CN116356248A - Light transmission color regulating and controlling method for PVD millimeter wave-transmitting metal film - Google Patents
Light transmission color regulating and controlling method for PVD millimeter wave-transmitting metal film Download PDFInfo
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- CN116356248A CN116356248A CN202310309541.1A CN202310309541A CN116356248A CN 116356248 A CN116356248 A CN 116356248A CN 202310309541 A CN202310309541 A CN 202310309541A CN 116356248 A CN116356248 A CN 116356248A
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 30
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- 238000000034 method Methods 0.000 title claims abstract description 23
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- 239000003607 modifier Substances 0.000 claims abstract description 56
- 229920001661 Chitosan Polymers 0.000 claims abstract description 38
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- 238000002156 mixing Methods 0.000 claims abstract description 15
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 15
- 238000007747 plating Methods 0.000 claims abstract description 8
- 238000007598 dipping method Methods 0.000 claims abstract 5
- 238000003756 stirring Methods 0.000 claims description 76
- 238000000498 ball milling Methods 0.000 claims description 45
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims description 37
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- 238000001035 drying Methods 0.000 claims description 31
- 238000005406 washing Methods 0.000 claims description 31
- 239000007864 aqueous solution Substances 0.000 claims description 29
- -1 sodium alkyl sulfonate Chemical class 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 21
- 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 21
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 20
- 239000003795 chemical substances by application Substances 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 19
- 238000009725 powder blending Methods 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 14
- 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 13
- 239000000661 sodium alginate Substances 0.000 claims description 13
- 235000010413 sodium alginate Nutrition 0.000 claims description 13
- 229940005550 sodium alginate Drugs 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 12
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 12
- 239000011734 sodium Substances 0.000 claims description 12
- 229910052708 sodium Inorganic materials 0.000 claims description 12
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 12
- QZCLKYGREBVARF-UHFFFAOYSA-N Acetyl tributyl citrate Chemical compound CCCCOC(=O)CC(C(=O)OCCCC)(OC(C)=O)CC(=O)OCCCC QZCLKYGREBVARF-UHFFFAOYSA-N 0.000 claims description 8
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 8
- 239000005977 Ethylene Substances 0.000 claims description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 8
- 239000012530 fluid Substances 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
- 239000002994 raw material Substances 0.000 claims description 8
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 claims description 8
- 229940039790 sodium oxalate Drugs 0.000 claims description 8
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 7
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 7
- 239000007853 buffer solution Substances 0.000 claims description 7
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 7
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 7
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 6
- YOCUPQPZWBBYIX-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Cu] YOCUPQPZWBBYIX-UHFFFAOYSA-N 0.000 claims description 6
- 239000008055 phosphate buffer solution Substances 0.000 claims description 6
- 235000002906 tartaric acid Nutrition 0.000 claims description 6
- 239000011975 tartaric acid Substances 0.000 claims description 6
- FWFGVMYFCODZRD-UHFFFAOYSA-N oxidanium;hydrogen sulfate Chemical compound O.OS(O)(=O)=O FWFGVMYFCODZRD-UHFFFAOYSA-N 0.000 claims description 4
- ZBYSZWDYDUIDAZ-UHFFFAOYSA-M sodium octadec-2-enoate Chemical compound [Na+].CCCCCCCCCCCCCCCC=CC([O-])=O ZBYSZWDYDUIDAZ-UHFFFAOYSA-M 0.000 claims description 4
- 239000002585 base Substances 0.000 abstract description 13
- 239000003513 alkali Substances 0.000 abstract description 6
- 239000000203 mixture Substances 0.000 abstract description 6
- 230000006872 improvement Effects 0.000 abstract description 3
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- 230000000052 comparative effect Effects 0.000 description 18
- 238000005470 impregnation Methods 0.000 description 16
- 238000005240 physical vapour deposition Methods 0.000 description 12
- 230000000694 effects Effects 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
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- 230000035699 permeability Effects 0.000 description 4
- 230000009977 dual effect Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 102100034112 Alkyldihydroxyacetonephosphate synthase, peroxisomal Human genes 0.000 description 2
- 101000799143 Homo sapiens Alkyldihydroxyacetonephosphate synthase, peroxisomal Proteins 0.000 description 2
- UMHKOAYRTRADAT-UHFFFAOYSA-N [hydroxy(octoxy)phosphoryl] octyl hydrogen phosphate Chemical compound CCCCCCCCOP(O)(=O)OP(O)(=O)OCCCCCCCC UMHKOAYRTRADAT-UHFFFAOYSA-N 0.000 description 2
- 238000000848 angular dependent Auger electron spectroscopy Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
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- 230000002195 synergetic effect Effects 0.000 description 2
- 238000009966 trimming Methods 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
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- 239000002131 composite material Substances 0.000 description 1
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- 230000008451 emotion Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
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- 238000003475 lamination Methods 0.000 description 1
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- 150000003839 salts Chemical class 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Classifications
-
- 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
- C23C14/0015—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterized by the colour of the layer
-
- 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
-
- 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
- C23C14/10—Glass or silica
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
-
- 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
- C23C14/5846—Reactive treatment
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/0009—Materials therefor
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/0102—Constructional details, not otherwise provided for in this subclass
Abstract
The invention discloses a light transmission color regulating and controlling method of a PVD millimeter wave-transmitting metal film, which comprises the following steps: the base layer color regulating film is sent into 8-12 times of chitosan complex-mixing treatment liquid for ultrasonic dispersion treatment, and the treatment is finished, washed and dried; preparing a double-regulating modifier; then the mixture is placed into a double modifier of 5 to 10 times for dipping treatment, and the treatment is finished, washed and dried. According to the invention, through plating of high and low refractive index film layers with different thicknesses, color adjustment of the film coating film layer is realized, ultrasonic dispersion treatment is carried out through chitosan complex modulation treatment liquid, and then dipping treatment is carried out in a complex modulation modifier, so that the prepared metal film can realize millimeter wave transmission improvement, wave transmission uniformity optimization and product coordination performance improvement on the basis of adjustable color, and meanwhile, the product has stable performance under the saline-alkali condition.
