CN116904946A - Preparation method of ultraviolet laser reflector and prepared ultraviolet laser reflector - Google Patents
Preparation method of ultraviolet laser reflector and prepared ultraviolet laser reflector Download PDFInfo
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- CN116904946A CN116904946A CN202311167598.9A CN202311167598A CN116904946A CN 116904946 A CN116904946 A CN 116904946A CN 202311167598 A CN202311167598 A CN 202311167598A CN 116904946 A CN116904946 A CN 116904946A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 238000011282 treatment Methods 0.000 claims abstract description 102
- 239000007788 liquid Substances 0.000 claims abstract description 85
- 238000004544 sputter deposition Methods 0.000 claims abstract description 66
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229910001887 tin oxide Inorganic materials 0.000 claims abstract description 45
- 239000000243 solution Substances 0.000 claims abstract description 44
- 238000000498 ball milling Methods 0.000 claims abstract description 40
- 239000000463 material Substances 0.000 claims abstract description 39
- 238000005245 sintering Methods 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 29
- 239000000758 substrate Substances 0.000 claims abstract description 29
- 239000007864 aqueous solution Substances 0.000 claims abstract description 27
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 25
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 24
- 230000004048 modification Effects 0.000 claims abstract description 20
- 238000012986 modification Methods 0.000 claims abstract description 20
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920001661 Chitosan Polymers 0.000 claims abstract description 14
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 12
- 239000007853 buffer solution Substances 0.000 claims abstract description 12
- 239000012530 fluid Substances 0.000 claims abstract description 12
- 239000001509 sodium citrate Substances 0.000 claims abstract description 9
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims description 77
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims description 32
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims description 30
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 19
- 230000001105 regulatory effect Effects 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 17
- 238000005406 washing Methods 0.000 claims description 17
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 14
- 235000010413 sodium alginate Nutrition 0.000 claims description 14
- 239000000661 sodium alginate Substances 0.000 claims description 14
- 229940005550 sodium alginate Drugs 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- 230000008595 infiltration Effects 0.000 claims description 12
- 238000001764 infiltration Methods 0.000 claims description 12
- 238000004321 preservation Methods 0.000 claims description 12
- QKIUAMUSENSFQQ-UHFFFAOYSA-N dimethylazanide Chemical compound C[N-]C QKIUAMUSENSFQQ-UHFFFAOYSA-N 0.000 claims description 10
- 239000000395 magnesium oxide Substances 0.000 claims description 10
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 10
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 10
- 239000003607 modifier Substances 0.000 claims description 10
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 9
- SNAMIIGIIUQQSP-UHFFFAOYSA-N bis(6-methylheptyl) hydrogen phosphate Chemical compound CC(C)CCCCCOP(O)(=O)OCCCCCC(C)C SNAMIIGIIUQQSP-UHFFFAOYSA-N 0.000 claims description 9
- 230000003750 conditioning effect Effects 0.000 claims description 9
- 238000000265 homogenisation Methods 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 8
- VQEHIYWBGOJJDM-UHFFFAOYSA-H lanthanum(3+);trisulfate Chemical compound [La+3].[La+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VQEHIYWBGOJJDM-UHFFFAOYSA-H 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000002310 reflectometry Methods 0.000 abstract description 13
- 230000007797 corrosion Effects 0.000 abstract description 7
- 238000005260 corrosion Methods 0.000 abstract description 7
- 239000002253 acid Substances 0.000 abstract description 6
- 230000000052 comparative effect Effects 0.000 description 10
- 230000000694 effects Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000008055 phosphate buffer solution Substances 0.000 description 3
- 230000035515 penetration Effects 0.000 description 2
- 238000002679 ablation Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 239000003574 free electron Substances 0.000 description 1
- 238000002430 laser surgery Methods 0.000 description 1
- 230000003902 lesion Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000001356 surgical procedure Methods 0.000 description 1
- 238000002211 ultraviolet spectrum Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/08—Mirrors
- G02B5/0891—Ultraviolet [UV] mirrors
-
- 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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
-
- 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
- C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
-
- 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
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention specifically discloses a preparation method of an ultraviolet laser reflector and the ultraviolet laser reflector prepared by the preparation method, wherein the reflector is prepared by adjusting treatment fluid to soak an aluminum substrate, then sputtering a modified sputtering material, and finally sintering and modifying. The product has improved reflectivity stability in the wavelength region, improved durability of acid corrosion resistance and temperature resistance, and coordinated performance; the modified sputtering material is prepared from tin oxide powder, phosphoric acid buffer solution and sodium citrate, yttrium nitrate solution and chitosan aqueous solution are matched to form ball milling modified liquid, the tin oxide powder is modified in a ball milling modification mode, and the optimized modified sputtering material is matched with a sintering process, so that the performance of the product is further improved.
