CN114196924A - Coating method of vacuum ultraviolet aluminum reflector on surface of copper substrate - Google Patents
Coating method of vacuum ultraviolet aluminum reflector on surface of copper substrate Download PDFInfo
- Publication number
- CN114196924A CN114196924A CN202111533081.8A CN202111533081A CN114196924A CN 114196924 A CN114196924 A CN 114196924A CN 202111533081 A CN202111533081 A CN 202111533081A CN 114196924 A CN114196924 A CN 114196924A
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- Prior art keywords
- aluminum
- film
- copper substrate
- layer
- substrate
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 121
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 119
- 239000000758 substrate Substances 0.000 title claims abstract description 102
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 80
- 239000010949 copper Substances 0.000 title claims abstract description 80
- 238000000576 coating method Methods 0.000 title claims abstract description 26
- 238000002310 reflectometry Methods 0.000 claims abstract description 32
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 26
- 238000007747 plating Methods 0.000 claims abstract description 21
- 230000001681 protective effect Effects 0.000 claims abstract description 21
- 239000011248 coating agent Substances 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 8
- 239000010937 tungsten Substances 0.000 claims abstract description 8
- 239000010410 layer Substances 0.000 claims description 54
- 229910001635 magnesium fluoride Inorganic materials 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- 125000006850 spacer group Chemical group 0.000 claims description 14
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 229910002319 LaF3 Inorganic materials 0.000 claims description 8
- 229910001512 metal fluoride Inorganic materials 0.000 claims description 8
- 229910044991 metal oxide Inorganic materials 0.000 claims description 8
- 150000004706 metal oxides Chemical class 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 238000002207 thermal evaporation Methods 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 229910052681 coesite Inorganic materials 0.000 claims description 6
- 229910052906 cristobalite Inorganic materials 0.000 claims description 6
- 238000000151 deposition Methods 0.000 claims description 6
- 238000010926 purge Methods 0.000 claims description 6
- 229910052682 stishovite Inorganic materials 0.000 claims description 6
- 229910052905 tridymite Inorganic materials 0.000 claims description 6
- 229910000838 Al alloy Inorganic materials 0.000 claims description 5
- JRBRVDCKNXZZGH-UHFFFAOYSA-N alumane;copper Chemical compound [AlH3].[Cu] JRBRVDCKNXZZGH-UHFFFAOYSA-N 0.000 claims description 5
- 239000011241 protective layer Substances 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 229910052593 corundum Inorganic materials 0.000 claims description 4
- 238000001659 ion-beam spectroscopy Methods 0.000 claims description 4
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Inorganic materials [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 4
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 4
- 238000000231 atomic layer deposition Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(IV) oxide Inorganic materials O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 claims description 3
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims description 3
- 238000005275 alloying Methods 0.000 claims description 2
- BYMUNNMMXKDFEZ-UHFFFAOYSA-K trifluorolanthanum Chemical compound F[La](F)F BYMUNNMMXKDFEZ-UHFFFAOYSA-K 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 abstract description 13
- 230000008020 evaporation Effects 0.000 abstract description 12
- 150000002222 fluorine compounds Chemical class 0.000 abstract 1
- 239000010408 film Substances 0.000 description 105
- 230000000052 comparative effect Effects 0.000 description 16
- 239000000463 material Substances 0.000 description 13
- 238000002360 preparation method Methods 0.000 description 10
- 239000007888 film coating Substances 0.000 description 9
- 238000009501 film coating Methods 0.000 description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 8
- 238000001228 spectrum Methods 0.000 description 8
- 239000010409 thin film Substances 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- 238000000985 reflectance spectrum Methods 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- 239000005350 fused silica glass Substances 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 239000010432 diamond Substances 0.000 description 3
- 229910003460 diamond Inorganic materials 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- 230000003746 surface roughness Effects 0.000 description 3
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 2
- 239000005751 Copper oxide Substances 0.000 description 2
- -1 SiO2 Chemical class 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910000431 copper oxide Inorganic materials 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000004611 spectroscopical analysis Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000010408 sweeping Methods 0.000 description 2
- 239000005294 BK7 Substances 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000012788 optical film Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 230000005469 synchrotron radiation Effects 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
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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
- C23C14/24—Vacuum evaporation
- C23C14/26—Vacuum evaporation by resistance or inductive heating of the source