Description
Technical Field
The invention relates to the technical field of composite rollers, in particular to a light transmission color regulating method of a PVD millimeter wave-transmission metal film.
Background
With the rapid development of electric, intelligent and light weight of automobiles, various innovative products are developed for the interior and exterior trim parts of automobiles. The luminous intelligent B-pillar board comprises luminous signs, luminous grids, luminous decorative strips, automobile luminous intelligent B-pillar boards and the like. Currently, automotive lighting exterior trim parts exhibit metallic bright silver when not lighted, and require projection using a white D65 light source with a light transmittance of 10% -20% when lighted. Meanwhile, most of the luminous exterior trimming parts are provided with ADAS millimeter wave radars, and millimeter waves need to be transmitted through the ADAS millimeter wave radars.
In the process of realizing these luminescent exterior trim pieces, PVD, physical vapor deposition, is widely used. The technology utilizes the modes of evaporation, sputtering and the like to deposit various film layers on the surface of a product under the vacuum condition, so that a very thin coating is obtained on the surface, and the technology has the advantages of rapidness, strong adhesive force and the like. Meanwhile, the PVD coating technology is an environment-friendly coating technology and has wide application in the fields of decoration, functionality and the like.
In addition, digital grilles are a popular trend in the current automotive industry. The digital grille can be used as a carrier of automobile brand LOGO, design idea and emotion appeal, and integrates modeling and functions. Furthermore, the digital grille can cover the engine room, so that the automobile body is purer.
In summary, with the rapid development of electric, intelligent and light weight of automobiles, interior and exterior trim parts of automobiles are continuously innovated. The light-emitting exterior trimming parts, the digital grids and other trend products are widely applied in the automobile industry. Meanwhile, the PVD coating technology is also attracting more attention in the field of coating, and becomes an important means for beautifying and improving functions of automobile interior and exterior trim parts.
The existing product realizes color regulation and control through multilayer base film lamination, but millimeter wave transmission is reduced, wave transmission is uneven, and the coordination performance of the millimeter wave transmission and the wave transmission is poor, so that the use of the product is limited, and the stability of the product is obviously reduced under the saline-alkali condition, so that the use efficiency of the product is reduced.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a light transmission color regulating method of a PVD millimeter wave-transmitting metal film, 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 light transmission color regulating method of a PVD millimeter wave-transmitting metal film, which comprises the following steps:
step one: setting of a base layer color regulation film: the color of the film is regulated and controlled by setting a nickel-copper plated metal film layer with the thickness of 50nm, a silicon oxide plated film layer with the thickness of 10nm and a titanium oxide plated film layer with the thickness of 10nm, and repeatedly plating the silicon oxide film layer and the titanium oxide film layer for 2-5 times;
step two: sending the base layer color regulating film in the step one into 8-12 times of chitosan complex-mixing treatment liquid for ultrasonic dispersion treatment, and after the treatment is finished, washing and drying;
step three: preparation of a double-regulating modifier:
step four: and (3) immersing the product obtained in the step (II) in a double modifier which is 5-10 times of the product, and washing and drying the product after the treatment is finished.
Preferably, the ultrasonic power of the ultrasonic dispersion is 500-1000W, the ultrasonic time is 20-30min, and the ultrasonic temperature is 42-45 ℃.
