JP2011202246A - 酸化物蒸着材と透明導電膜 - Google Patents
酸化物蒸着材と透明導電膜 Download PDFInfo
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- JP2011202246A JP2011202246A JP2010071801A JP2010071801A JP2011202246A JP 2011202246 A JP2011202246 A JP 2011202246A JP 2010071801 A JP2010071801 A JP 2010071801A JP 2010071801 A JP2010071801 A JP 2010071801A JP 2011202246 A JP2011202246 A JP 2011202246A
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- film
- vapor deposition
- oxide
- deposition material
- oxygen
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- 239000000463 material Substances 0.000 title claims abstract description 182
- 230000008021 deposition Effects 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 85
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 43
- 229910003437 indium oxide Inorganic materials 0.000 claims abstract description 35
- 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 35
- 238000000151 deposition Methods 0.000 claims abstract description 26
- 238000007740 vapor deposition Methods 0.000 claims description 174
- 239000002994 raw material Substances 0.000 claims description 15
- 238000010894 electron beam technology Methods 0.000 claims description 13
- 238000007733 ion plating Methods 0.000 claims description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 125
- 229910052760 oxygen Inorganic materials 0.000 abstract description 125
- 239000001301 oxygen Substances 0.000 abstract description 125
- 239000000203 mixture Substances 0.000 abstract description 57
- 238000004519 manufacturing process Methods 0.000 abstract description 29
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 abstract description 20
- 229910001882 dioxygen Inorganic materials 0.000 abstract description 20
- 238000001771 vacuum deposition Methods 0.000 abstract description 16
- 230000001603 reducing effect Effects 0.000 abstract description 4
- 239000010408 film Substances 0.000 description 266
- 230000015572 biosynthetic process Effects 0.000 description 69
- 239000011135 tin Substances 0.000 description 61
- 238000002156 mixing Methods 0.000 description 48
- 239000000843 powder Substances 0.000 description 43
- 239000000758 substrate Substances 0.000 description 39
- 229910052718 tin Inorganic materials 0.000 description 36
- 230000000052 comparative effect Effects 0.000 description 34
- 239000007789 gas Substances 0.000 description 34
- 238000002834 transmittance Methods 0.000 description 25
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 22
- 238000005245 sintering Methods 0.000 description 20
- 238000011156 evaluation Methods 0.000 description 19
- 239000002245 particle Substances 0.000 description 17
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 13
- 229910001887 tin oxide Inorganic materials 0.000 description 13
- 229910052786 argon Inorganic materials 0.000 description 11
- 229910006404 SnO 2 Inorganic materials 0.000 description 10
- 238000001704 evaporation Methods 0.000 description 10
- 206010021143 Hypoxia Diseases 0.000 description 9
- 230000008020 evaporation Effects 0.000 description 9
- 238000000465 moulding Methods 0.000 description 8
- 239000010409 thin film Substances 0.000 description 8
- 239000011230 binding agent Substances 0.000 description 7
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 6
- 238000013461 design Methods 0.000 description 6
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- 230000000694 effects Effects 0.000 description 6
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- 229910052738 indium Inorganic materials 0.000 description 6
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 6
- 230000009467 reduction Effects 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 238000005566 electron beam evaporation Methods 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