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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
- C23C14/0694—Halides
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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
- C23C14/08—Oxides
- C23C14/081—Oxides of aluminium, magnesium or beryllium
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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
- C23C14/08—Oxides
- C23C14/083—Oxides of refractory metals or yttrium
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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
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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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- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
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- C23C14/24—Vacuum evaporation
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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
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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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
- C23C14/46—Sputtering by ion beam produced by an external ion source
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- 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
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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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- 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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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
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Abstract
The invention relates to a method for coating a vacuum ultraviolet aluminum reflecting mirror on the surface of a copper substrate. The dielectric spacing layer can be plated in a vacuum chamber before the aluminum film is plated, or can be plated in other vacuum chambers, and then is transferred to a plating vacuum chamber for plating the aluminum film and the fluoride protective film in the atmospheric environment, and the copper substrate containing the dielectric spacing layer is used as the substrate for plating the aluminum film and the fluoride protective film; the aluminum film is prepared by conducting tungsten wires and then heating the aluminum wires for evaporation, and the fluoride protective film layer is prepared by evaporating fluorides by using an evaporation boat or an electron gun. The method for plating the vacuum ultraviolet aluminum reflector on the surface of the copper substrate realizes high reflectivity of the aluminum reflector on the copper substrate by utilizing the action of the medium spacing layer.
Description
Technical Field
The invention relates to the technical field of optical film preparation, in particular to a method for realizing high reflectivity in a vacuum ultraviolet wavelength range on the surface of a copper substrate.
Background
The vacuum ultraviolet reflector is widely applied to optical systems in the fields of space detection, synchrotron radiation light sources, gas monitoring and the like. There are two methods of making vacuum ultraviolet mirrors: a dielectric multilayer film mirror and a metal mirror. The multilayer dielectric film comprises a high-refractive-index dielectric film layer with low ultraviolet light absorption and a low-refractive-index dielectric film layer, and the usable high-refractive-index material for the vacuum ultraviolet reflecting film in the vacuum ultraviolet wavelength range comprises LaF3The low refractive index material comprises MgF2，AlF3And the like. As the metal thin film reflective film, only an aluminum film can be used as the metal thin film in the vacuum ultraviolet wavelength range. The aluminum can be quickly oxidized to generate Al when exposed to the air2O3Has obvious absorption to vacuum ultraviolet light with the wavelength less than 190nm, so LaF needs to be deposited on the surface of the aluminum film3，MgF2，AlF3And the combination of the films, so as to isolate the influence of air on the films, and obtain the metal vacuum ultraviolet reflecting mirror which can be used under different conditions.
Compared with the dielectric multilayer film reflecting mirror, the metal aluminum film reflecting mirror has high reflectivity in the whole vacuum ultraviolet wavelength range, so that the coating of an optical system in a large incident angle range can be met; the reflectivity is less influenced by the thickness nonuniformity of the film, and the requirement of coating the vacuum ultraviolet reflecting mirror on the surface of a special optical element can be met.
Generally, a coated substrate of a vacuum ultraviolet mirror based on an aluminum film includes fused silica, BK7, microcrystals, and the like. In recent years, vacuum ultraviolet reflectors using copper as a substrate have also been used to some extent, and particularly in time projection cavity detectors using rare gas liquid as a working medium, copper is a key material for manufacturing electrodes in the time projection cavity detectors due to low radiation characteristics. Since copper and aluminum readily form copper-aluminum alloys, the structure, composition, and properties of the aluminum film are altered, which can significantly reduce the reflectivity of the aluminum mirror. Therefore, new coating techniques are needed to achieve high reflectivity of aluminum mirrors on copper substrates.
Disclosure of Invention
The invention provides a preparation method of an aluminum reflector based on a copper substrate.