Description
Technical Field
The invention relates to the technical field of reflectors, in particular to a preparation method of an ultraviolet laser reflector and the prepared ultraviolet laser reflector.
Background
Lasers have found wide application in the military, processing, medical and scientific research fields due to their unique irreplaceable properties of monochromaticity, consistency, collimation, etc. The method is commonly used for laser ranging, laser guidance, laser drilling and cutting, atmosphere detection, laser remote sensing, ophthalmic surgery and the like. Depending on the application, different laser wavelengths are often required, for example, in laser surgery, lasers with different wavelengths are required to be selected for different lesions, so as to ensure the ablation effect. The high reflector is one of important optical elements in the research aspects of vacuum ultraviolet band astronomical observation, free electron laser device and the like. Al is the preferred material for the high reflection element in this band, since Al film has the highest inherent reflectivity and better adhesion of any known film material in the uv spectrum region above 100 nm.
The existing Al-based laser reflector has good or bad reflectivity in the ultraviolet spectrum region with the wavelength region more than 100nm and poor stability, and has low reflectivity durability in acid corrosion resistance and temperature resistance, so that the product is difficult to realize stable reflectivity in the wavelength region and poor stability in acid corrosion resistance and temperature resistance.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide an ultraviolet laser reflector and a preparation method thereof so as to solve the problems in the prior art.
The invention solves the technical problems by adopting the following technical scheme:
the invention provides a preparation method of an ultraviolet laser reflector, wherein the reflector is an aluminum substrate which is subjected to infiltration treatment by adjusting treatment fluid, then subjected to sputtering treatment by a modified sputtering material, and finally subjected to sintering modification, so that the ultraviolet laser reflector is obtained;
the specific method comprises the following steps:
step one: placing the aluminum substrate in 4-5 times of adjusting treatment liquid for ultrasonic infiltration treatment, wherein the ultrasonic power is 450-550W, the ultrasonic time is 10-20 min, the ultrasonic temperature is 42-45 ℃, and the ultrasonic treatment is finished, and washing and drying are performed;
step two: sputtering the infiltrated aluminum substrate by using a modified sputtering material, wherein argon is used as a working gas in the sputtering process, the flow is 200-220 sccm, the ion source current is 10-30A, the sputtering power is 30-35 Kw, the electric bias is 100-120V, and the sputtering thickness is 0.45-0.65 mm;
step three: finally, sintering, modifying and heat homogenizing treatment is carried out, and the ultraviolet laser reflector can be obtained after the treatment is finished.
Preferably, the preparation method of the conditioning treatment fluid comprises the following steps:
s01: firstly, carrying out heat treatment on the hydroxyapatite at 55-65 ℃ for 5-10 min, then stirring and dispersing the heat treatment product in 3-5 times of modified liquid uniformly, washing with water and drying to obtain a hydroxyapatite agent;
s02: adding 3-5 parts of 5-10% lanthanum sulfate solution into 10-15 parts of hydrochloric acid solution, and stirring for the first time;
s03: and then adding 2-4 parts of hydroxyapatite modifier and 1-3 parts of sodium dodecyl sulfate into the S02 product, and carrying out secondary stirring treatment to obtain the regulating treatment liquid.
Preferably, the mass fraction of the hydrochloric acid solution is 2-5%.
Preferably, the rotating speed of the primary stirring treatment is 450-650 r/min, the stirring temperature is 42-46 ℃, and the stirring time is 20-30 min; the rotational speed of the secondary stirring treatment is 750-850 r/min, the stirring temperature is 48-50 ℃, and the stirring time is 10-20 min.
Preferably, the modifying liquid comprises the following raw materials in parts by weight: 1-3 parts of N, N-dimethylamide, 2-5 parts of magnesium oxide, 6-10 parts of sodium alginate aqueous solution, 0.45-0.65 part of diisooctyl phosphate and 0.25-0.35 part of silane coupling agent KH560.
Preferably, the mass fraction of the sodium alginate aqueous solution is 10-15%.
Preferably, the preparation method of the modified sputtering material comprises the following steps:
s11: adding tin oxide powder into deionized water according to a weight ratio of 1:5, then adding a phosphoric acid buffer solution accounting for 10-15% of the total weight of the tin oxide powder and sodium citrate accounting for 2-6% of the total weight of the tin oxide powder, and stirring fully to obtain a tin oxide liquid;
s12: adding chitosan water solution into yttrium nitrate solution according to the weight ratio of 3:1, and stirring fully to obtain ball milling regulating solution.
S13: adding ball milling regulating liquid accounting for 20-30% of the total amount into the tin oxide liquid, transferring the tin oxide liquid into a ball mill for ball milling treatment, wherein the ball milling rotating speed is 1000-1500 r/min, ball milling is carried out for 1-2 hours, and after ball milling, water washing and drying are carried out, so as to obtain the modified sputtering material.
