JP2019196521A - 複合タングステン酸化物膜及びその製造方法、並びに該膜を有する膜形成基材及び物品 - Google Patents
複合タングステン酸化物膜及びその製造方法、並びに該膜を有する膜形成基材及び物品 Download PDFInfo
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- JP2019196521A JP2019196521A JP2018090939A JP2018090939A JP2019196521A JP 2019196521 A JP2019196521 A JP 2019196521A JP 2018090939 A JP2018090939 A JP 2018090939A JP 2018090939 A JP2018090939 A JP 2018090939A JP 2019196521 A JP2019196521 A JP 2019196521A
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- 239000002131 composite material Substances 0.000 title claims abstract description 122
- 229910001930 tungsten oxide Inorganic materials 0.000 title claims abstract description 120
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 title claims abstract description 119
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 31
- 239000000463 material Substances 0.000 title claims abstract description 18
- 238000002834 transmittance Methods 0.000 claims abstract description 28
- 239000000203 mixture Substances 0.000 claims abstract description 23
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 19
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000001301 oxygen Substances 0.000 claims abstract description 18
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 18
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical group [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000010937 tungsten Substances 0.000 claims abstract description 14
- 229910052738 indium Inorganic materials 0.000 claims abstract description 11
- 229910052742 iron Inorganic materials 0.000 claims abstract description 10
- 229910052716 thallium Inorganic materials 0.000 claims abstract description 10
- 229910052718 tin Inorganic materials 0.000 claims abstract description 10
- 239000002585 base Substances 0.000 claims abstract description 9
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 7
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 7
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims abstract description 7
- 150000001342 alkaline earth metals Chemical class 0.000 claims abstract description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 62
- 238000010438 heat treatment Methods 0.000 claims description 53
- 239000000758 substrate Substances 0.000 claims description 46
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- 238000000034 method Methods 0.000 claims description 37
- 239000007789 gas Substances 0.000 claims description 31
- 238000004544 sputter deposition Methods 0.000 claims description 22
- 239000011521 glass Substances 0.000 claims description 16
- 239000011261 inert gas Substances 0.000 claims description 8
- 229910052701 rubidium Inorganic materials 0.000 claims description 4
- 238000002835 absorbance Methods 0.000 claims description 3
- 229910052792 caesium Inorganic materials 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 229910052712 strontium Inorganic materials 0.000 claims description 3
- 230000006870 function Effects 0.000 abstract description 52
- 230000035699 permeability Effects 0.000 abstract description 8
- 239000010408 film Substances 0.000 description 279
- 239000010419 fine particle Substances 0.000 description 29
- 238000006243 chemical reaction Methods 0.000 description 20