Preferably, the preparation method of the chitosan complex-mixing treatment fluid comprises the following steps:
s01: adding 3-6 parts of 5% chitosan aqueous solution by mass into 10-15 parts of sodium alginate aqueous solution, then adding 0.2-0.5 part of phosphoric acid buffer solution, and uniformly stirring;
s02: adding 1-5 parts of silane coupling agent into the S01 product, adding 0.2-0.5 part of sodium alkyl sulfonate and 0.25-0.35 part of carboxymethyl cellulose, and stirring fully to obtain chitosan remixing treatment liquid.
Preferably, the mass fraction of the sodium alginate aqueous solution is 10-15%; the pH value of the phosphate buffer solution is 5.0.
Preferably, the silane coupling agent is a silane coupling agent KH560.
Preferably, the preparation method of the double-regulating modifier comprises the following steps:
s101: feeding ITO powder into a furnace at 100-110 ℃ for heat treatment for 10-20min, and then air-cooling to 40-45 ℃ at a speed of 1-3 ℃/min;
s102: adding the S101 product into sulfuric acid water solution 3-5 times of the S101 product, carrying out primary stirring modification treatment, then adding lanthanum sulfate 2-5% and sodium oxalate 1-3% of the total amount of the S02 product, carrying out secondary stirring modification, washing with water, and drying to obtain an ITO powder blending agent;
s103: adding hydroxyapatite into hydrochloric acid solution with the mass fraction of 5% which is 3-5 times that of the hydroxyapatite, stirring uniformly, then adding ITO powder blending agent with the total amount of 4-7% of the hydroxyapatite, stirring fully, washing with water, and drying to obtain the hydroxyapatite complex modulation modifier;
s104: adding the hydroxyapatite compound modifier into ball milling liquid accounting for 5-10% of the total amount of the hydroxyapatite compound modifier, performing ball milling modification treatment, wherein the ball milling rotating speed is 1000-1500r/min, the ball milling time is 45-55min, and performing water washing and drying after ball milling to obtain the double-adjustment modifier.
Preferably, the mass concentration of the sulfuric acid aqueous solution is 5-10%.
Preferably, the rotational speed of the primary stirring modification is 300-400r/min, the stirring time is 10-20min, and the stirring temperature is 45-50 ℃; the rotation speed of the secondary stirring modification is 800-1200r/min, the stirring time is 35-45min, and the stirring temperature is 40-42 ℃.
Preferably, the ball milling liquid comprises the following raw materials in parts by weight:
3-5 parts of acetyl tributyl citrate, 10-15 parts of ethanol, 1-5 parts of bis (dioctyl-oxy-pyrophosphato) ethylene titanate, 0.25-0.45 part of tartaric acid and 0.5-0.9 part of sodium octadecenoate.
Preferably, the impregnation pressure of the impregnation treatment is 10-15MPa, and the impregnation time is 20-25min.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, through plating of high and low refractive index film layers with different thicknesses, the color of a film coating film layer is adjustable, through ultrasonic dispersion treatment of chitosan complex modulation treatment liquid, and then matching with immersion treatment in a double modulation modifier, the prepared metal film can realize improvement of millimeter wave transmission on the basis of adjustable color, optimized wave transmission uniformity, improved product coordination performance, and stable performance of the product under saline-alkali conditions; the chitosan compound modified treatment fluid adopts chitosan aqueous solution, sodium alginate aqueous solution and phosphoric acid buffer solution to compound the most basal body, enhances the surface capacity, activation and modification of the basal body on the metal film, simultaneously, the silane coupling agent, sodium alkyl sulfonate and carboxymethyl cellulose are matched, the interfacial activity of the metal film is further optimized, the optimized synergistic effect is achieved for the subsequent impregnation of the double-modified agent, the double-modified agent adopts ITO powder to perform heat treatment and constant temperature cooling, the first-stage stirring modification treatment and the second-stage stirring modification treatment in sulfuric acid aqueous solution, lanthanum sulfate and sodium oxalate are performed, the raw materials are matched through a multistage modification method, the optimized ITO powder modifier is matched with hydroxyapatite to cooperate together, and synergistic effect is achieved, so that the formed hydroxyapatite compound modified agent can further optimize the uniformity of the film layer, simultaneously, the wave transmission effect of the film layer is improved, the wave transmission uniformity is enhanced, finally, the ball milling liquid ball milling modification is performed, the raw material coordination modification through ball milling liquid is performed, and the salt and alkali resistance stability of the modified product is remarkably 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.
The light transmission color regulation and control method of the PVD millimeter wave-transmitting metal film comprises the following steps:
step one: setting of a base layer color regulation film: the color of the film is regulated and controlled by setting a nickel-copper plated metal film layer with the thickness of 50nm, a silicon oxide plated film layer with the thickness of 10nm and a titanium oxide plated film layer with the thickness of 10nm, and repeatedly plating the silicon oxide film layer and the titanium oxide film layer for 2-5 times;
step two: sending the base layer color regulating film in the step one into 8-12 times of chitosan complex-mixing treatment liquid for ultrasonic dispersion treatment, and after the treatment is finished, washing and drying;
step three: preparation of a double-regulating modifier:
step four: and (3) immersing the product obtained in the step (II) in a double modifier which is 5-10 times of the product, and washing and drying the product after the treatment is finished.