Preferably, the pH value of the phosphoric acid buffer solution is 4.5-5.5; the mass fraction of the yttrium nitrate solution is 2-5%; the mass fraction of the chitosan aqueous solution is 4-8%.
Preferably, the specific operation steps of the sintering modification heat homogenization treatment are as follows:
s101: sintering at the temperature of 350-360 ℃ for 10-20 min, then heating to 410-420 ℃ at the speed of 1-3 ℃/min, and continuing sintering for 5-10 min;
s102: then cooling the S101 product to 65-70 ℃ at a speed of 2-5 ℃/min, and carrying out heat preservation treatment;
s103: and then air cooling the heat preservation product to room temperature.
The invention also provides an ultraviolet laser reflector prepared by the preparation method of the ultraviolet laser reflector.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, an aluminum substrate is soaked by adjusting treatment liquid, the adjusting treatment liquid is stirred for one time by using lanthanum sulfate solution and hydrochloric acid solution, then is matched with hydroxyapatite modifier and sodium dodecyl sulfate for secondary stirring, the prepared adjusting treatment liquid can improve the activity penetration of the substrate and the basic penetration, the hydroxyapatite modifier is subjected to heat treatment for 5-10 min at 55-65 ℃ by using hydroxyapatite, the modifying liquid is stirred and modified, the modifying liquid is mutually matched by adopting N, N-dimethylamide, magnesium oxide, sodium alginate aqueous solution, diisooctyl phosphate and silane coupling agent KH560, the modified hydroxyapatite is matched in the adjusting treatment liquid to absorb and bond the substrate, and is matched in the substrate, the modified hydroxyapatite modifier can optimize the bonding strength of the aluminum substrate and a sputtering material, and is matched with the sputtering and sintering modification thermal homogenization treatments of the sputtering material, the reflectivity stability of the wavelength region of the product is improved, the stability of the corrosion resistance and the temperature resistance performance is improved, and the performance of the product is coordinated.
The modified sputtering material is prepared from tin oxide powder, phosphoric acid buffer solution and sodium citrate, yttrium nitrate solution and chitosan aqueous solution are matched to form ball milling modified liquid, the tin oxide powder is modified in a ball milling modification mode, and the optimized modified sputtering material is matched with a sintering process, so that the performance of the product is further improved.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
According to the preparation method of the ultraviolet laser reflector, an aluminum substrate is firstly soaked by adjusting treatment liquid, then is sputtered by a modified sputtering material, and finally is sintered and modified, so that the ultraviolet laser reflector can be obtained;
the specific method comprises the following steps:
step one: placing the aluminum substrate in 4-5 times of adjusting treatment liquid for ultrasonic infiltration treatment, wherein the ultrasonic power is 450-550W, the ultrasonic time is 10-20 min, the ultrasonic temperature is 42-45 ℃, and the ultrasonic treatment is finished, and washing and drying are performed;
step two: sputtering the infiltrated aluminum substrate by using a modified sputtering material, wherein argon is used as a working gas in the sputtering process, the flow is 200-220 sccm, the ion source current is 10-30A, the sputtering power is 30-35 Kw, the electric bias is 100-120V, and the sputtering thickness is 0.45-0.65 mm;
step three: finally, sintering, modifying and heat homogenizing treatment is carried out, and the ultraviolet laser reflector can be obtained after the treatment is finished.
The preparation method of the conditioning treatment fluid in this embodiment is as follows:
s01: firstly, carrying out heat treatment on the hydroxyapatite at 55-65 ℃ for 5-10 min, then stirring and dispersing the heat treatment product in 3-5 times of modified liquid uniformly, washing with water and drying to obtain a hydroxyapatite agent;
s02: adding 3-5 parts of 5-10% lanthanum sulfate solution into 10-15 parts of hydrochloric acid solution, and stirring for the first time;
s03: and then adding 2-4 parts of hydroxyapatite modifier and 1-3 parts of sodium dodecyl sulfate into the S02 product, and carrying out secondary stirring treatment to obtain the regulating treatment liquid.
Wherein the mass fraction of the hydrochloric acid solution is 2-5%.
Specifically, the rotating speed of one-time stirring treatment is 450-650 r/min, the stirring temperature is 42-46 ℃, and the stirring time is 20-30 min; the rotational speed of the secondary stirring treatment is 750-850 r/min, the stirring temperature is 48-50 ℃, and the stirring time is 10-20 min.
The modified liquid comprises the following raw materials in parts by weight: 1-3 parts of N, N-dimethylamide, 2-5 parts of magnesium oxide, 6-10 parts of sodium alginate aqueous solution, 0.45-0.65 part of diisooctyl phosphate and 0.25-0.35 part of silane coupling agent KH560.
Specifically, the mass fraction of the sodium alginate aqueous solution is 10-15%.