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- 238000005477 sputtering target Methods 0.000 description 18
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- 238000010521 absorption reaction Methods 0.000 description 14
- 230000003287 optical effect Effects 0.000 description 11
- 230000008569 process Effects 0.000 description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 10
- 150000001875 compounds Chemical class 0.000 description 10
- 229910001882 dioxygen Inorganic materials 0.000 description 10
- 238000000576 coating method Methods 0.000 description 9
- 230000031700 light absorption Effects 0.000 description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
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- 239000000243 solution Substances 0.000 description 6
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- 229910052786 argon Inorganic materials 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- VPXSRGLTQINCRV-UHFFFAOYSA-N dicesium;dioxido(dioxo)tungsten Chemical compound [Cs+].[Cs+].[O-][W]([O-])(=O)=O VPXSRGLTQINCRV-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
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- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 230000001590 oxidative effect Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
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- 230000008021 deposition Effects 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
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- 230000007774 longterm Effects 0.000 description 3
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- -1 tungsten oxide compound Chemical class 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
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- 150000004767 nitrides Chemical class 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- OHUPZDRTZNMIJI-UHFFFAOYSA-N [Cs].[W] Chemical compound [Cs].[W] OHUPZDRTZNMIJI-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
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- 239000000470 constituent Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
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- 238000005265 energy consumption Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000000383 hazardous chemical 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
- 230000001771 impaired effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 208000035824 paresthesia Diseases 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000009751 slip forming Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 239000005341 toughened glass Substances 0.000 description 1
- 150000003658 tungsten compounds Chemical class 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 239000011800 void material 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
- 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
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
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- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
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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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Abstract
Description