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- 238000012360 testing method Methods 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 238000010494 dissociation reaction Methods 0.000 description 4
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- 238000007254 oxidation reaction Methods 0.000 description 4
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 4
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- 229910052751 metal Inorganic materials 0.000 description 3
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 2
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- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
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- 241000238876 Acari Species 0.000 description 1
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- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 230000005355 Hall effect Effects 0.000 description 1
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- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
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- 239000002313 adhesive film Substances 0.000 description 1
- 230000002411 adverse Effects 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
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005401 electroluminescence Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
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- 239000011737 fluorine Substances 0.000 description 1
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- 239000008187 granular material Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 229920001903 high density polyethylene Polymers 0.000 description 1
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- 230000001771 impaired effect Effects 0.000 description 1
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- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
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- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
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- 238000000859 sublimation Methods 0.000 description 1
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- 230000009974 thixotropic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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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
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- C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
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- C01P2006/00—Physical properties of inorganic compounds
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/3286—Gallium oxides, gallates, indium oxides, indates, thallium oxides, thallates or oxide forming salts thereof, e.g. zinc gallate
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Abstract
【解決手段】この酸化物蒸着材は、酸化インジウムを主成分としSn/In原子数比で0.001〜0.614のスズを含む酸化物焼結体により構成され、CIE1976表色系におけるL*値が54〜75であることを特徴とする。L*値が54〜75である本発明の酸化物蒸着材は最適な酸素量を有するため、成膜真空槽への酸素ガス導入量が少なくても低抵抗で可視域における高透過性の透明導電膜を真空蒸着法で製造でき、酸素ガスの導入量が少ないため膜と蒸着材との組成差を小さくすることができ、量産時の膜組成の変動や特性の変動も低減することが可能となる。
【選択図】なし
Description
酸化物蒸着材において、
酸化インジウムを主成分とし、スズを含む酸化物焼結体により構成され、かつ、スズの含有量がSn/In原子数比で0.001〜0.614であり、CIE1976表色系におけるL*値が54〜75であることを特徴とし、
請求項2に係る発明は、
請求項1に記載の発明に係る酸化物蒸着材において、
上記スズの含有量がSn/In原子数比で0.040〜0.163であることを特徴とする。
酸化インジウムを主成分とし、スズを含む透明導電膜において、
請求項1に記載の酸化物蒸着材を原料として用い、電子ビーム蒸着法、イオンプレーティング法若しくは高密度プラズマアシスト蒸着法により成膜された結晶性の透明導電膜で構成され、かつ、スズの含有量がSn/In原子数比で0.001〜0.614であることを特徴とし、
請求項4に係る発明は、
請求項3に記載の発明に係る透明導電膜において、
請求項2に記載の酸化物蒸着材を原料として用い、電子ビーム蒸着法、イオンプレーティング法若しくは高密度プラズマアシスト蒸着法により成膜された結晶性の透明導電膜で構成され、かつ、スズの含有量がSn/In原子数比で0.040〜0.163であり、比抵抗が3.5×10-4Ωcm以下であることを特徴とする。