Specifically, the preparation method of the modified sputtering material comprises the following steps:
s11: adding tin oxide powder into deionized water according to a weight ratio of 1:5, then adding a phosphoric acid buffer solution accounting for 10-15% of the total weight of the tin oxide powder and sodium citrate accounting for 2-6% of the total weight of the tin oxide powder, and stirring fully to obtain a tin oxide liquid;
s12: adding chitosan aqueous solution into yttrium nitrate solution according to the weight ratio of 3:1, and stirring fully to obtain ball milling regulating solution;
s13: adding ball milling regulating liquid accounting for 20-30% of the total amount into the tin oxide liquid, transferring the tin oxide liquid into a ball mill for ball milling treatment, wherein the ball milling rotating speed is 1000-1500 r/min, ball milling is carried out for 1-2 hours, and after ball milling, water washing and drying are carried out, so as to obtain the modified sputtering material.
Wherein the pH value of the phosphoric acid buffer solution is 4.5-5.5; the mass fraction of the yttrium nitrate solution is 2-5%; the mass fraction of the chitosan aqueous solution is 4-8%.
Specifically, the specific operation steps of the sintering modification heat homogenization treatment are as follows:
s101: sintering at the temperature of 350-360 ℃ for 10-20 min, then heating to 410-420 ℃ at the speed of 1-3 ℃/min, and continuing sintering for 5-10 min;
s102: then cooling the S101 product to 65-70 ℃ at a speed of 2-5 ℃/min, and carrying out heat preservation treatment;
s103: and then air cooling the heat preservation product to room temperature.
The ultraviolet laser reflector is prepared by the preparation method of the ultraviolet laser reflector.
Example 1
According to the preparation method of the ultraviolet laser reflector, the reflector is an aluminum substrate which is subjected to infiltration treatment firstly through adjusting treatment liquid, then subjected to sputtering treatment through a modified sputtering material, and finally subjected to sintering modification, so that the ultraviolet laser reflector can be obtained;
the specific method comprises the following steps:
step one: placing the aluminum substrate in 4 times of adjusting treatment liquid for ultrasonic infiltration treatment, wherein the ultrasonic power is 450W, the ultrasonic time is 10min, the ultrasonic temperature is 42 ℃, and the ultrasonic treatment is finished, washed and dried;
step two: sputtering the infiltrated aluminum substrate by using a modified sputtering material, wherein argon is used as working gas in sputtering, the flow is 200sccm, the ion source current is 10A, the sputtering power is 30Kw, the electric bias is 100V, and the sputtering thickness is 0.45mm;
step three: finally, sintering, modifying and heat homogenizing treatment is carried out, and the ultraviolet laser reflector can be obtained after the treatment is finished.
The preparation method of the conditioning treatment fluid in this embodiment is as follows:
s01: firstly, placing the hydroxyapatite into a modified liquid with the temperature of 55 ℃ for heat treatment for 5min, then stirring and dispersing the heat treatment product in the modified liquid with the weight of 3 times uniformly, and washing and drying the mixture after the stirring is finished to obtain a hydroxyapatite agent;
s02: adding 3 parts of 5% lanthanum sulfate solution into 10 parts of hydrochloric acid solution, and stirring for the first time;
s03: then adding 2 parts of hydroxyapatite modifier and 1 part of sodium dodecyl sulfate into the S02 product, and stirring again to obtain the regulating treatment liquid.
The mass fraction of the hydrochloric acid solution of this example was 2%.
The rotational speed of the primary stirring treatment in the embodiment is 450r/min, the stirring temperature is 42 ℃, and the stirring time is 20min; the rotational speed of the secondary stirring treatment is 750r/min, the stirring temperature is 48 ℃, and the stirring time is 10min.
The modified liquid of the embodiment comprises the following raw materials in parts by weight: 1 part of N, N-dimethylamide, 2 parts of magnesium oxide, 6 parts of sodium alginate aqueous solution, 0.45 part of diisooctyl phosphate and 0.25 part of silane coupling agent KH560.
The mass fraction of the sodium alginate aqueous solution of this example was 10%.
The preparation method of the modified sputtering material of the embodiment comprises the following steps:
s11: adding tin oxide powder into deionized water according to a weight ratio of 1:5, then adding a phosphoric acid buffer solution accounting for 10% of the total weight of the tin oxide powder and sodium citrate accounting for 2% of the total weight of the tin oxide powder, and stirring fully to obtain a tin oxide liquid;
s12: adding chitosan aqueous solution into yttrium nitrate solution according to the weight ratio of 3:1, and stirring fully to obtain ball milling regulating solution;
s13: adding ball milling regulating liquid accounting for 20% of the total amount into the tin oxide liquid, transferring the tin oxide liquid into a ball mill for ball milling treatment, wherein the ball milling rotating speed is 1000r/min, ball milling is carried out for 1h, and after ball milling, water washing and drying are carried out, thus obtaining the modified sputtering material.
