CN115584145A - Preparation method of low-emissivity colored composite pigment - Google Patents
Preparation method of low-emissivity colored composite pigment Download PDFInfo
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- 239000000049 pigment Substances 0.000 title claims abstract description 42
- 239000002131 composite material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 62
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 48
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910052709 silver Inorganic materials 0.000 claims abstract description 38
- 239000004332 silver Substances 0.000 claims abstract description 38
- 238000000576 coating method Methods 0.000 claims abstract description 31
- 239000011248 coating agent Substances 0.000 claims abstract description 29
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 24
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 21
- 238000007747 plating Methods 0.000 claims abstract description 12
- 238000003980 solgel method Methods 0.000 claims abstract description 11
- 238000004040 coloring Methods 0.000 claims abstract description 10
- 238000000975 co-precipitation Methods 0.000 claims abstract description 9
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 24
- 238000004544 sputter deposition Methods 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 239000002244 precipitate Substances 0.000 claims description 17
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 14
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 14
- 238000000151 deposition Methods 0.000 claims description 14
- 230000008021 deposition Effects 0.000 claims description 14
- 239000012153 distilled water Substances 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- 239000004094 surface-active agent Substances 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 10
- 239000003513 alkali Substances 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 239000002585 base Substances 0.000 claims description 5
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 4
- 229920000570 polyether Polymers 0.000 claims description 4
- 229920000223 polyglycerol Polymers 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 3
- 150000007942 carboxylates Chemical class 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- 239000010452 phosphate Substances 0.000 claims description 3
- UEZVMMHDMIWARA-UHFFFAOYSA-M phosphonate Chemical compound [O-]P(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-M 0.000 claims description 3
- 238000006068 polycondensation reaction Methods 0.000 claims description 3
- 239000000758 substrate Substances 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 3
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- 230000001276 controlling effect Effects 0.000 description 16
- 229910052782 aluminium Inorganic materials 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- 230000003595 spectral effect Effects 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
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- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 239000011246 composite particle Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- UCNNJGDEJXIUCC-UHFFFAOYSA-L hydroxy(oxo)iron;iron Chemical compound [Fe].O[Fe]=O.O[Fe]=O UCNNJGDEJXIUCC-UHFFFAOYSA-L 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000011146 organic particle Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
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- 230000005855 radiation Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0081—Composite particulate pigments or fillers, i.e. containing at least two solid phases, except those consisting of coated particles of one compound
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/62—Metallic pigments or fillers
- C09C1/64—Aluminium
- C09C1/642—Aluminium treated with inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/063—Coating
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/066—Treatment or coating resulting in a free metal containing surface-region
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/30—Camouflage paints
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Abstract
The invention discloses a preparation method of a low-emissivity colored composite pigment, which comprises the following steps: s1, magnetron sputtering silver plating; s2: coating the silver layer by a sol-gel method; s3: coloring by a coprecipitation method. The composite pigment prepared by the scheme has good compatibility and stealth performance in visible light and infrared bands. The emissivity is regulated and controlled through the thickness of the silver coating on the surface of the aluminum powder, the infrared stealth requirement is met, and compared with the method that pure silver powder is used as a substrate, the cost of silver-coated aluminum powder is lower. The silver layer is protected by the silicon dioxide, so that oxidation is prevented, the weather resistance is improved, and the hydrophilicity of the silicon dioxide layer and the pits on the surface are beneficial to the compounding of the pigment, so that the invisible requirement of visible light is met.
Description
Technical Field
The invention relates to the technical field of stealth coatings, in particular to a preparation method of a low-emissivity colored composite pigment.
Background
In the technical development of stealth coating materials, the low-emissivity coating achieves the effect of reducing the detected rate of a target material through extremely low infrared heat radiation. Meanwhile, in order to realize the visible light stealth (camouflage) effect of the material, the requirement is also provided for the color diversity of the stealth coating, and the infrared and visible light synchronous stealth (camouflage) can be compatible finally. Most of the low-emissivity coatings developed at present have the disadvantages of complex processing process, harsh production environment, high cost and poor product stability. In the infrared stealth field, the common color metallic pigment in the current market hardly meets the requirement of enough low emission rate; in the field of visible light stealth, the existing infrared stealth coating products are colorized, but the existing infrared stealth coating products are still insufficient in color types, do not reach the standard in colorimetry data, and are difficult to be compatible with the low-emissivity performance requirement.