The ultrasonic power of the ultrasonic dispersion of the embodiment is 500-1000W, the ultrasonic time is 20-30min, and the ultrasonic temperature is 42-45 ℃.
The preparation method of the chitosan complex-mixing treatment fluid in the embodiment comprises the following steps:
s01: adding 3-6 parts of 5% chitosan aqueous solution by mass into 10-15 parts of sodium alginate aqueous solution, then adding 0.2-0.5 part of phosphoric acid buffer solution, and uniformly stirring;
s02: adding 1-5 parts of silane coupling agent into the S01 product, adding 0.2-0.5 part of sodium alkyl sulfonate and 0.25-0.35 part of carboxymethyl cellulose, and stirring fully to obtain chitosan remixing treatment liquid.
The mass fraction of the sodium alginate aqueous solution in the embodiment is 10-15%; the pH value of the phosphate buffer solution is 5.0.
The silane coupling agent of this example is a silane coupling agent KH560.
The preparation method of the double-regulating modifier comprises the following steps:
s101: feeding ITO powder into a furnace at 100-110 ℃ for heat treatment for 10-20min, and then air-cooling to 40-45 ℃ at a speed of 1-3 ℃/min;
s102: adding the S101 product into sulfuric acid water solution 3-5 times of the S101 product, carrying out primary stirring modification treatment, then adding lanthanum sulfate 2-5% and sodium oxalate 1-3% of the total amount of the S02 product, carrying out secondary stirring modification, washing with water, and drying to obtain an ITO powder blending agent;
s103: adding hydroxyapatite into hydrochloric acid solution with the mass fraction of 5% which is 3-5 times that of the hydroxyapatite, stirring uniformly, then adding ITO powder blending agent with the total amount of 4-7% of the hydroxyapatite, stirring fully, washing with water, and drying to obtain the hydroxyapatite complex modulation modifier;
s104: adding the hydroxyapatite compound modifier into ball milling liquid accounting for 5-10% of the total amount of the hydroxyapatite compound modifier, performing ball milling modification treatment, wherein the ball milling rotating speed is 1000-1500r/min, the ball milling time is 45-55min, and performing water washing and drying after ball milling to obtain the double-adjustment modifier.
The mass concentration of the sulfuric acid aqueous solution of this example was 5-10%.
The rotational speed of the primary stirring modification is 300-400r/min, the stirring time is 10-20min, and the stirring temperature is 45-50 ℃; the rotation speed of the secondary stirring modification is 800-1200r/min, the stirring time is 35-45min, and the stirring temperature is 40-42 ℃.
The ball milling liquid of the embodiment comprises the following raw materials in parts by weight:
3-5 parts of acetyl tributyl citrate, 10-15 parts of ethanol, 1-5 parts of bis (dioctyl-oxy-pyrophosphato) ethylene titanate, 0.25-0.45 part of tartaric acid and 0.5-0.9 part of sodium octadecenoate.
The impregnation pressure of the impregnation treatment of this example was 10-15MPa and the impregnation time was 20-25min.
Example 1.
The light transmission color regulation and control method of the PVD millimeter wave-transmitting metal film comprises the following steps:
step one: setting of a base layer color regulation film: the color of the film is regulated and controlled by setting a nickel-copper plated metal film layer with the thickness of 50nm, a silicon oxide plated film layer with the thickness of 10nm and a titanium oxide plated film layer with the thickness of 10nm, and repeatedly plating the silicon oxide film layer and the titanium oxide film layer for 2 times;
step two: sending the base layer color regulating film in the first step into 8 times of chitosan complex-mixing treatment liquid for ultrasonic dispersion treatment, and after the treatment is finished, washing and drying;
step three: preparation of a double-regulating modifier:
step four: and (3) immersing the product obtained in the step (II) in a double modifier of which the time is 5 times, washing with water and drying.
The ultrasonic power of the ultrasonic dispersion in this example was 500W, the ultrasonic time was 20min, and the ultrasonic temperature was 42 ℃.
The preparation method of the chitosan complex-mixing treatment fluid in the embodiment comprises the following steps:
s01: adding 3 parts of 5% chitosan aqueous solution by mass into 10 parts of sodium alginate aqueous solution, then adding 0.2 part of phosphoric acid buffer solution, and uniformly stirring;
s02: adding 1 part of silane coupling agent into the S01 product, adding 0.2 part of sodium alkyl sulfonate and 0.25 part of carboxymethyl cellulose, and stirring thoroughly to obtain chitosan remixing treatment liquid.