The invention adopts the following technical scheme:
a coating method of a vacuum ultraviolet aluminum reflector on the surface of a copper substrate is provided, the ultraviolet reflector prepared by the method comprises the copper substrate, and a medium spacing layer, an aluminum film and a fluoride protective film layer are sequentially plated on the copper substrate from the copper substrate, and the method comprises the following steps:
(1) cleaning the copper substrate by using a nitrogen purging organic solution mode;
(2) depositing a metal oxide or metal fluoride medium spacing layer on the surface of the copper substrate;
(3) preparing an aluminum film on the medium spacing layer in a tungsten filament conductive and heating aluminum filament evaporation mode in a vacuum chamber;
(4) and preparing a fluoride protective film on the surface of the aluminum film.
Further, in the step (2), the dielectric spacing layer is used for isolating the aluminum film and the copper substrate from alloy reaction to form copper-aluminum alloy.
Further, in the step (2), the medium spacing layer can be exposed to the atmospheric environment after being coated in other coating machines, and is transferred and placed into an aluminum reflector coating vacuum chamber in the atmospheric environment to realize the preparation of the copper substrate surface reflector; or the plating of the dielectric spacing layer film layer is firstly completed in the same plating vacuum chamber, and then the plating of the aluminum film and the fluoride protective film layer is completed.
Further, in step (2), the dielectric spacer layer comprises a metal oxide such as SiO2，HfO2，Ta2O5，Al2O3Or metal fluorides such as MgF2，LaF3。
Further, in the step (2), the dielectric spacer layer may be implemented by ion beam sputtering, magnetron sputtering, thermal evaporation, and atomic layer deposition coating technology.
Further, in the step (3), the plating of the aluminum film is realized at the substrate temperature of 80-100 ℃.
Further, in the step (4), the fluoride protective film is formed by MgF2，LiF，AlF3，LaF3And the like to achieve high reflectivity in the vacuum ultraviolet wavelength range.
Further, in step (4), the thickness of the fluoride protective layer is optimized to provide the operating wavelength of the mirror with high reflectivity.
Further, in the step (4), a fluoride protective layer of about 5nm is first coated at the same substrate temperature as that in the case of aluminum film plating, and then the substrate temperature is raised to 200 ℃ or higher to coat the remaining fluoride film layer.
Compared with the currently adopted preparation method of the vacuum ultraviolet aluminum reflector, the preparation method has the technical advantages that:
(1) the copper is adopted as the ultraviolet reflector coating substrate, so that the ultraviolet high reflectivity is realized, and the specific requirements of some special application occasions on the vacuum ultraviolet reflecting element substrate are met.
(2) The metal oxide and the metal fluoride dielectric film are used as the intermediate layer, so that the copper substrate and the aluminum film layer are effectively isolated, and the spectral performance of the ultraviolet aluminum reflector on the surface of the copper substrate is improved.
Drawings
FIG. 1: the spectra of the copper substrate prepared in the comparative example and the vacuum ultraviolet aluminum mirror plated on the surface of the fused quartz substrate were compared.
FIG. 2: and (3) a transmission electron microscope image of the vacuum ultraviolet aluminum reflector on the surface of the copper substrate prepared by the comparative example.
FIG. 3: the relation of the change of the material components in the vacuum ultraviolet aluminum reflecting mirror on the surface of the copper substrate prepared by the comparative example along with the thickness is shown.
FIG. 4: the structural model of the vacuum ultraviolet aluminum reflector on the surface of the copper substrate prepared by the invention is utilized.
FIG. 5: a cross-sectional transmission electron microscope image of the aluminum reflective film on the surface of the copper substrate prepared in example 1.
FIG. 6: reflection spectra of aluminum mirrors on the surface of copper substrates prepared in examples 1 and 2.