The pH of the phosphate buffer solution of this example was 4.5; the mass fraction of the yttrium nitrate solution is 2%; the mass fraction of the chitosan aqueous solution is 4%.
The specific operation steps of the sintering modification heat homogenization treatment in this embodiment are as follows:
s101: sintering at 350 ℃ for 10min, then heating to 410 ℃ at a speed of 1 ℃/min, and continuing sintering for 5min;
s102: then cooling the S101 product to 65 ℃ at a speed of 2 ℃/min, and carrying out heat preservation treatment;
s103: and then air cooling the heat preservation product to room temperature.
Example 2
According to the preparation method of the ultraviolet laser reflector, the reflector is an aluminum substrate, the aluminum substrate is subjected to infiltration treatment through adjusting treatment fluid, then subjected to sputtering treatment through modified sputtering materials, and finally subjected to sintering modification, so that the ultraviolet laser reflector can be obtained;
the specific method comprises the following steps:
step one: placing the aluminum substrate in 5 times of adjusting treatment liquid for ultrasonic infiltration treatment, wherein the ultrasonic power is 550W, the ultrasonic time is 20min, the ultrasonic temperature is 45 ℃, the ultrasonic treatment is finished, and the aluminum substrate is washed and dried;
step two: sputtering the infiltrated aluminum substrate by using a modified sputtering material, wherein argon is used as working gas in sputtering, the flow is 220sccm, the ion source current is 30A, the sputtering power is 35Kw, the electric bias is 120V, and the sputtering thickness is 0.65mm;
step three: finally, sintering, modifying and heat homogenizing treatment is carried out, and the ultraviolet laser reflector can be obtained after the treatment is finished.
The preparation method of the conditioning treatment fluid in this embodiment is as follows:
s01: firstly, placing the hydroxyapatite into a modified liquid with the temperature of 65 ℃ for heat treatment for 10min, then stirring and dispersing the heat treatment product in the modified liquid with the weight of 5 times uniformly, and washing and drying the mixture after the stirring is finished to obtain a hydroxyapatite agent;
s02: adding 5 parts of 10% lanthanum sulfate solution into 15 parts of hydrochloric acid solution, and stirring for the first time;
s03: then adding 4 parts of hydroxyapatite modifier and 3 parts of sodium dodecyl sulfate into the S02 product, and stirring for the second time to obtain the regulating treatment liquid.
The mass fraction of the hydrochloric acid solution of this example was 5%.
The rotational speed of the primary stirring treatment in the embodiment is 650r/min, the stirring temperature is 46 ℃, and the stirring time is 30min; the rotational speed of the secondary stirring treatment is 850r/min, the stirring temperature is 50 ℃, and the stirring time is 20min.
The modified liquid of the embodiment comprises the following raw materials in parts by weight: 3 parts of N, N-dimethylamide, 5 parts of magnesium oxide, 10 parts of sodium alginate aqueous solution, 0.65 part of diisooctyl phosphate and 0.35 part of silane coupling agent KH560.
The mass fraction of the sodium alginate aqueous solution of this example was 15%.
The preparation method of the modified sputtering material of the embodiment comprises the following steps:
s11: adding tin oxide powder into deionized water according to a weight ratio of 1:5, then adding a phosphoric acid buffer solution accounting for 15% of the total weight of the tin oxide powder and sodium citrate accounting for 6% of the total weight of the tin oxide powder, and stirring fully to obtain a tin oxide liquid;
s12: adding chitosan aqueous solution into yttrium nitrate solution according to the weight ratio of 3:1, and stirring fully to obtain ball milling regulating solution;
s13: adding 30% of ball milling regulating liquid into the tin oxide liquid, transferring to a ball mill for ball milling treatment, wherein the ball milling rotating speed is 1500r/min, ball milling is carried out for 2 hours, and after ball milling, water washing and drying are carried out, thus obtaining the modified sputtering material.
The pH of the phosphate buffer solution of this example was 5.5; the mass fraction of the yttrium nitrate solution is 2-5%; the mass fraction of the chitosan aqueous solution is 8%.
The specific operation steps of the sintering modification heat homogenization treatment in this embodiment are as follows:
s101: sintering at 360 ℃ for 20min, then heating to 420 ℃ at a rate of 3 ℃/min, and continuing sintering for 10min;
s102: then cooling the S101 product to 70 ℃ at a speed of 5 ℃/min, and carrying out heat preservation treatment;
s103: and then air cooling the heat preservation product to room temperature.