The mass fraction of the sodium alginate aqueous solution in the embodiment is 10%; the pH value of the phosphate buffer solution is 5.0.
The silane coupling agent of this example is a silane coupling agent KH560.
The preparation method of the double-regulating modifier comprises the following steps:
s101: feeding the ITO powder into a furnace for heat treatment at 100 ℃ for 10min, and then air-cooling to 40 ℃ at a speed of 1 ℃/min;
s102: adding the S101 product into sulfuric acid water solution which is 3 times of the S101 product, carrying out primary stirring modification treatment, then adding lanthanum sulfate which is 2% of the total amount of the S02 product and sodium oxalate which is 1% of the total amount of the S02 product, carrying out secondary stirring modification, washing with water, and drying to obtain an ITO powder blending agent;
s103: adding hydroxyapatite into hydrochloric acid solution with the mass fraction of 5% which is 3 times that of the hydroxyapatite, stirring uniformly, then adding ITO powder blending agent with the mass fraction of 4% of the total amount of the hydroxyapatite, stirring fully, washing with water, and drying to obtain the hydroxyapatite compound modifier;
s104: adding the hydroxyapatite compound modifier into ball milling liquid accounting for 5% of the total amount of the hydroxyapatite compound modifier, performing ball milling modification treatment, wherein the ball milling rotating speed is 1000r/min, the ball milling time is 45min, and performing water washing and drying after ball milling to obtain the double-adjustment modifier.
The mass concentration of the aqueous sulfuric acid solution of this example was 5%.
The rotational speed of the primary stirring modification is 300r/min, the stirring time is 10min, and the stirring temperature is 45 ℃; the rotation speed of the secondary stirring modification is 800r/min, the stirring time is 35min, and the stirring temperature is 40 ℃.
The ball milling liquid of the embodiment comprises the following raw materials in parts by weight:
3 parts of acetyl tributyl citrate, 10 parts of ethanol, 1 part of bis (dioctyl-oxy-pyrophosphato) ethylene titanate, 0.25 part of tartaric acid and 0.5 part of sodium stearyl.
The impregnation pressure of the impregnation treatment of this example was 10MPa and the impregnation time was 20min.
Example 2.
The light transmission color regulation and control method of the PVD millimeter wave-transmitting metal film comprises the following steps:
step one: setting of a base layer color regulation film: the color of the film is regulated and controlled by setting a nickel-copper plated metal film layer with the thickness of 50nm, a silicon oxide plated film layer with the thickness of 10nm and a titanium oxide plated film layer with the thickness of 10nm, and repeatedly plating the silicon oxide film layer and the titanium oxide film layer for 5 times;
step two: sending the base layer color regulating film in the first step into 12 times of chitosan complex-mixing treatment liquid for ultrasonic dispersion treatment, and after the treatment is finished, washing and drying;
step three: preparation of a double-regulating modifier:
step four: and (3) immersing the product obtained in the step (II) in 10 times of double modifier, washing with water and drying.
The ultrasonic power of the ultrasonic dispersion in this example was 1000W, the ultrasonic time was 30min, and the ultrasonic temperature was 45 ℃.
The preparation method of the chitosan complex-mixing treatment fluid in the embodiment comprises the following steps:
s01: adding 6 parts of 5% chitosan aqueous solution by mass into 15 parts of sodium alginate aqueous solution, then adding 0.5 part of phosphoric acid buffer solution, and uniformly stirring;
s02: and 5 parts of silane coupling agent is added into the S01 product, then 0.5 part of sodium alkyl sulfonate and 0.35 part of carboxymethyl cellulose are added, and the mixture is fully stirred, so that the chitosan remixing treatment liquid is obtained.
The mass fraction of the sodium alginate aqueous solution in the embodiment is 15%; the pH value of the phosphate buffer solution is 5.0.
The silane coupling agent of this example is a silane coupling agent KH560.
The preparation method of the double-regulating modifier comprises the following steps:
s101: feeding the ITO powder into a furnace at 110 ℃ for heat treatment for 20min, and then air-cooling to 45 ℃ at a speed of 3 ℃/min;
s102: adding the S101 product into a sulfuric acid aqueous solution which is 5 times of the S101 product, carrying out primary stirring modification treatment, then adding lanthanum sulfate which is 5% of the total amount of the S02 product and sodium oxalate which is 3%, carrying out secondary stirring modification, washing with water, and drying to obtain an ITO powder blending agent;
s103: adding hydroxyapatite into 5 times of hydrochloric acid solution with the mass fraction of 5%, uniformly stirring, then adding ITO powder blending agent with the mass fraction of 7% of the total amount of the hydroxyapatite, fully stirring, washing with water, and drying to obtain the hydroxyapatite compound modifier;
s104: adding the hydroxyapatite compound modifier into ball milling liquid accounting for 10 percent of the total amount of the hydroxyapatite compound modifier, performing ball milling modification treatment, wherein the ball milling rotating speed is 1500r/min, the ball milling time is 55min, and performing water washing and drying after ball milling to obtain the double-adjustment modifier.
