JP2017529306A - 基板上に耐擦傷性結晶化層を形成するための方法及びこれで形成された物品 - Google Patents
基板上に耐擦傷性結晶化層を形成するための方法及びこれで形成された物品 Download PDFInfo
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- JP2017529306A JP2017529306A JP2017515076A JP2017515076A JP2017529306A JP 2017529306 A JP2017529306 A JP 2017529306A JP 2017515076 A JP2017515076 A JP 2017515076A JP 2017515076 A JP2017515076 A JP 2017515076A JP 2017529306 A JP2017529306 A JP 2017529306A
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- 238000000034 method Methods 0.000 title claims abstract description 69
- 238000002425 crystallisation Methods 0.000 title claims abstract description 18
- 230000008025 crystallization Effects 0.000 title claims abstract description 18
- 230000003678 scratch resistant effect Effects 0.000 title claims abstract description 18
- 239000002243 precursor Substances 0.000 claims abstract description 70
- 238000010438 heat treatment Methods 0.000 claims abstract description 32
- 238000002844 melting Methods 0.000 claims abstract description 27
- 230000008018 melting Effects 0.000 claims abstract description 27
- 238000001816 cooling Methods 0.000 claims abstract description 17
- 150000004767 nitrides Chemical class 0.000 claims abstract description 11
- 239000010431 corundum Substances 0.000 claims description 27
- 229910052593 corundum Inorganic materials 0.000 claims description 27
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 27
- 238000000151 deposition Methods 0.000 claims description 13
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 7
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 7
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims description 7
- 229910001936 tantalum oxide Inorganic materials 0.000 claims description 7
- GSWGDDYIUCWADU-UHFFFAOYSA-N aluminum magnesium oxygen(2-) Chemical compound [O--].[Mg++].[Al+3] GSWGDDYIUCWADU-UHFFFAOYSA-N 0.000 claims description 5
- 150000001247 metal acetylides Chemical class 0.000 claims description 4
- 239000010410 layer Substances 0.000 description 181
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 30
- 239000011521 glass Substances 0.000 description 14
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 12
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000010924 continuous production Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000003618 dip coating Methods 0.000 description 4
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- 238000007764 slot die coating Methods 0.000 description 4
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
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- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- ZTJWUVMPZRLXAB-UHFFFAOYSA-N [Ta].[Ti].[W] Chemical compound [Ta].[Ti].[W] ZTJWUVMPZRLXAB-UHFFFAOYSA-N 0.000 description 2
- IYABWNGZIDDRAK-UHFFFAOYSA-N allene Chemical compound C=C=C IYABWNGZIDDRAK-UHFFFAOYSA-N 0.000 description 2