(1)成膜工程において、不活性ガス中でスパッタリング成膜した後、熱処理工程において、膜を酸素が含まれるガス中で400℃〜600℃の温度で熱処理する。
(2)成膜工程において、酸素を含むガス中でスパッタリング成膜した後、熱処理工程において、膜を不活性雰囲気中または還元雰囲気中で400℃〜900℃の温度で熱処理する。
1.複合タングステン酸化物膜
2.複合タングステン酸化物膜の製造方法
2−1.成膜工程
2−2.熱処理工程
3.膜形成基材
4.物品
本発明の一実施形態に係る複合タングステン酸化物膜について説明する。本発明の一実施形態に係る複合タングステン酸化物膜は、一般式MxWyOz(ただし、Mは、アルカリ金属、アルカリ土類金属、Fe、In、Tl、Snの内から選択される1種以上の元素、Wはタングステン、Oは酸素)で表される組成を主成分とする膜であり、0.001≦x/y≦1、2.2≦z/y≦3.0の範囲の構成である。
次に、複合タングステン酸化物膜の製造方法について説明する。図3は、本発明の一実施形態に係る複合タングステン酸化物膜の製造方法の概略を示す工程図である。本発明の一実施形態に係る複合タングステン酸化物膜の製造方法は、元素MとタングステンWと酸素Oを主成分とする複合タングステン酸化物膜の製造方法であって、物理的な成膜法を用いて膜を形成する成膜工程S1と、膜を熱処理する熱処理工程S2とを有する。以下、各工程について詳細に説明する。
成膜工程S1では、物理的な成膜法を用いて膜を形成する。本発明の一実施形態に係る複合タングステン酸化物膜の物理的な成膜方法としては、真空蒸着法、スパッタリング法、イオンプレーティング法、イオンビーム法などがある。この中でも、スパッタリング法は、成膜粒子のエネルギーが大きく付着力が強く、成膜が緻密で膜質が強く、かつ成膜プロセスが安定していて膜質、膜厚の制御が高い精度で可能である。さらに、スパッタリング法は、高融点金属・合金・化合物の成膜が可能で、反応性ガスの導入で酸化物や窒化物などの成膜が可能であり、組成の調整が比較的容易などの特長を持ち、液晶表示素子やハードディスク等の電子機器、ウィンドフィルムやミラー等の汎用品など幅広い分野で多く利用され、製造装置も多いことから好ましい。
次に、熱処理工程S2では、成膜工程S1で得られた膜を熱処理する。本発明に記載の膜特性を得るには、成膜工程S1における成膜雰囲気の酸素ガスの割合に応じて、膜の熱処理雰囲気の条件を変える必要がある。熱処理の雰囲気は、酸化性または不活性または還元雰囲気中で行う。
本発明の一実施形態に係る膜形成基材は、上述した複合タングステン酸化物膜が被成膜基材の少なくとも一方の面に形成されたものである。被成膜基材は、本発明の一実施形態に係る複合タングステン酸化物膜の形成が可能であれば特に限定されるものではない。
本発明の一実施形態に係る物品は、上述した複合タングステン酸化物膜及び/又は膜形成基材を1又は複数有する。本発明の複合タングステン酸化物膜及び/又は膜形成基材とを有する物品は、複合タングステン酸化物膜が光を吸収して遮蔽する機能、光を吸収して発熱する機能、光を吸収して電子を放出する機能のいずれか、またはそれら複数の機能を有する物品であればどのような物品でも構わない。
実施例1では、Cs/W原子比が0.33のセシウムタングステン酸化物粉末(住友金属鉱山株式会社製YM−01)をホットプレス装置に投入し、真空雰囲気、温度950℃、押し圧250kgf/cm2の条件で焼結し、セシウムタングステン酸化物焼結体を作製した。焼結体組成を化学分析した結果、Cs/Wは0.33であった。この酸化物焼結体を直径153mm、厚み5mmに機械加工で研削し、ステンレス製バッキングプレートに金属インジウム蝋材を用いて接合して、セシウムタングステン酸化物スパッタリングターゲットを作製した。
実施例1と同様に同じ装置を用い、表1及び表2に記載されているように元素M、膜厚、成膜雰囲気、熱処理雰囲気および時間を変えて複合タングステン酸化物膜の作成を行い、膜の特性を調べた。表1及び表2に実施例及び比較例の結果を示す。
(1)成膜工程において、不活性ガス中でスパッタリング成膜した後、熱処理工程において、膜を酸素が含まれるガス中で400℃〜600℃の温度で熱処理する。
(2)成膜工程において、酸素を含むガス中でスパッタリング成膜した後、熱処理工程において、膜を不活性雰囲気中または還元雰囲気中で400℃〜900℃の温度で熱処理する。
Claims (10)
- 一般式MxWyOz(ただし、Mはアルカリ金属、アルカリ土類金属、Fe、In、Tl、Snの内から選択される1種以上の元素、Wはタングステン、Oは酸素)で表される組成を主成分とする複合タングステン酸化物膜であって、
0.001≦x/y≦1、2.2≦z/y≦3.0であり、
有機物成分を実質的に含まず、シート抵抗が105Ω/□以上で、
波長550nmにおける透過率が50%以上、波長1400nmにおける透過率が30%以下、かつ、波長1400nmにおける吸収率が35%以上であることを特徴とする複合タングステン酸化物膜。 - 波長1400nmにおける吸収率に対する波長800nmにおける吸収率が80%以下であることを特徴とする請求項1に記載の複合タングステン酸化物膜。
- スパッタリング成膜由来であることを特徴とする請求項1又は請求項2に記載の複合タングステン酸化物膜。
- 前記Mは、Cs、Rb、K、Tl、In、Ba、Li、Na、Ca、Sr、Fe、およびSnの内から選択される1種以上の元素であることを特徴とする請求項1乃至請求項3のいずれか1項に記載の複合タングステン酸化物膜。
- 20nmより厚い膜厚を有することを特徴とする請求項1乃至請求項4のいずれか1項に記載の複合タングステン酸化物膜。
- 請求項1乃至請求項5のいずれか1項に記載の複合タングステン酸化物膜が被成膜基材の少なくとも一方の面に形成されている膜形成基材。
- 400℃以上の軟化点もしくは熱変形温度を有することを特徴とする請求項6に記載の膜形成基材。
- 前記被成膜基材がガラスであることを特徴とする請求項6又は請求項7に記載の膜形成基材。
- 請求項1乃至請求項5のいずれか1項に記載の複合タングステン酸化物膜及び/又は請求項6乃至請求項8のいずれか1項に記載の膜形成基材を1又は複数有することを特徴とする物品。
- 複合タングステン酸化物膜の製造方法であって、
物理的な成膜法により膜を形成する成膜工程と、
前記膜を熱処理する熱処理工程とを有し、
前記成膜工程と前記熱処理工程の条件が下記(1)、(2)のいずれかであることを特徴とする複合タングステン酸化物膜の製造方法。
(1)前記成膜工程において、不活性ガス中でスパッタリング成膜した後、前記熱処理工程において、前記膜を酸素が含まれるガス中で400℃〜600℃の温度で熱処理する。
(2)前記成膜工程において、酸素を含むガス中でスパッタリング成膜した後、前記熱処理工程において、前記膜を不活性雰囲気中または還元雰囲気中で400℃〜900℃の温度で熱処理する。
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WO2019216134A1 (ja) | 2019-11-14 |
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TW201947048A (zh) | 2019-12-16 |
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