The mass concentration of the aqueous sulfuric acid solution of this example was 10%.
The rotational speed of the primary stirring modification is 400r/min, the stirring time is 20min, and the stirring temperature is 50 ℃; the rotation speed of the secondary stirring modification is 1200r/min, the stirring time is 45min, and the stirring temperature is 42 ℃.
The ball milling liquid of the embodiment comprises the following raw materials in parts by weight:
5 parts of acetyl tributyl citrate, 15 parts of ethanol, 5 parts of bis (dioctyl-oxy-pyrophosphato) ethylene titanate, 0.45 part of tartaric acid and 0.9 part of sodium stearyl.
The impregnation pressure of the impregnation treatment of this example was 15MPa and the impregnation time was 25min.
Example 3.
The light transmission color regulation and control method of the PVD millimeter wave-transmitting metal film comprises the following steps:
step one: setting of a base layer color regulation film: the color of the film is regulated and controlled by setting a nickel-copper plated metal film layer with the thickness of 50nm, a silicon oxide plated film layer with the thickness of 10nm and a titanium oxide plated film layer with the thickness of 10nm, and repeatedly plating the silicon oxide film layer and the titanium oxide film layer for 4 times;
step two: sending the base layer color regulating film in the first step into 10 times of chitosan complex-mixing treatment liquid for ultrasonic dispersion treatment, and after the treatment is finished, washing and drying;
step three: preparation of a double-regulating modifier:
step four: and (3) immersing the product obtained in the step (II) in a double modifier of which the number is 7, washing with water and drying.
The ultrasonic power of the ultrasonic dispersion of this example was 750W, the ultrasonic time was 25min, and the ultrasonic temperature was 43 ℃.
The preparation method of the chitosan complex-mixing treatment fluid in the embodiment comprises the following steps:
s01: adding 4 parts of 5% chitosan aqueous solution by mass into 12 parts of sodium alginate aqueous solution, then adding 0.35 part of phosphoric acid buffer solution, and uniformly stirring;
s02: 3 parts of silane coupling agent is added into the S01 product, then 0.35 part of sodium alkyl sulfonate and 0.30 part of carboxymethyl cellulose are added, and the mixture is stirred fully, so that the chitosan remixing treatment liquid is obtained.
The mass fraction of the sodium alginate aqueous solution in the embodiment is 12%; the pH value of the phosphate buffer solution is 5.0.
The silane coupling agent of this example is a silane coupling agent KH560.
The preparation method of the double-regulating modifier comprises the following steps:
s101: feeding the ITO powder into a furnace at 105 ℃ for heat treatment for 15min, and then air-cooling to 42 ℃ at a speed of 2 ℃/min;
s102: adding the S101 product into a sulfuric acid aqueous solution with the concentration of 4 times that of the S101 product, carrying out primary stirring modification treatment, then adding lanthanum sulfate with the concentration of 3.5% and sodium oxalate with the concentration of 2% in the total amount of the S02 product, carrying out secondary stirring modification, washing with water, and drying to obtain an ITO powder blending agent;
s103: adding hydroxyapatite into hydrochloric acid solution with the mass fraction of 5% which is 4 times that of the hydroxyapatite, uniformly stirring, then adding ITO powder blending agent with the mass fraction of 5% of the total amount of the hydroxyapatite, fully stirring, washing with water, and drying to obtain the hydroxyapatite compound modifier;
s104: adding the hydroxylapatite compound modifier into ball milling liquid accounting for 7.5 percent of the total amount of the hydroxylapatite compound modifier, performing ball milling modification treatment, wherein the ball milling rotating speed is 1250r/min, the ball milling time is 50min, and after ball milling, washing and drying to obtain the double-adjustment modifier.
The mass concentration of the aqueous sulfuric acid solution of this example was 7.5%.
The rotational speed of the primary stirring modification is 350r/min, the stirring time is 15min, and the stirring temperature is 47 ℃; the rotation speed of the secondary stirring modification is 1000r/min, the stirring time is 40min, and the stirring temperature is 41 ℃.
The ball milling liquid of the embodiment comprises the following raw materials in parts by weight:
4 parts of acetyl tributyl citrate, 12.5 parts of ethanol, 3 parts of bis (dioctyl-oxy-pyrophosphate) ethylene titanate, 0.30 part of tartaric acid and 0.7 part of sodium stearyl acid.
The impregnation pressure of the impregnation treatment of this example was 12.5MPa and the impregnation time was 22min.