Example 3
According to the preparation method of the ultraviolet laser reflector, the reflector is an aluminum substrate, the aluminum substrate is subjected to infiltration treatment through adjusting treatment fluid, then subjected to sputtering treatment through modified sputtering materials, and finally subjected to sintering modification, so that the ultraviolet laser reflector can be obtained;
the specific method comprises the following steps:
step one: placing the aluminum substrate in 4.5 times of adjusting treatment liquid for ultrasonic infiltration treatment, wherein the ultrasonic power is 500W, the ultrasonic time is 15min, the ultrasonic temperature is 43 ℃, the ultrasonic treatment is finished, and the aluminum substrate is washed and dried;
step two: sputtering the infiltrated aluminum substrate by using a modified sputtering material, wherein argon is used as working gas in sputtering, the flow is 210sccm, the ion source current is 20A, the sputtering power is 32.5Kw, the electric bias is 110V, and the sputtering thickness is 0.50mm;
step three: finally, sintering, modifying and heat homogenizing treatment is carried out, and the ultraviolet laser reflector can be obtained after the treatment is finished.
The preparation method of the conditioning treatment fluid in this embodiment is as follows:
s01: firstly, placing the hydroxyapatite into a modification liquid with the temperature of 60 ℃ for heat treatment for 7.5min, then stirring and dispersing the heat treatment product in the modification liquid with the weight of 4 times uniformly, and washing and drying the mixture after stirring is finished to obtain a hydroxyapatite agent;
s02: adding 4 parts of 7.5% lanthanum sulfate solution into 12.5 parts of hydrochloric acid solution, and stirring for the first time;
s03: then adding 3 parts of hydroxyapatite modifier and 2 parts of sodium dodecyl sulfate into the S02 product, and stirring for the second time to obtain the regulating treatment liquid.
The mass fraction of the hydrochloric acid solution of this example was 3.5%.
The rotational speed of the primary stirring treatment in the embodiment is 500r/min, the stirring temperature is 44 ℃, and the stirring time is 25min; the rotation speed of the secondary stirring treatment is 800r/min, the stirring temperature is 49 ℃, and the stirring time is 15min.
The modified liquid of the embodiment comprises the following raw materials in parts by weight: 2 parts of N, N-dimethylamide, 3.5 parts of magnesium oxide, 8 parts of sodium alginate aqueous solution, 0.50 part of diisooctyl phosphate and 0.30 part of silane coupling agent KH560.
The mass fraction of the sodium alginate aqueous solution of this example was 12.5%.
The preparation method of the modified sputtering material of the embodiment comprises the following steps:
s11: adding tin oxide powder into deionized water according to a weight ratio of 1:5, then adding a phosphoric acid buffer solution accounting for 12% of the total weight of the tin oxide powder and sodium citrate accounting for 4% of the total weight of the tin oxide powder, and stirring fully to obtain a tin oxide liquid;
s12: adding chitosan aqueous solution into yttrium nitrate solution according to the weight ratio of 3:1, and stirring fully to obtain ball milling regulating solution;
s13: adding ball milling regulating liquid accounting for 25% of the total amount into the tin oxide liquid, transferring the tin oxide liquid into a ball mill for ball milling treatment, wherein the ball milling rotating speed is 1250r/min, ball milling is carried out for 1.5 hours, and after ball milling, water washing and drying are carried out, thus obtaining the modified sputtering material.
The pH of the phosphate buffer solution of this example was 4.7; the mass fraction of the yttrium nitrate solution is 3.5%; the mass fraction of the chitosan aqueous solution is 6%.
The specific operation steps of the sintering modification heat homogenization treatment in this embodiment are as follows:
s101: sintering at 355 ℃ for 15min, then heating to 415 ℃ at a rate of 2 ℃/min, and continuing sintering for 7.5min;
s102: then cooling the S101 product to 67 ℃ at a speed of 3.5 ℃/min, and carrying out heat preservation treatment;
s103: and then air cooling the heat preservation product to room temperature.
Comparative example 1
The difference from example 3 is that no conditioning treatment liquid infiltration was used.
Comparative example 2
The difference from example 3 is that no hydroxyapatite agent was added in the preparation of the conditioning treatment liquid.
Comparative example 3
The difference from example 3 is that no modification liquid treatment was used in the preparation of the hydroxyapatite agent.
Comparative example 4
The procedure for preparing the conditioning treatment fluid was as follows, except for example 3:
s01: uniformly stirring and dispersing the hydroxyapatite in 4 times of modified liquid, and washing and drying after stirring is finished to obtain a hydroxyapatite agent;
s02: adding 4 parts of lanthanum sulfate solution with the mass fraction of 7.5% into 12.5 parts of hydrochloric acid solution, adding 3 parts of hydroxyapatite modifier and 2 parts of sodium dodecyl sulfate, and stirring to obtain a regulating treatment solution; the stirring speed is 800r/min, the stirring temperature is 49 ℃, the stirring time is 25min, and the preparation of the modified liquid is the same as that of the invention.
