JP6682188B2 - 硬質反射防止膜並びにその製造及びその使用 - Google Patents
硬質反射防止膜並びにその製造及びその使用 Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
- 239000004576 sand Substances 0.000 claims description 8
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 7
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
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- 239000011651 chromium Substances 0.000 claims description 6
- 150000004767 nitrides Chemical class 0.000 claims description 6
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- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 239000010936 titanium Substances 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- 229910052726 zirconium Inorganic materials 0.000 claims description 6
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052796 boron Inorganic materials 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 238000005259 measurement Methods 0.000 claims description 5
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- 239000006018 Li-aluminosilicate Substances 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 4
- 239000005354 aluminosilicate glass Substances 0.000 claims description 4
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- 229910052759 nickel Inorganic materials 0.000 claims description 4
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- 238000001341 grazing-angle X-ray diffraction Methods 0.000 description 3
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- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 2
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- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
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Classifications
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
- G02B1/113—Anti-reflection coatings using inorganic layer materials only
- G02B1/115—Multilayers
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- 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
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
-
- 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
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
- C03C17/3429—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating
- C03C17/3435—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating comprising a nitride, oxynitride, boronitride or carbonitride
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
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- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
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- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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- 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
- 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
-
- 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
- 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
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- 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
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/73—Anti-reflective coatings with specific characteristics
- C03C2217/734—Anti-reflective coatings with specific characteristics comprising an alternation of high and low refractive indexes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24942—Structurally defined web or sheet [e.g., overall dimension, etc.] including components having same physical characteristic in differing degree
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24942—Structurally defined web or sheet [e.g., overall dimension, etc.] including components having same physical characteristic in differing degree
- Y10T428/2495—Thickness [relative or absolute]
- Y10T428/24967—Absolute thicknesses specified
- Y10T428/24975—No layer or component greater than 5 mils thick