Comparative example 1.
The difference from example 3 is that the chitosan complex-modulated treatment solution was not used.
Comparative example 2.
The difference from example 3 is that sodium alkyl sulfonate is not added in the preparation of the chitosan complex preparation treatment fluid.
Comparative example 3.
The difference from example 3 is that no silane coupling agent is added in the preparation of the chitosan complex preparation treatment liquid.
Comparative example 4.
The difference from example 3 is that deionized water is used instead of the chitosan aqueous solution in the preparation of the chitosan complex-preparation treatment solution.
Comparative example 5.
The difference from example 3 is that no ITO powder modifier is added in the preparation of the dual modifier.
Comparative example 6.
The difference from example 3 is that the ITO powder formulation agent is replaced with ITO powder.
Comparative example 7.
The difference from example 3 is that the preparation of the ITO powder formulation did not use S101 treatment.
Comparative example 8.
The preparation method of the ITO powder blending agent is different from that of the embodiment 3, and the other steps are the same except that;
adding the S101 product into a sulfuric acid aqueous solution which is 4 times of the S101 product, then adding lanthanum sulfate accounting for 3.5% of the total amount of the S02 product and sodium oxalate accounting for 2%, stirring and modifying, wherein the stirring and modifying speed is 1000r/min, the stirring time is 40min, and the stirring temperature is 47 ℃; and after modification, washing and drying to obtain the ITO powder blending agent.
Comparative example 9.
The difference from example 3 is that no ball milling solution treatment was used in the preparation of the dual modifier.
Comparative example 10.
The difference from example 3 is that no acetyl tributyl citrate was added to the ball milling liquid.
Comparative example 11.
The difference from example 3 is that bis (dioctyl pyrophosphate) ethylene titanate was not added to the ball mill liquor.
Comparative example 12.
Except that sodium octadecenoic acid was not added to the ball milling liquid as in example 3.
Comparative example 13.
The difference from example 3 is that the base layer color control film of step one is used without any treatment.
Test conditions: and the angle intersection measurement, azimuth angle, -55 degrees, elevation angle: -30 DEG, the distance between the radar antenna and the product is 30mm, and a 76.5GHz millimeter wave radar is adopted for bidirectional attenuation test.
Meanwhile, the product is placed for 24 hours under the conventional condition and under the condition of 2% sodium chloride salt fog, and then the wave-transmitting performance of the product is tested;
and at azimuth angles of 5 ° and 10 °, elevation angles of 30 °; measuring the wave permeability of the product at the positions of azimuth angle 55 degrees and elevation angle-5 degrees respectively, and observing the wave permeability of the product at all directions;
the products of examples 1-3 and comparative examples 1-13 were subjected to performance testing;
as can be seen from comparative examples 1 to 13 and examples 1 to 3; the product of example 3 has excellent wave-transmitting properties, excellent wave-transmitting effects in different directions, strong wave-transmitting uniformity, and excellent wave-transmitting stability.
As can be seen from comparative examples 1 to 4 and example 3, the wave-transmitting property and the wave-transmitting uniformity of the product are obviously deteriorated without adopting the chitosan complex-mixing treatment solution, sodium alkyl sulfonate is not added in the preparation of the chitosan complex-mixing treatment solution, a silane coupling agent is not added, the chitosan aqueous solution is replaced by deionized water, the performance of the product is in a deterioration trend, and only the chitosan complex-mixing treatment solution prepared by the method has the most obvious performance effect;
as can be seen from comparative examples 5-8 and example 3, the preparation of the dual modifier is not added with the ITO powder modifier, the wave permeability and the wave permeability uniformity of the product are both obviously deteriorated, meanwhile, the ITO powder modifier is replaced by the ITO powder, and the performance of the product is obviously deteriorated under the saline-alkali condition; in addition, the preparation of the ITO powder blending agent is not processed by S101, the preparation methods of the ITO powder blending agent are different, and the performance of the product is prone to deterioration;
as can be seen from comparative examples 6-13 and example 3, the performance of the product is obviously degraded without ball milling liquid treatment in the preparation of the double-regulating modifier, and the performances of the product are all degraded without adding acetyl tributyl citrate, di (dioctyl pyrophosphate) ethylene titanate and sodium octadecenoate in the ball milling liquid, and only the ball milling liquid prepared by the mixture ratio of the invention is matched with the double-regulating modifier prepared by other processes of the double-regulating modifier, so that the performance effect of the product is most obvious, and the wave-transmitting property, wave-transmitting uniformity and saline-alkali stability effect of the product are most obvious.