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- QSWDMMVNRMROPK-UHFFFAOYSA-K chromium(3+) trichloride Chemical compound [Cl-].[Cl-].[Cl-].[Cr+3] QSWDMMVNRMROPK-UHFFFAOYSA-K 0.000 description 2
- 238000005137 deposition process Methods 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 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 2
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- 230000001590 oxidative effect Effects 0.000 description 2
- 239000003880 polar aprotic solvent Substances 0.000 description 2
- MWWATHDPGQKSAR-UHFFFAOYSA-N propyne Chemical group CC#C MWWATHDPGQKSAR-UHFFFAOYSA-N 0.000 description 2
- 229910001750 ruby Inorganic materials 0.000 description 2
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
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- 229910052596 spinel Inorganic materials 0.000 description 2
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
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- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
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- 239000005328 architectural glass Substances 0.000 description 1
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- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- LJMRAZJIDWENJS-UHFFFAOYSA-N cesium magnesium oxygen(2-) Chemical compound [Cs+].[O-2].[Mg+2] LJMRAZJIDWENJS-UHFFFAOYSA-N 0.000 description 1
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- 150000003841 chloride salts Chemical class 0.000 description 1
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- 238000006073 displacement reaction Methods 0.000 description 1
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- 239000012530 fluid Substances 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- UPWPDUACHOATKO-UHFFFAOYSA-K gallium trichloride Chemical compound Cl[Ga](Cl)Cl UPWPDUACHOATKO-UHFFFAOYSA-K 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
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- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
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- 239000004065 semiconductor Substances 0.000 description 1
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
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- 229910003468 tantalcarbide Inorganic materials 0.000 description 1
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
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- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1295—Process of deposition of the inorganic material with after-treatment of the deposited inorganic material
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
- C03C17/25—Oxides by deposition from the liquid phase
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
- C23C18/1216—Metal oxides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1229—Composition of the substrate