Detailed Description
The aluminum reflector is usually fabricated on the surface of the substrate by heating an aluminum wire with a tungsten wire in a vacuum environment. Aluminum has high reflectivity to vacuum ultraviolet light with wavelength of more than 80nm, but aluminum metal is very active and rapidly reacts with oxygen in air to generate aluminum oxide (Al)2O3) In the case of normal incidence, Al2O3The film has remarkable absorption to vacuum ultraviolet light with the wavelength of 80nm to 190nm, and the reflectivity of the film is rapidly reduced in air. Therefore, it is necessary to deposit a protective film on the surface of the aluminum thin film to isolate the influence of air on the aluminum reflective film. Protective films suitable for use in vacuum ultraviolet reflective films are typically made of MgF2，LiF，AlF3，LaF3And preparing the fluoride material.
For a film layer requiring a higher reflectance at a specific wavelength, the fluoride protective film can not only protect the aluminum film from air but also achieve an enhancement in reflectance.
The thickness of the fluoride protective layer for realizing the reflectivity enhancement can be obtained by changing the thickness of the fluoride thin film layer through commercially applied film system design software, so that the maximum reflectivity is obtained, and the optimal thickness of the fluoride thin film layer is determined.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the comparative examples and the embodiments of the present invention. The fluoride protective film layers described in the comparative examples and examples employ MgF2And (5) realizing.
Comparative example:
this comparative example shows the method used for commonly used aluminum-plated vacuum ultraviolet mirrors, and the properties at the vacuum ultraviolet wavelength of aluminum mirrors prepared on the surface of a copper substrate by this method, as a comparison of the methods shown in the present invention.
The method for plating the aluminum vacuum ultraviolet reflector described in the comparative example comprises the following steps:
(1) a copper substrate 25mm in diameter was cleaned by purging the mixed organic solution of alcohol and ether with nitrogen. The surface of the copper substrate is treated by a diamond lathe, and the surface roughness is about 0.8 nm;
(2) placing the copper substrate into a vacuum chamber, and vacuumizing to 2.0 × 10-6mbar, heating the substrate to 80 ℃, conducting electricity by adopting a tungsten wire in a vacuum chamber, heating an aluminum wire for evaporation, and preparing an aluminum film on the substrate. The purity of the used aluminum wire is more than 99.995%, the diameter is 1mm, and the film plating rate of the aluminum film is about 3.0 nm/s;
(3) preparing MgF with thickness of about 5nm on the surface of the aluminum film2Protecting the film, heating the substrate to 200 deg.C, and depositing residual MgF2And (5) protecting the film. The MgF2The total thickness of the film was about 46nm, giving an enhanced reflectivity at 175 nm. The MgF2Heating MgF by tungsten evaporation boat2The film material is prepared by evaporation, and the film coating speed is 0.2 nm/s.
The reflectance spectrum is realized using a vacuum ultraviolet spectrophotometer (ML6500) produced by metelux, germany, and the spectrum shown is the result measured at a beam incidence angle of 10 °.
FIG. 1 is a view showing a vacuum ultraviolet ray coated surface of a copper substrate and a quartz substrate prepared in comparative exampleSpectra of aluminum mirrors were compared. As shown in FIG. 1, 101 is a film using the same aluminum film and MgF as in the comparative example2The reflectivity of 175nm of the reflection spectrum of the aluminum reflector prepared by optically polishing and melting the quartz surface of the film parameter reaches 86.4 percent. 102 is the reflectance spectrum of the aluminum mirror prepared on the copper substrate in this comparative example, with a 175nm reflectance of only 30.2%. The copper substrate is therefore not suitable for direct use in the thermal evaporation preparation of aluminum mirrors.
FIG. 2 shows the result of imaging a cross section of a copper surface aluminum mirror prepared in a comparative example using a transmission electron microscope, the cross section being prepared by a focused ion beam. Determined by the structural characteristics and the coating sequence of the film, 201 is MgF2The protective film 202 is a copper oxide thin film having a thickness of about 1.8nm, which is oxidized by exposing the copper substrate to air, as analyzed by energy dispersion spectroscopy using a transmission electron microscope. Thus located at 202 and MgF2The film layer 203 between the films is an aluminum film, and below 202 is a copper substrate 204.