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 light transmission color regulating and controlling method of the PVD millimeter wave-transmitting metal film is characterized by comprising the following steps of:
step one: setting of a base layer color regulation film: the color of the film is regulated and controlled by setting a nickel-copper plated metal film layer with the thickness of 50nm, a silicon oxide plated film layer with the thickness of 10nm and a titanium oxide plated film layer with the thickness of 10nm, and repeatedly plating the silicon oxide film layer and the titanium oxide film layer for 2-5 times;
step two: sending the base layer color regulating film in the step one into 8-12 times of chitosan complex-mixing treatment liquid for ultrasonic dispersion treatment, and after the treatment is finished, washing and drying;
step three: preparation of a double-regulating modifier:
step four: and (3) immersing the product obtained in the step (II) in a double modifier which is 5-10 times of the product, and washing and drying the product after the treatment is finished.
2. The method for regulating and controlling the light transmission color of the PVD millimeter wave-transmitting metal film according to claim 1, wherein the ultrasonic power of ultrasonic dispersion is 500-1000W, the ultrasonic time is 20-30min, and the ultrasonic temperature is 42-45 ℃.
3. The method for regulating and controlling the light transmission color of the PVD millimeter wave-transmitting metal film according to claim 1, wherein the preparation method of the chitosan complex regulating treatment fluid is as follows:
s01: adding 3-6 parts of 5% chitosan aqueous solution by mass into 10-15 parts of sodium alginate aqueous solution, then adding 0.2-0.5 part of phosphoric acid buffer solution, and uniformly stirring;
s02: adding 1-5 parts of silane coupling agent into the S01 product, adding 0.2-0.5 part of sodium alkyl sulfonate and 0.25-0.35 part of carboxymethyl cellulose, and stirring fully to obtain chitosan remixing treatment liquid.
4. The light-transmitting color regulating method of the PVD millimeter wave-transmitting metal film according to claim 3, wherein the mass fraction of the sodium alginate aqueous solution is 10-15%; the pH value of the phosphate buffer solution is 5.0.
5. The method for regulating and controlling the light transmission color of the PVD millimeter wave-transmitting metal film according to claim 3, wherein the silane coupling agent is silane coupling agent KH560.
6. The method for regulating and controlling the light transmission color of the PVD millimeter wave-transmitting metal film according to claim 1, wherein the preparation method of the double-regulating modifier is as follows:
s101: feeding ITO powder into a furnace at 100-110 ℃ for heat treatment for 10-20min, and then air-cooling to 40-45 ℃ at a speed of 1-3 ℃/min;
s102: adding the S101 product into sulfuric acid water solution 3-5 times of the S101 product, carrying out primary stirring modification treatment, then adding lanthanum sulfate 2-5% and sodium oxalate 1-3% of the total amount of the S02 product, carrying out secondary stirring modification, washing with water, and drying to obtain an ITO powder blending agent;
s103: adding hydroxyapatite into hydrochloric acid solution with the mass fraction of 5% which is 3-5 times that of the hydroxyapatite, stirring uniformly, then adding ITO powder blending agent with the total amount of 4-7% of the hydroxyapatite, stirring fully, washing with water, and drying to obtain the hydroxyapatite complex modulation modifier;
s104: adding the hydroxyapatite compound modifier into ball milling liquid accounting for 5-10% of the total amount of the hydroxyapatite compound modifier, performing ball milling modification treatment, wherein the ball milling rotating speed is 1000-1500r/min, the ball milling time is 45-55min, and performing water washing and drying after ball milling to obtain the double-adjustment modifier.
7. The method for controlling the light transmission color of the PVD millimeter wave-transmitting metal film according to claim 6, wherein the mass concentration of the sulfuric acid aqueous solution is 5-10%.
8. The method for regulating and controlling the light transmission color of the PVD millimeter wave-transmitting metal film according to claim 6, wherein the primary stirring modification speed is 300-400r/min, the stirring time is 10-20min, and the stirring temperature is 45-50 ℃; the rotation speed of the secondary stirring modification is 800-1200r/min, the stirring time is 35-45min, and the stirring temperature is 40-42 ℃.
9. The method for regulating and controlling the light transmission color of the PVD millimeter wave-transmitting metal film according to claim 6, wherein the ball milling liquid comprises the following raw materials in parts by weight:
3-5 parts of acetyl tributyl citrate, 10-15 parts of ethanol, 1-5 parts of bis (dioctyl-oxy-pyrophosphato) ethylene titanate, 0.25-0.45 part of tartaric acid and 0.5-0.9 part of sodium octadecenoate.
10. The method for regulating and controlling the light transmission color of the PVD millimeter wave-transmitting metal film according to claim 1, wherein the dipping pressure of the dipping treatment is 10-15MPa, and the dipping time is 20-25min.
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| CN116904946B (en) * | 2023-09-12 | 2023-12-08 | 江苏天凯光电有限公司 | Preparation method of ultraviolet laser reflector and prepared ultraviolet laser reflector |
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