Comparative example 5
The difference from example 3 is that the modified sputter material is replaced by tin oxide.
Comparative example 6
The difference from example 3 is the preparation method of the modified sputter material:
adding tin oxide powder into deionized water according to a weight ratio of 1:5, then adding a phosphoric acid buffer solution with the total amount of 12% of the tin oxide powder and sodium citrate with the total amount of 4% of the tin oxide powder, stirring fully to obtain tin oxide liquid, washing with water, and drying to obtain the modified sputtering material.
Comparative example 7
The difference from example 3 is that no sinter modification heat homogenization treatment was employed.
The products of examples 1 to 3 and comparative examples 1 to 7 were tested for reflectivity at wavelengths of 110nm, 115nm and 120nm under conventional conditions, and for acid corrosion resistance at 2% acid corrosion conditions for 1 hour and at 65℃for 2 hours, with the following results.
As can be seen from comparative examples 1 to 7 and examples 1 to 3;
the product of the embodiment 3 has excellent reflectivity, the reflectivity of the product is excellent in the wavelength regions of 110nm, 115nm and 120nm, the reflectivity performance is stable, and meanwhile, the reflectivity of the product can be continuously stable under the acid corrosion and temperature resistance performance, and the performance coordination of the product is improved;
as shown in comparative examples 1-7, the products are not immersed by the adjusting treatment liquid, the modified sputtering material is replaced by tin oxide and the sintering modification thermal homogenization treatment is not adopted, the reflectivity performance of the products is obviously deteriorated, the three are adopted to cooperate, the performance of the products is synergistically enhanced, the performance improvement is obvious, the hydroxyapatite agent is not added in the preparation of the adjusting treatment liquid, the modification liquid is not adopted in the preparation of the hydroxyapatite agent, the preparation methods of the adjusting treatment liquid are different, the performances of the products are in a deterioration trend, and the performance effect of the products is obvious only by adopting the adjusting treatment liquid prepared by the method of the invention.
In addition, the preparation methods of the modified sputtering material are different, the performance of the product also tends to be poor, and meanwhile, the inventor of the invention also finds that the preparation of the hydroxyapatite agent is not treated by a modified liquid, so that the performance of the product is obviously poor, and based on the modified sputtering material, the invention further improves the product;
the invention further explores the product performance through the hydroxyapatite agent treated by the modifying liquid;
the modified liquid comprises the following raw materials in parts by weight: 2 parts of N, N-dimethylamide, 3.5 parts of magnesium oxide, 8 parts of sodium alginate aqueous solution, 0.50 part of diisooctyl phosphate and 0.30 part of silane coupling agent KH560.
Experimental example 1
The procedure of example 3 was repeated except that N, N-dimethylamide was not added to the modified liquid.
Experimental example 2
The procedure of example 3 was repeated except that magnesium oxide was not added to the modified liquid.
Experimental example 3
The procedure of example 3 was repeated except that diisooctyl phosphate was not added to the modified liquid.
Experimental example 4
The procedure of example 3 was repeated except that the silane coupling agent KH560 was not added to the modified liquid.
As can be seen from experimental examples 1-4, the reflectivity performance of the product is most obvious due to the fact that no magnesium oxide is added into the modified liquid, the performance is most obviously deteriorated among the composition factors of the modified liquid, the composition of the modified liquid is different due to the fact that no N, N-dimethylamide is added, the performance of the product is prone to be deteriorated, and meanwhile, the performance effect of the product is most obvious due to the fact that only raw materials of the modified liquid are adopted for compounding, and the effect of the modified liquid is not obvious compared with that of the modified liquid which is formed by adopting other raw materials instead of the modified liquid.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (10)
1. The preparation method of the ultraviolet laser reflector is characterized in that the reflector is an aluminum substrate, the aluminum substrate is subjected to infiltration treatment by adjusting treatment fluid, then subjected to sputtering treatment by modified sputtering materials, and finally subjected to sintering modification, so that the ultraviolet laser reflector is obtained;
the specific method comprises the following steps:
step one: placing the aluminum substrate in 4-5 times of adjusting treatment liquid for ultrasonic infiltration treatment, wherein the ultrasonic power is 450-550W, the ultrasonic time is 10-20 min, the ultrasonic temperature is 42-45 ℃, and the ultrasonic treatment is finished, and washing and drying are performed;
step two: sputtering the infiltrated aluminum substrate by using a modified sputtering material, wherein argon is used as a working gas in the sputtering process, the flow is 200-220 sccm, the ion source current is 10-30A, the sputtering power is 30-35 Kw, the electric bias is 100-120V, and the sputtering thickness is 0.45-0.65 mm;
step three: finally, sintering, modifying and heat homogenizing treatment is carried out, and the ultraviolet laser reflector can be obtained after the treatment is finished.