本発明の酸化物蒸着材は、酸化インジウムを主成分とし、かつ、スズがSn/In原子数比で0.001〜0.614の割合で含有された組成を有する。そして、本発明の酸化物蒸着材を用いて真空蒸着法により製造された透明導電膜の組成は、酸化物蒸着材の組成に極めて近いため、製造される膜組成も、酸化インジウムを主成分としかつSn/In原子数比でスズが0.001〜0.614の割合だけ含有する組成となる。スズを上記割合だけ含有させる理由としては、酸化インジウム膜の移動度を増加させることができるからである。膜組成、すなわち酸化物蒸着材組成のスズ含有量(Sn/In原子数比)が0.001未満では、キャリア濃度増加の効果(すなわち移動度増加の効果)が小さくて低抵抗の膜を得ることができない。また、0.614を超えると、膜中のスズ量が多過ぎて、電子移動の際の中性不純物散乱が大きくなってしまい、移動度が低下する影響を受けてしまい低抵抗の膜が得られない。より高いキャリア濃度を発揮して低抵抗の膜を得るためのより好ましいスズの含有量は、Sn/In原子数比で0.040〜0.163であり、更にその膜が結晶膜であることである。
酸化インジウムを主成分としスズを含む酸化物焼結体により構成され、スズの含有量がSn/In原子数比で0.001〜0.614で、CIE1976表色系におけるL*値が54〜75である本発明に係る酸化物蒸着材を適用し、電子ビーム蒸着法、イオンプレーティング法や高密度プラズマアシスト蒸着法等の各種真空蒸着法により、スズを含有する酸化インジウムの結晶膜(透明導電膜)を製造することができる。
酸化物蒸着材の作製
平均粒径が0.8μmのIn2O3粉末、および、平均粒径が1μmのSnO2粉末を原料粉末とし、これ等のIn2O3粉末とSnO2粉末を、Sn/Inの原子数比が0.048となるような割合で調合し、かつ、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20時間とした。
(1)透明導電膜の作製には磁場偏向型電子ビーム蒸着装置を用いた。
実施例1〜4において、焼結体酸素量調整工程における導入ガスの混合比のみを変えて酸化物焼結体を製造した。すなわち、比較例1では、O2/Ar流量比で30/70とし、比較例2では100/0とした。得られた焼結体について、密度、比抵抗、結晶粒経、組成を同様に評価したが実施例1〜4と同等であった。得られた酸化物焼結体の表面と内部の色身は同等であり、そのL*値を測定したところ表1のような値を示した。
次に、特開平5−112866号公報(参考公報)に紹介されたスパッタターゲットの焼結体作製技術に従ってスズを含有する酸化インジウム焼結体を製造した。
In2O3粉末とSnO2粉末を調合する際、Sn/Inの原子数比が0.102となるような割合で調合した以外は、焼結体酸素量調整の条件も含めて実施例1〜4と全く同様の条件で実施例5〜8の酸化物焼結体(酸化物蒸着材)を作製した。
比較例1〜2において、In2O3粉末とSnO2粉末を調合する際のSn/Inの原子数比を0.102とした以外は、比較例1〜2と同様の条件で酸化物蒸着材を作製した。すなわち、焼結体酸素量調整の条件が、比較例4では、O2/Ar流量比で30/70とし、比較例5では100/0とした。得られた焼結体について、密度、比抵抗、結晶粒経、組成を同様に評価したが、実施例5〜8と同等であった。また、得られた焼結体の表面と内部の色身は同等であり、そのL*値を測定したところ、表1のような値を示した。
比較例3において、In2O3粉末とSnO2粉末を調合する際のSn/Inの原子数比を0.102とした以外は、比較例3と同様の条件で酸化物蒸着材を作製した。得られた焼結体について、密度、比抵抗、結晶粒経、組成を同様に評価したが、比較例3と同等であった。また、得られた焼結体の表面と内部の色身は同等であり、そのL*値を測定したところ表1のような値を示した。
In2O3粉末とSnO2粉末を調合する際の配合割合が、Sn/In原子数比で0.001(実施例9)、0.009(実施例10)、0.028(実施例11)、0.163(実施例12)、0.230(実施例13)および0.614(実施例14)となるように変化させた以外は、実施例2と同じ条件(すなわち、酸素ガス/アルゴンガス流量比が「60/40」の条件)で実施例9〜14の酸化物焼結体(酸化物蒸着材)を作製した。
次に、特開平8−104978号公報(特許文献1)に紹介されたITO酸化物蒸着材を製造して同様の評価を行った。
また、特開2007−84881号公報(特許文献2)に紹介されたITO酸化物蒸着材を製造して同様の評価を行った。
Claims (4)
- 酸化インジウムを主成分とし、スズを含む酸化物焼結体により構成され、かつ、スズの含有量がSn/In原子数比で0.001〜0.614であり、CIE1976表色系におけるL*値が54〜75であることを特徴とする酸化物蒸着材。
- 上記スズの含有量がSn/In原子数比で0.040〜0.163であることを特徴とする請求項1に記載の酸化物蒸着材。
- 酸化インジウムを主成分とし、スズを含む透明導電膜において、
請求項1に記載の酸化物蒸着材を原料として用い、電子ビーム蒸着法、イオンプレーティング法若しくは高密度プラズマアシスト蒸着法により成膜された結晶性の透明導電膜で構成され、かつ、スズの含有量がSn/In原子数比で0.001〜0.614であることを特徴とする透明導電膜。 - 請求項2に記載の酸化物蒸着材を原料として用い、電子ビーム蒸着法、イオンプレーティング法若しくは高密度プラズマアシスト蒸着法により成膜された結晶性の透明導電膜で構成され、かつ、スズの含有量がSn/In原子数比で0.040〜0.163であり、比抵抗が3.5×10-4Ωcm以下であることを特徴とする請求項3に記載の透明導電膜。
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CN201180014684.5A CN102812150B (zh) | 2010-03-26 | 2011-02-21 | 氧化物蒸镀材料和透明导电膜 |
PCT/JP2011/054413 WO2011118334A1 (ja) | 2010-03-26 | 2011-02-21 | 酸化物蒸着材と透明導電膜 |
KR1020127023103A KR101322800B1 (ko) | 2010-03-26 | 2011-02-21 | 산화물 증착재와 투명 도전막 |
MYPI2012700666A MY159313A (en) | 2010-03-26 | 2011-02-21 | Oxide evaporation material and method for producing the same |
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JP2015108192A (ja) * | 2012-06-07 | 2015-06-11 | 日東電工株式会社 | 透明導電性フィルム |
US20190062900A1 (en) * | 2016-02-29 | 2019-02-28 | Sumitomo Metal Mining Co., Ltd. | Oxide sintered body and sputtering target |
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JP7378938B2 (ja) * | 2019-02-22 | 2023-11-14 | 日東電工株式会社 | 光透過性導電フィルム |
JP7378937B2 (ja) * | 2019-02-22 | 2023-11-14 | 日東電工株式会社 | 光透過性導電フィルム |
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CN112466509B (zh) * | 2020-11-20 | 2022-04-15 | 无锡晶睿光电新材料有限公司 | 一种低温高耐磨导电银浆及其制备方法 |
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US20190062900A1 (en) * | 2016-02-29 | 2019-02-28 | Sumitomo Metal Mining Co., Ltd. | Oxide sintered body and sputtering target |
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