Energy dispersion spectroscopy measurements were taken on the aluminum mirror prepared in comparative example in a direction perpendicular to the surface of the copper substrate as indicated at 205 in fig. 2 to determine the material composition of the aluminum mirror from air to the interior of the copper substrate, the results being shown in fig. 3. 301 represents fluorine (F) element, 302 magnesium (Mg) element, 303 copper element, 304 aluminum element, and 305 shows the position of the copper oxide film. The measurements show that the interaction of the materials in the aluminum film and the copper substrate forms an alloyed material, causing copper elements to enter the aluminum film, affecting the composition and optical parameters of the aluminum film, resulting in a significant decrease in reflectivity in the reflectivity spectrum 102. The reduction in reflectivity aluminum of aluminum mirrors prepared with copper substrate surfaces relative to fused silica substrate surfaces is therefore due to the alloying of copper and aluminum.
Example 1
FIG. 4 is a structural model of an aluminum reflector on a surface of a copper substrate, which is realized by the method for vacuum ultraviolet coating of an aluminum reflector on a surface of a copper substrate. The structure of the copper-based dielectric spacer comprises a copper substrate 401, a dielectric spacer layer 402 deposited on the copper substrate, an aluminum film 403 deposited on the surface of the dielectric spacer layer, and a fluoride protective film 404 deposited on the surface of the aluminum film 403. According to the method, the dielectric spacing layer is additionally arranged between the surface of the copper substrate and the aluminum film layer, so that the high reflectivity of the aluminum reflector on the copper substrate in a vacuum ultraviolet band is realized. The detailed implementation steps of the coating method of the vacuum ultraviolet aluminum reflector on the surface of the copper substrate are as follows:
(1) and cleaning the copper substrate by using organic liquid modes such as cleaning nitrogen purging alcohol, ether and the like. Because the copper substrate has low hardness, the substrate is damaged by cleaning the surface of the copper substrate in a manual contact mode or by adopting methods such as ultrasonic cleaning and the like, so that organic solvents such as alcohol and the like continuously flowing to the surface of the substrate are swept by nitrogen, dust and oil stains on the surface of the substrate are cleaned by utilizing the interaction between the sweeping pressure acting force of the organic solvents in the nitrogen and the substrate, and organic liquid remained on the surface is removed by utilizing a cleaning nitrogen sweeping mode to obtain a clean copper substrate 401;
(2) a metal oxide or metal fluoride dielectric spacer layer 402 is deposited on the copper substrate surface. The dielectric spacer layer comprises a metal oxide such as SiO2，HfO2，Ta2O5，Al2O3Or metal fluorides such as MgF2，LaF3And the like, can be realized by adopting ion beam sputtering, magnetron sputtering, thermal evaporation and atomic layer deposition coating technology. The medium spacing layer is used for isolating the aluminum and the copper substrate from alloy reaction to form copper-aluminum alloy, can be exposed in the atmospheric environment after being coated in other coating machines, and is transferred and placed into the aluminum reflector coating vacuum chamber in the atmospheric environment; or the plating of the dielectric spacing layer film layer can be firstly completed in the same plating vacuum chamber, and then the plating of the aluminum film and the fluoride film layer can be completed;
(3) and adopting tungsten wires to conduct electricity in a vacuum chamber, heating aluminum wires to evaporate, and preparing the aluminum film 403 on the medium spacing layer. In the film coating process of the aluminum film, the temperature of the substrate is 80-100 ℃;
(4) a fluoride protective film 404 is prepared on the surface of the aluminum reflective film. The fluoride protective film is made of MgF2，LiF，AlF3，LaF3Of equal material preparation to achieve high vacuum ultraviolet reflectivity, fluoride protection of layersThe thickness is optimized, so that the working wavelength of the reflector has high reflectivity; the coating process of the protective film comprises the following steps: firstly, a fluoride protective layer with the thickness of about 5nm is plated at the same substrate temperature as that of the aluminum film plating, then the substrate temperature is raised to 200 ℃ and above, and the residual fluoride film layer is plated.