- C23C18/1241—Metallic substrates
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1229—Composition of the substrate
- C23C18/1245—Inorganic substrates other than metallic
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
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Abstract
Description
塩化アルミニウムのDMF内1M溶液を含むゾルゲルをHPFD(登録商標)ガラス基板上に被着し、層をアニールするため、MAPP/空気炎で約2000℃に加熱した。このプロセスを5層の溶液が被着されてアニールされるまで反復した。この結果、ガラス基板上に厚さが150nmと200nmの間の非晶質酸化アルミニウム層が得られた。次いで、酸化アルミニウム層を融解するため、酸化アルミニウム層を、手動タイプのチェックボックス内の大気雰囲気条件の下でほぼ30秒、水素/酸素炎で約3200℃に局所加熱した。次いで、融解酸化アルミニウム層を冷却し、結晶化して、厚さが約150nmと200nmの間のα−酸化アルミニウム(コランダム)にした。コランダムの存在は、GIXRD(斜入射X線回折)を用いて確認した。図3は、コランダムが存在することを示す、2θ(°)対強度(カウント)のプロットとしてのGIXRD分析のプロットである。
1M硝酸溶液と1:1の比で混合した塩化アルミニウムのDMF内1M溶液を含むゾルゲルをEAGLE XG(登録商標)ガラス基板上にスピンコーティングし、層をアニールするため、MAPP/空気炎で約2000℃に加熱した。このプロセスを15層の溶液が被着されてアニールされるまで反復した。この結果、ガラス基板上に厚さが1000nmと1200nmの間の非晶質酸化アルミニウム層が得られた。次いで、酸化アルミニウム層を融解するため、酸化アルミニウム層を、手動タイプのチェックボックス内の大気雰囲気条件の下でほぼ30秒、水素/酸素炎で約3200℃に局所加熱した。次いで、融解酸化アルミニウム層を冷却し、結晶化して、厚さが1000nmと1200nmの間のα−酸化アルミニウム(コランダム)にした。コランダムの存在は、GIXRD(斜入射X線回折)を用いて確認した。図4は、コランダムが、またムライトも、存在することを示す、2θ(°)対強度(カウント)のプロットとしてのGIXRD分析のプロットである。しかし、水素/酸素炎の高熱によりガラス基板がある程度融解し、得られた結晶化層は、実施例1で形成された結晶化層よりも、結晶粒径が大きくなり、曇っていた。非晶質酸化アルミニウム層が厚くなるほど、非晶質酸化アルミニウム層を融解するに必要な熱が多くなり、したがってガラス基板が融解する可能性が一層高くであろうと考えられる。また大きくなった厚さ及び増大した熱によりコランダムの内のいくらかの、結晶化層に曇りを生じさせる、ムライトへの転換が可能になることも考えられる。
実施例1のプロセスにしたがって、14層コランダム膜及び6層コランダム膜を形成した。16層コランダム膜では、図5に示されるように、マクロスケール(200μm及び100μm)及びマイクロスケール(50μm及び20μm)のいずれにおいてもかなりのマッドクラックの発生を示した。しかし、6層コランダム膜では、図6に示されるように、マッドクラックの発生はほとんど全く示されなかった。すなわち、コランダム層の厚さはコランダム層にわたる表面硬度の変動度に影響し、層が厚くなるほど変動度が大きくなる。
結晶化層を形成するための方法において、
基板の表面上に形成された、酸化物、窒化物、炭化物及び酸窒化物からなる群から選ばれる前駆体層を融解する工程であって、前記前駆体層を局所加熱する工程を含む工程、及び
前記融解前駆体層が結晶化して結晶化層を形成するように前記融解前駆体層を冷却する工程、
を含む方法。
前記局所加熱する工程が約0.25cm/秒〜約2cm/秒の範囲にある速度で実施される、実施形態1に記載の方法。
前記局所加熱する工程が前記前駆体層をレーザで加熱する工程を含む、実施形態1または2に記載の方法。
前記局所加熱する工程が前記前駆体層をトーチで加熱する工程を含む、実施形態1または2に記載の方法。
前記トーチが水素−酸素トーチである、実施形態4に記載の方法。
前記前駆体層が、酸化アルミニウム、酸化マグネシウムアルミニウム、酸化タンタル及び酸化クロムからなる群から選ばれる酸化物である、実施形態1から5のいずれかに記載の方法。
前記前駆体層が非晶質酸化アルミニウムである、実施形態1から6のいずれかに記載の方法。
前記非晶質酸化アルミニウムが結晶化してコランダムになる、実施形態7に記載の方法。
前記非晶質酸化アルミニウムが結晶化してルビーになる、実施形態7に記載の方法。
前記基板が、ガラス、セラミック、ガラス−セラミック及び金属からなる群から選ばれる、実施形態1から9のいずれかに記載の方法。
前記基板上に前記前駆体層を被着する工程をさらに含む、実施形態1から10のいずれかに記載の方法。
前記被着する工程が、スロットダイコーティング、ディップコーティング、スピンコーティング、スプレーコーティング、テープキャスティング、原子層堆積、プラズマ強化化学的気相成長、化学的気相成長、分子ビームエピタキシー、蒸着及びスパッタリングからなる群から選ばれる、実施形態11に記載の方法。
前記結晶化層の硬度が15GPa以上である、実施形態1から12のいずれかに記載の方法。
前記結晶化層の光透過率が400nm〜800nmの波長において85%以上である、実施形態1から13のいずれかに記載の方法。
前記基板をロールで提供する工程及び前記融解する工程と前記冷却する工程を連続プロセスとして実施する工程をさらに含む、実施形態1から14のいずれかに記載の方法。
結晶化層を形成するための方法において、
基板上に酸化物層を被着する工程、
前記酸化物層を融解するために前記酸化物層を局所加熱する工程、及び
前記融解酸化物層が結晶化して結晶化層を形成するように前記融解酸化物層を冷却する工程、
を含む方法。
前記酸化物層が、酸化アルミニウム、酸化マグネシウムアルミニウム、酸化タンタル及び酸化クロムからなる群から選ばれる、実施形態16に記載の方法。
前記被着する工程が前記基板にゾルゲルを塗布する工程を含む、実施形態16または17に記載の方法。
