2O3粉末、および平均粒径が1μm以下のWO3粉末、さらに平均粒径が1μm以下のZnO粉末を原料粉末とし、In2O3粉末とWO3粉末を、W/Inの原子数比が0.012、Zn/Inの原子数比が0.008となるような割合で調合し、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。
焼結時間を0.5時間とした以外は、実施例13と同じ条件で酸化物焼結体タブレットを作製したところ、密度は3.8g/cm3であった。測定結果を表2に示す。
焼結温度を1200℃とし、焼結時間を4時間とした以外は、実施例18と同じ条件で酸化物焼結体タブレットを作製したところ、密度は6.8g/cm3であった。測定結果を表2に示す。
焼結中に焼結炉内に酸素を導入しないこととした以外は、実施例17と同じ条件で常圧焼結法で酸化物焼結体タブレットを作製したところ、密度は6.2g/cm3であった。測定結果を表2に示す。
酸化物焼結体タブレットの組成(W/In原子数比、Zn/In原子数比)を(0.001、0)、(0.025、0)、(0.034、0)として、実施例1〜6と同様に、ホットプレス焼結法で焼結条件を変えて種々の密度の蒸着用焼結体タブレットを作製し、同様に電子ビーム照射による耐久性を調べた。
平均粒径が約10μmのIn2O3粉末を用いた以外は実施例3と同様の条件で酸化物焼結体タブレットを作製したところ、密度は4.5g/cm3であった。また、酸化物焼結体の電子ビーム照射面に対し、四端針法抵抗率計ロレスタEP(ダイアインスツルメンツ社製、MCP−T360型)で電子ビーム照射面である円形面の表面抵抗を測定して比抵抗を算出したところ、0.9kΩcm以下であった。
酸化物焼結体タブレットの組成(W/In原子数比、Zn/In原子数比)を(0.018、0.008)とし、焼結体作製時において、常圧焼結後の冷却の際に焼結炉内に導入していた酸素を止めずに5L/minの割合で酸素導入したまま降温した以外は、実施例14と同様の条件で酸化物焼結体タブレットを作製したところ、密度は4.7g/cm3であった。
実施例1〜19、比較例1〜11の酸化物焼結体タブレットを用いて、プラズマガンを用いた高密度プラズマアシスト蒸着法(HDPE法)による成膜を行い、酸化物焼結体タブレットとしての耐久性を調べた。その結果、実施例1〜19、比較例1〜11で得られた結果と同様の傾向を示しており、密度が4.0〜6.5g/cm3の酸化物焼結体タブレットを使用することで、割れやクラックの発生しない蒸着用タブレットが得られることがわかった。
Claims (14)
- タングステンを固溶したインジウム酸化物を含有し、タングステンがインジウムに対する原子数比で0.001以上0.034以下含まれ、密度が4.0g/cm3以上6.5g/cm3以下であることを特徴とする酸化物焼結体。
- タングステン、亜鉛を固溶したインジウム酸化物を含有し、タングステンがインジウムに対する原子数比で0.001以上0.034以下含まれ、亜鉛がインジウムに対する原子数比で0.00018以上0.017以下含まれ、密度が4.0g/cm3以上6.5g/cm3以下であることを特徴とする酸化物焼結体。
- 金属相が含まれていないことを特徴とする請求項1または2に記載の酸化物焼結体。
- 前記酸化物焼結体の結晶粒径の平均値が10μm以下であることを特徴とした請求項1〜3のいずれかに記載の酸化物焼結体。
- 比抵抗が1kΩcm以下であることを特徴とする請求項1〜4のいずれかに記載の酸化物焼結体。
- タングステンのインジウムに対する原子数比が0.001以上0.034以下となるように酸化インジウム粉末と酸化タングステン粉末を調合し、混合する工程1と、工程1で得られた混合物を、温度:700℃以上900℃以下、時間:1h以上3h未満、圧力:2.45MPa以上29.40MPa以下でホットプレスして酸化物焼結体を得る工程2と、を有することを特徴とする酸化物焼結体の製造方法。
- タングステンのインジウムに対する原子数比が0.001以上0.034以下、亜鉛のインジウムに対する原子数比が0.00018以上0.017以下となるように酸化インジウム粉末と酸化タングステン粉末と酸化亜鉛粉末を調合し、混合する工程1と、工程1で得られた混合物を、温度:700℃以上900℃以下、時間:1h以上3h未満、圧力:2.45MPa以上29.40MPa以下でホットプレスして酸化物焼結体を得る工程2と、を有することを特徴とする酸化物焼結体の製造方法。
- タングステンのインジウムに対する原子数比が0.001以上0.034以下となるように酸化インジウム粉末と酸化タングステン粉末を調合し、混合する工程1と、工程1で得られた混合物を、圧力:9.8MPa以上294MPa以下の冷間静水圧プレスで成形して成形体を得る工程2と、工程2で得られた成形体を、常圧で、温度:1300℃以上、時間:5h以上で焼結させて酸化物焼結体を得る工程3と、を有することを特徴とする酸化物焼結体の製造方法。
- タングステンのインジウムに対する原子数比が0.001以上0.034以下、亜鉛のインジウムに対する原子数比が0.00018以上0.017以下となるように酸化インジウム粉末と酸化タングステン粉末と酸化亜鉛粉末を調合し、混合する工程1と、工程1で得られた混合物を、圧力:9.8MPa以上294MPa以下の冷間静水圧プレスで成形して成形体を得る工程2と、工程2で得られた成形体を、常圧で、温度:1000℃以上1300℃以下、時間:1h以上5h以下で焼結させて酸化物焼結体を得る工程3と、を有することを特徴とする酸化物焼結体の製造方法。
- 焼結工程を、焼結炉内に、炉内容積0.1m3当たり3〜8L/minの割合の酸素を導入する雰囲気で実施する請求項8または9に記載の酸化物焼結体の製造方法。
- 焼結工程の後の炉冷を行うに際して、酸素の導入を中止する請求項10に記載の酸化物焼結体の製造方法。
- 請求項1〜5のいずれかに記載の酸化物焼結体のタブレットを用い、真空蒸着法によって作製された酸化物透明導電膜であって、比抵抗が9×10-4Ωcm以下であり、波長400〜800nmの光に対する膜自体の平均透過率が82%以上であることを特徴とする酸化物透明導電膜。
- 波長900〜1100nmの光に対する膜自体の平均透過率が80%以上であることを特徴とする請求項12に記載の酸化物透明導電膜。
- 請求項1〜5のいずれかに記載の酸化物焼結体のタブレットを用いて、130℃以下の基板上に真空蒸着法によって膜を作製した後、作製した膜を不活性ガス中または真空中で200〜400℃で熱処理をすることを特徴とする酸化物透明導電膜の製造方法。
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Also Published As
Publication number | Publication date |
---|---|
KR100819621B1 (ko) | 2008-04-04 |
EP1734150B1 (en) | 2011-03-09 |
TWI323724B (en) | 2010-04-21 |
ES2362615T3 (es) | 2011-07-08 |
TW200708482A (en) | 2007-03-01 |
EP1734150A1 (en) | 2006-12-20 |
KR20060131657A (ko) | 2006-12-20 |
DE602006020522D1 (de) | 2011-04-21 |
JP4760154B2 (ja) | 2011-08-31 |
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