FIG. 5 is a thin film microstructure of a vacuum ultraviolet aluminum mirror with enhanced reflectivity at 175nm made using the method illustrated in the present invention. The preparation parameters of the reflector are as follows:
(1) a copper substrate 25mm in diameter was cleaned by purging the mixed organic solution of alcohol and ether with nitrogen. The surface of the copper substrate is treated by a diamond lathe, and the surface roughness is about 0.8 nm.
(2) Depositing SiO with the thickness of 10nm on the surface of a copper substrate2Film of said SiO2The film is realized by adopting a German Laibao optical SYRUSpro1110 film coating machine, and SiO is evaporated by an electron gun2Preparing particles, wherein the temperature of the substrate is 160 ℃, the coating speed is 0.4nm/s, and taking the copper substrate out of the vacuum chamber after coating.
(3) Putting the copper substrate into an aluminum reflector coating vacuum chamber, and vacuumizing to 2.0 multiplied by 10-6mbar, heating the substrate to 80 ℃, conducting electricity by adopting a tungsten wire in a vacuum chamber, heating an aluminum wire for evaporation, and preparing an aluminum film on the substrate. The purity of the used aluminum wire is more than 99.995%, the diameter of the aluminum wire is 1mm, and the film coating rate of the aluminum film is about 3.0 nm/s.
(4) Preparing MgF with thickness of about 5nm on the surface of the aluminum film2Protecting the film, heating the substrate to 200 deg.C, and depositing residual MgF2And (5) protecting the film. The MgF2The total thickness of the film was about 46nm, giving an enhanced reflectivity at 175 nm. The MgF2Heating MgF by tungsten evaporation boat2The film material is prepared by evaporation, and the film coating speed is 0.2 nm/s.
According to the analysis of the coating sequence, 501 in FIG. 5 is MgF2The protective film 502 is an aluminum film, 503 is silicon dioxide (SiO)2) The prepared dielectric spacer layer 504 is a copper substrate. As can be seen by comparing the cross-sectional microstructure of the mirror shown in comparative example FIG. 2, SiO2The dielectric spacing layer effectively isolates the copper substrateAnd an aluminum film, so that the formation of copper-aluminum alloy is avoided.
FIG. 6 illustrates the use of MgF2Film and SiO2And after the thin film is used as a medium spacing layer, the reflection spectrum of the aluminum reflection film obtained on the copper substrate. The reflectance spectrum is realized using a vacuum ultraviolet spectrophotometer (ML6500) produced by metelux, germany, and the spectrum shown is the result measured at a beam incidence angle of 10 °. 601 is SiO in this example2Reflectance spectrum of aluminum reflective film on dielectric spacer layer. Compared with the reflectivity of the aluminum reflector directly plated on the copper substrate, the reflectivity is improved by more than 2 times. In FIG. 6, 101 is a case where the same aluminum film and MgF as the comparative example of the present invention were used2The reflectivity of 175nm of an aluminum reflecting mirror prepared on the surface of the optically polished fused quartz reaches 86.4 percent according to film coating parameters.
Example 2
Example 2 use of MgF2As a dielectric spacer, a vacuum ultraviolet aluminum mirror with enhanced reflectivity at 175nm was implemented. The preparation parameters of the reflector are as follows:
(1) a copper substrate 25mm in diameter was cleaned by purging the mixed organic solution of alcohol and ether with nitrogen. The surface of the copper substrate is treated by a diamond lathe, and the surface roughness is about 0.8 nm.
(2) Putting the copper substrate into an aluminum reflector coating vacuum chamber, and vacuumizing to 2.0 multiplied by 10-6mbar, heating the substrate to 200 deg.C, and heating MgF with tungsten evaporation boat2Preparation of MgF by evaporation of film material2The film thickness is 10nm, and the film coating speed is 0.2 nm/s.
(3) And reducing the temperature of the coating vacuum chamber to 80 ℃, adopting a tungsten wire to conduct electricity, heating an aluminum wire to evaporate, and preparing an aluminum film on the substrate. The purity of the used aluminum wire is more than 99.995%, the diameter of the aluminum wire is 1mm, and the film coating rate of the aluminum film is about 3.0 nm/s.