前記被着されたゾルゲルをアニールする工程をさらに含む、実施形態18に記載の方法。
複数の酸化物層を形成するために前記被着する工程及び前記アニールする工程を反復する工程をさらに含む、実施形態19に記載の方法。
前記酸化物層が非晶質酸化アルミニウムである、実施形態16から20のいずれかに記載の方法。
前記非晶質酸化アルミニウムが結晶化してコランダムになる、実施形態21に記載の方法。
前記局所加熱する工程が約0.25cm/秒〜約2cm/秒の範囲にある速度で実施される、実施形態16から22のいずれかに記載の方法。
前記局所加熱する工程が前記層をレーザで加熱する工程を含む、実施形態16から23のいずれかに記載の方法。
前記局所加熱する工程が前記層をトーチで加熱する工程を含む、実施形態16から23のいずれかに記載の方法。
前記トーチが水素−酸素トーチである、実施形態25に記載の方法。
前記基板が、ガラス、セラミック、ガラス−セラミック及び金属からなる群から選ばれる、実施形態16から26のいずれかに記載の方法。
前記被着する工程が、スロットダイコーティング、ディップコーティング、スピンコーティング、スプレーコーティング、テープキャスティング、原子層堆積、プラズマ強化化学的気相成長、化学的気相成長、分子ビームエピタキシー、蒸着及びスパッタリングからなる群から選ばれる、実施形態16から27のいずれかに記載の方法。
前記結晶化層の硬度が15GPa以上である、実施形態16から28のいずれかに記載の方法。
前記結晶化層の光透過率が400nm〜800nmの波長において85%以上である、実施形態16から29のいずれかに記載の方法。
前記基板をロールで提供する工程及び前記融解する工程と前記冷却する工程を連続プロセスとして実施する工程をさらに含む、実施形態16から30のいずれかに記載の方法。
前記結晶化層が約1000nm以下の厚さを有する、実施形態16から31のいずれかに記載の方法。
物品において、
基板、及び
前記基板の表面上に形成された、コランダムを含み、15GPa以上の硬度を有する、結晶化層、
を有する物品。
前記耐擦傷性結晶化層が約2000nm以下の厚さを有する、実施形態33に記載の物品。
前記耐擦傷性結晶化層が約1000nm以下の厚さを有する、実施形態33に記載の物品。
前記耐擦傷性結晶化層が約600nm以下の厚さを有する、実施形態33に記載の物品。
前記耐擦傷性結晶化層の光透過率が400nm〜800nmの波長において85%以上である、実施形態33から36のいずれかに記載の物品。
14 基板
16 耐擦傷性結晶化層
Claims (10)
- 結晶化層を形成するための方法において、
基板の表面上に形成された、酸化物、窒化物、炭化物及び酸窒化物からなる群から選ばれる前駆体層を融解する工程であって、前記前駆体層を局所加熱する工程を含む工程、及び
前記融解前駆体層が結晶化して結晶化層を形成するように前記融解前駆体層を冷却する工程、
を含むことを特徴とする方法。 - 前記局所加熱する工程が約0.25cm/秒〜約2cm/秒の範囲にある速度で実施されることを特徴とする請求項1に記載の方法。
- 前記前駆体層が、酸化アルミニウム、酸化マグネシウムアルミニウム、酸化タンタル及び酸化クロムからなる群から選ばれる酸化物であることを特徴とする請求項1または2に記載の方法。
- 前記結晶化層の硬度が15GPa以上であることを特徴値する請求項1から3のいずれかに記載の方法。
- 結晶化層を形成するための方法において、
基板上に酸化物層を被着する工程、
前記酸化物層を融解するために前記酸化物層を局所加熱する工程、及び
前記融解酸化物層が結晶化して結晶化層を形成するように前記融解酸化物層を冷却する工程、
を含むことを特徴とする方法。 - 前記酸化物層が、酸化アルミニウム、酸化マグネシウムアルミニウム、酸化タンタル及び酸化クロムからなる群から選ばれることを特徴とする請求項5に記載の方法。
- 前記被着する工程が前記基板にゾルゲルを塗布する工程を含むことを特徴とする請求項5または6に記載の方法。
- 前記結晶化層の硬度が15GPa以上であることを特徴とする請求項5から7のいずれかに記載の方法。
- 物品において、
基板、及び
前記基板の表面上に形成された、コランダムを含み、15GPa以上の硬度を有する、結晶化層、
を有することを特徴とする物品。 - 前記耐擦傷性結晶化層が約2000nm以下の厚さを有することを特徴とする請求項9に記載の物品。
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- 2015-09-14 US US14/853,191 patent/US9976230B2/en active Active
- 2015-09-17 JP JP2017515076A patent/JP6817196B2/ja active Active
- 2015-09-17 CN CN201580050621.3A patent/CN107075682A/zh active Pending
- 2015-09-17 KR KR1020177010120A patent/KR20170056637A/ko not_active Application Discontinuation
- 2015-09-17 WO PCT/US2015/050587 patent/WO2016044528A1/en active Application Filing
- 2015-09-17 EP EP15771417.1A patent/EP3194347A1/en not_active Withdrawn
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KR20170056637A (ko) | 2017-05-23 |
JP6817196B2 (ja) | 2021-01-20 |
US20160083863A1 (en) | 2016-03-24 |
EP3194347A1 (en) | 2017-07-26 |
TW201620853A (zh) | 2016-06-16 |
TWI710534B (zh) | 2020-11-21 |
CN107075682A (zh) | 2017-08-18 |
WO2016044528A1 (en) | 2016-03-24 |
US9976230B2 (en) | 2018-05-22 |
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