2. The method for preparing an ultraviolet laser reflecting mirror according to claim 1, wherein the method for preparing the conditioning treatment fluid comprises the following steps:
s01: firstly, carrying out heat treatment on the hydroxyapatite at 55-65 ℃ for 5-10 min, then stirring and dispersing the heat treatment product in 3-5 times of modified liquid uniformly, washing with water and drying to obtain a hydroxyapatite agent;
s02: adding 3-5 parts of 5-10% lanthanum sulfate solution into 10-15 parts of hydrochloric acid solution, and stirring for the first time;
s03: and then adding 2-4 parts of hydroxyapatite modifier and 1-3 parts of sodium dodecyl sulfate into the S02 product, and carrying out secondary stirring treatment to obtain the regulating treatment liquid.
3. The method for preparing the ultraviolet laser reflecting mirror according to claim 2, wherein the mass fraction of the hydrochloric acid solution is 2-5%.
4. The method for manufacturing an ultraviolet laser reflecting mirror according to claim 2, wherein the rotational speed of the primary stirring treatment is 450-650 r/min, the stirring temperature is 42-46 ℃, and the stirring time is 20-30 min; the rotational speed of the secondary stirring treatment is 750-850 r/min, the stirring temperature is 48-50 ℃, and the stirring time is 10-20 min.
5. The method for preparing the ultraviolet laser reflecting mirror according to claim 2, wherein the modifying liquid comprises the following raw materials in parts by weight: 1-3 parts of N, N-dimethylamide, 2-5 parts of magnesium oxide, 6-10 parts of sodium alginate aqueous solution, 0.45-0.65 part of diisooctyl phosphate and 0.25-0.35 part of silane coupling agent KH560.
6. The method for preparing the ultraviolet laser reflecting mirror according to claim 5, wherein the mass fraction of the sodium alginate aqueous solution is 10-15%.
7. The method for preparing an ultraviolet laser reflecting mirror according to claim 1, wherein the method for preparing the modified sputtering material is as follows:
s11: adding tin oxide powder into deionized water according to a weight ratio of 1:5, then adding a phosphoric acid buffer solution accounting for 10-15% of the total weight of the tin oxide powder and sodium citrate accounting for 2-6% of the total weight of the tin oxide powder, and stirring fully to obtain a tin oxide liquid;
s12: adding chitosan aqueous solution into yttrium nitrate solution according to the weight ratio of 3:1, and stirring fully to obtain ball milling regulating solution;
s13: adding ball milling regulating liquid accounting for 20-30% of the total amount into the tin oxide liquid, transferring the tin oxide liquid into a ball mill for ball milling treatment, wherein the ball milling rotating speed is 1000-1500 r/min, ball milling is carried out for 1-2 hours, and after ball milling, water washing and drying are carried out, so as to obtain the modified sputtering material.
8. The method for preparing an ultraviolet laser reflecting mirror according to claim 7, wherein the pH value of the phosphoric acid buffer solution is 4.5-5.5; the mass fraction of the yttrium nitrate solution is 2-5%; the mass fraction of the chitosan aqueous solution is 4-8%.
9. The method for preparing an ultraviolet laser reflecting mirror according to claim 1, wherein the specific operation steps of the sintering modification heat homogenization treatment are as follows:
s101: sintering at the temperature of 350-360 ℃ for 10-20 min, then heating to 410-420 ℃ at the speed of 1-3 ℃/min, and continuing sintering for 5-10 min;
s102: then cooling the S101 product to 65-70 ℃ at a speed of 2-5 ℃/min, and carrying out heat preservation treatment;
s103: and then air cooling the heat preservation product to room temperature.
10. An ultraviolet laser mirror prepared by the method for preparing an ultraviolet laser mirror according to any one of claims 1 to 9.
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CN106796312A (en) * | 2014-10-27 | 2017-05-31 | 阿尔姆科有限责任公司 | The surface reflector of temperature and corrosion stable |
CN114114490A (en) * | 2021-12-06 | 2022-03-01 | 湖北久之洋红外系统股份有限公司 | Ultralow-stress durable metal reflecting film and preparation method and application thereof |
CN116356248A (en) * | 2023-03-28 | 2023-06-30 | 嘉兴敏惠汽车零部件有限公司 | Light transmission color regulating and controlling method for PVD millimeter wave-transmitting metal film |
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CN102141642A (en) * | 2010-02-01 | 2011-08-03 | 株式会社神户制钢所 | Reflective film laminate |
CN106796312A (en) * | 2014-10-27 | 2017-05-31 | 阿尔姆科有限责任公司 | The surface reflector of temperature and corrosion stable |
CN114114490A (en) * | 2021-12-06 | 2022-03-01 | 湖北久之洋红外系统股份有限公司 | Ultralow-stress durable metal reflecting film and preparation method and application thereof |
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