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- Metallurgy (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Laminated Bodies (AREA)
- Surface Treatment Of Optical Elements (AREA)
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Description
本発明によりコーティングされた基材は、反射を防止する膜(以下では反射防止膜とも呼ぶ)を有する。ここで、反射防止膜は、複数の誘電体層を有する光干渉膜として作製されている。膜の層系は、交互に低屈折率層と高屈折率層とを有し、かつ少なくとも2つの低屈折率層と少なくとも1つの高屈折率層で形成されている。高屈折率層は、2つの低屈折率層の間に配置されている。一番上の誘電体層は、低屈折率層である。一番上の層は、基材に対して最も距離を隔てている層を意味する。それに応じて、膜の一番下の層は、基材の上に直接配置されている。
− それぞれの層の斜入射XRD(GIXRD)スペクトルの収集、すなわち薄膜X線回折
− 34°から37°の間の範囲での相応する(001)反射I(001)の最大強度の測定
− 32°から34°の間の範囲での(100)反射I(100)の最大強度の測定
− 37°から39°の間の範囲での(101)反射I(101)の最大強度の測定
x(001)=I(001)/(I(001)+I(100))
及びy(001)=I(001)/(I(001)+I(101))
この方法は、少なくとも以下の工程:
a)基材を準備する工程、
b)基材を、低屈折率のSiO2含有層でコーティングする工程、
c)工程b)でコーティングされる基材を、アルミニウム含有ターゲットを備えたスパッタリング装置中で準備する工程、
d)スパッタ粒子を、ターゲット面積1cm2当たり8〜1000W、有利には10〜100Wの範囲の出力密度で放出する工程、及び
e)更なる低屈折率のSiO2含有層を、工程d)で得られるコーティングされた基材上に堆積させる工程
を有する。
y(001)=I(001)/(I(001)+I(101))
Claims (17)
- 反射防止膜を有するコーティングされた基材であって、ここで、前記基材は、ガラス又はガラスセラミックであり、前記反射防止膜が、少なくとも2つの低屈折率層及び少なくとも1つの高屈折率層を有し、前記高屈折率層は、前記少なくとも2つの低屈折率層の間に配置されている光干渉膜として形成されており、前記高屈折率層は、透明な硬質物質層であり、前記硬質物質層は、主たる(001)優先配向を示す六方晶結晶構造を有する結晶性窒化アルミニウムを有し、かつ前記低屈折率層はSiO2 及び/若しくはドープされたSiO 2 を有する、前記コーティングされた基材。
- 前記低屈折率層のSiO 2 が、アルミニウム、ホウ素、ジルコニウム、チタン、ニッケル、クロム及び炭素から成る群から選択される元素の1種以上の酸化物及び/若しくは窒化物及び/若しくは炭化物及び/若しくは炭窒化物でドープされており、かつ/又はN2を有する、請求項1記載のコーティングされた基材。
- 前記低屈折率層が、550nmの波長で1.3〜1.6の範囲の屈折率値を有し、かつ前記高屈折率層が、550nmの波長で1.8〜2.3の範囲の屈折率値を有する、請求項1又は2記載のコーティングされた基材。
- XRD測定により求めた、(001)優先配向を示す前記結晶構造x (001) 及びy (001) の割合が0.5より大きく、ここで、
x(001)=I(001)/(I(001)+I(100))
及び
y(001)=I(001)/(I(001)+I(101))
である、請求項1から3までのいずれか1項記載のコーティングされた基材。 - 前記高屈折率層が、10mNの試験加重で80〜250GPaの範囲の弾性係数を有し、かつ/又は前記弾性係数に対する硬度の比が、少なくとも0.08である、請求項1から4までのいずれか1項記載のコーティングされた基材。
- 前記硬質物質層の全層厚が、最大でも600nmである、請求項1から5までのいずれか1項記載のコーティングされた基材。
- 前記硬質物質層における酸素の割合が、最大でも10原子%である、請求項1から6までのいずれか1項記載のコーティングされた基材。
- 90gの砂を積んで13500回振動させるバイエル試験にかけた後に、前記コーティングされた基材の残留反射率が、750nmの波長で5%未満であり、かつ/又は
90gの砂を積んで13500回振動させるバイエル試験にかけた後に、前記コーティングの曇り度が、この負荷試験前より最大5%高い、請求項1から7までのいずれか1項記載のコーティングされた基材。 - 前記膜が3つの誘電体層を、第一及び第二の低屈折率層並びに1つの高屈折率の硬質物質層の形で有し、ここで、前記第一の低屈折率層は、前記基材と前記高屈折率の硬質物質層との間に配置されており、かつ前記第二の低屈折率層は、前記高屈折率の硬質物質層の上に配置されており、ここで、前記第一の低屈折率層の層厚は、5〜50nmの範囲にあり、前記第二の低屈折率層の層厚は、40〜120nmの範囲にあり、かつ/又は前記高屈折率の硬質物質層の層厚は、80〜1200nmの範囲にある、請求項1から8までのいずれか1項記載のコーティングされた基材。
- 前記膜が少なくとも5つの誘電体層を有し、前記膜は、第一、第二及び第三の低屈折率層並びに第一及び第二の高屈折率の硬質物質層を有し、ここで、前記第一の低屈折率層は、前記基材と前記第一の高屈折率の硬質物質層との間に配置されており、前記第二の低屈折率層は、前記第一と前記第二の高屈折率の硬質物質層との間に配置されており、かつ前記第三の低屈折率の硬質物質層は、前記第二の高屈折率の硬質物質層の上に配置されており、ここで、前記第一の低屈折率層の層厚は、10〜60nmの範囲にあり、前記第二の低屈折率層の層厚は、10〜40nmの範囲にあり、前記第三の低屈折率層の層厚は、60〜120nmの範囲にあり、前記第一の高屈折率の硬質物質層の層厚は、10〜40nmの範囲にあり、かつ/又は前記第二の高屈折率の硬質物質層の層厚は、100〜1000nmの範囲にある、請求項1から8までのいずれか1項記載のコーティングされた基材。
- 前記基材が、サファイアガラス、ホウケイ酸塩ガラス、アルミノケイ酸塩ガラス、石灰ソーダガラス、合成石英ガラス、リチウムアルミノケイ酸塩ガラス、または光学ガラスである、請求項1から10までのいずれか1項記載のコーティングされた基材。
- 前記低屈折率層が、ドーパントとしてのアルミニウムによりドープされたSiO 2 を含む、請求項1から11までのいずれか1項記載のコーティングされた基材。
- 反射防止膜を有するコーティングされた基材の製造法であって、前記基材は、ガラス又はガラスセラミックであり、前記反射防止膜が、少なくとも2つの低屈折率層及び少なくとも1つの高屈折率層を有し、前記高屈折率層は、前記少なくとも2つの低屈折率層の間に配置されている光干渉膜として形成されており、少なくとも以下の工程:
a)基材を準備する工程、
b)前記基材を、低屈折率のSiO2含有層でコーティングする工程、
c)工程b)でコーティングされる前記基材を、アルミニウム含有ターゲットを備えたスパッタリング装置中で準備する工程、
d)スパッタ粒子を、ターゲット面積1cm2当たり8〜1000Wの範囲の出力密度で、最大でも2*10-5mbarの最終圧力にて放出する工程、及び
e)更なる低屈折率のSiO2含有層を、工程d)で得られるコーティングされた基材上に堆積させる工程
を有する、前記製造法。 - 工程a)において、高屈折率の硬質物質層を有する基材を準備し、かつ/又は工程c)〜e)のシーケンスを数回実施する、請求項13記載の方法。
- 前記基材が、サファイアガラス、ホウケイ酸塩ガラス、アルミノケイ酸塩ガラス、石灰ソーダガラス、合成石英ガラス、リチウムアルミノケイ酸塩ガラス、または光学ガラスである、請求項13または14記載の方法。
- 前記低屈折率層が、ドーパントとしてのアルミニウムによりドープされたSiO 2 を含む、請求項13から15までのいずれか1項に記載の方法。
- 時計用ガラス、光学部品、クックトップ、乗り物領域におけるディスプレイ又は覗き窓、暖炉窓、オーブン窓、家庭用器具におけるガラス部品若しくはガラスセラミック部品、又はディスプレイとしての、請求項1から12までのいずれか1項記載のコーティングされた基材の使用。
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