(4) Preparing MgF with thickness of about 5nm on the surface of the aluminum film2Protecting the film, heating the substrate to 200 deg.C, and depositing residual MgF2And (5) protecting the film. The MgF2The total thickness of the film was about 46nm, giving an enhanced reflectivity at 175 nm. The MgF2Heating MgF by tungsten evaporation boat2The film material is prepared by evaporation, and the film coating speed is 0.2 nm/s.
As shown in FIG. 6, the MgF employed in the present embodiment is shown at 6022The reflectance spectrum of the aluminum mirror as the dielectric spacer layer was realized using a vacuum ultraviolet spectrophotometer (ML6500) produced by metelux, germany, and the spectrum shown is the result measured at a beam incident angle of 10 °. In FIG. 6, 101 is a case where the same aluminum film and MgF as the comparative example of the present invention were used2The reflectivity of 175nm of an aluminum reflecting mirror prepared by optically polishing and melting the quartz surface according to the film parameters reaches 86.4 percent.
The difference of the reflectivity of the reflectors plated on the two dielectric spacing layers is mainly caused by the difference of the roughness of the dielectric spacing layers, so that a film layer with lower roughness relative to the surface of the dielectric spacing layer plated by thermal evaporation is prepared by adopting methods such as magnetron sputtering, ion beam sputtering and the like, and the higher reflectivity of the aluminum reflector is obtained.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (8)
1. A coating method of a vacuum ultraviolet aluminum reflector on the surface of a copper substrate is characterized in that the ultraviolet reflector prepared by the method comprises the copper substrate, and a dielectric spacing layer, an aluminum film and a fluoride protective film layer are sequentially plated on the copper substrate from the copper substrate, and the method comprises the following steps:
(1) cleaning the copper substrate by using a nitrogen purging organic solution mode;
(2) depositing a metal oxide or metal fluoride medium spacing layer on the surface of the copper substrate;
(3) preparing an aluminum film on the medium spacing layer in a tungsten filament conductive and heating aluminum filament evaporation mode in a vacuum chamber;
(4) and preparing a fluoride protective film on the surface of the aluminum film.
2. The method as claimed in claim 1, wherein in step (2), the dielectric spacer layer is used to isolate the aluminum film from the copper substrate for alloying reaction to form copper-aluminum alloy.
3. The method according to claim 1, wherein in the step (2), the dielectric spacing layer is exposed to the atmospheric environment after being plated, and the mirror on the surface of the copper substrate is prepared by transferring and placing an aluminum mirror film plating vacuum chamber in the atmospheric environment; or the plating of the dielectric spacing layer film layer is firstly completed in the same plating vacuum chamber, and then the plating of the aluminum film and the fluoride protective film layer is completed.
4. The method of claim 1 wherein in step (2), said dielectric spacer layer comprises a metal oxide or a metal fluoride; preferably, the metal oxide is SiO2，HfO2，Ta2O5Or Al2O3(ii) a Preferably, the metal fluoride is MgF2Or LaF3。
5. The method of claim 1, wherein in step (2), the dielectric spacer layer is formed by ion beam sputtering, magnetron sputtering, thermal evaporation or atomic layer deposition coating.
6. The method according to claim 1, wherein in the step (3), the plating of the aluminum film is performed at a substrate temperature of 80 ℃ to 100 ℃.
7. The method of claim 1, wherein in step (4), the fluoride protective film is formed of MgF2，LiF，AlF3Or LaF3Prepared to achieve high reflectivity in the vacuum ultraviolet wavelength range.
8. The method according to claim 1, wherein in step (4), a fluoride protective layer of 5nm is first formed at the same substrate temperature as in the case of aluminum film plating, and then the substrate temperature is raised to 200 ℃ or higher to form a remaining fluoride film layer.
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| CN109136840A (en) * | 2018-08-06 | 2019-01-04 | 中国科学院光电技术研究所 | A kind of preparation method of vacuum ultraviolet aluminium reflector |
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Application publication date: 20220318 |