The flake aluminum powder is easy to obtain due to low price, and is used as a preferred pigment of the low-emissivity coating. The aluminum flake pigment has low thermal infrared reflection characteristics, but shows high brightness and whiteness in visible light, which has great adverse effect on the visible light color modulation band required by the stealth coating. In addition, the simple aluminum is very easy to oxidize, and the emissivity is greatly increased after oxidation, so that the performance is deteriorated. The silver simple substance has excellent low emissivity property and is not easy to oxidize in air, but also shows high brightness and high whiteness in visible light. In addition, the silver powder directly used as a coating substrate has high cost and is not easy to obtain, and is not suitable for mass production.
Research shows that the surface of the flake aluminum powder is coated with one or more layers of inorganic or organic particles by physical or chemical means, so that the composite particles have various particle characteristics at the same time, and the effect of coloring the aluminum powder or attaching other functional characteristics is achieved. The method has the advantages that a layer of metal oxide is directly coated on the surface of the flake aluminum powder by adopting a liquid phase precipitation method, the process is simple, the particle structure is simple, the low-emissivity characteristic is realized, the pigment firmness is poor, and the aluminum in an aqueous phase environment is extremely easy to corrode. CN200510027121.6 discloses a surface coating F with low emissivitye 3 O 4 An aluminum flake pigment and a preparation method thereof. The sheet aluminum powder coated with iron black on the surface has the average particle diameter of 1-100 mu m, no luster, tan color and the average emissivity of an infrared band (the wavelength is 8-14 mu m) of 0.50-0.65. However, the temperature of the reaction system in the preparation process of the method is between 65 and 98 ℃, the aluminum powder is easy to oxidize and corrode, and in addition, fe is easy to generate 2 O 3 Impurities affect the color requirement, so the emissivity is difficult to be lower, and the extremely low emissivity required by the stealth coating is not met. CN201911305627.7 provides SiO 2 The preparation method of the color aluminum pigment with double-layer coating of the color pigment is to form a layer of SiO on the surface of the flaky aluminum pigment 2 Film, thereby improving the corrosion resistance of aluminum powder, siO 2 The intermediate layer can enhance the adhesive force of pigment particles, the color is stable, but the infrared emissivity of the pigment is greatly changed due to the increase of the thickness of the coating layer, and the emissivity cannot be reduced to a greater extent. Therefore, how to overcome the extremely low emissivity required by the existing color aluminum pigment for the infrared stealth coating, and simultaneously satisfy the color diversification required by the visible light stealth field becomes a problem to be solved in the stealth coating technology.
Disclosure of Invention
The invention aims to provide a preparation method of a low-emissivity color composite pigment, which is used for solving the technical problems in the background technology.
The technical scheme of the invention provides a preparation method of a low-emissivity color composite pigment, which comprises the following steps:
s1, magnetron sputtering silver plating: the scaly aluminum powder with the grain diameter of 60-70 microns is spread on the sputtering base material; placing the sputtering substrate into a magnetron sputtering anode cover, adjusting sputtering parameters, performing sputtering reaction for 5-40min, cooling to room temperature after sputtering is finished, and taking out;
s2: coating the silver layer by a sol-gel method: through the hydrolysis-polycondensation reaction of ethyl orthosilicate, hydrated silicon dioxide precipitate is generated and deposited on the surface of the silver-plated aluminum powder, and the silver-plated aluminum powder coated with silicon dioxide is obtained.
S3: coloring by a coprecipitation method: and (3) simultaneously adding the color pigment and the silver-plated aluminum powder coated with silicon dioxide obtained in the step (S2) into a solvent, dropwise adding 1-1.5mol/L alkali solution until the pH value is 7.5-8, then adding a surfactant, continuously stirring for 1-2h, after the reaction is finished, centrifugally collecting precipitates, respectively washing the precipitates with distilled water and ethanol for 2-3 times, drying the obtained product at 100-120 ℃ for 1.5-2h, and then cooling to room temperature to obtain the low-emissivity color composite pigment.
In a preferred embodiment, the magnetron sputtering parameters in S1 are: background pressure: 3*10 -4 -4*10 -4 Pa; the sputtering parameters are as follows: the purity of Ar gas is 99.9 percent, the flow value of Ar gas is 35-40sccm, the deposition pressure is 0.2-0.4Pa, the deposition temperature is 50-60 ℃, the target working current is 0.3-0.6A, and the target working voltage is 450-500V.
In a preferred embodiment, the thickness of the silver layer of the magnetron sputtering silver plating in S1 is 5-80nm.
In a preferred embodiment, the step of coating the silver layer in S2 by a sol-gel method comprises: weighing silver-plated aluminum powder, placing the silver-plated aluminum powder into isopropanol, pouring the silver-plated aluminum powder into a three-neck flask after ultrasonic dispersion, placing the three-neck flask into a constant-temperature water bath at 40-45 ℃, stirring, measuring a certain amount of tetraethoxysilane, adding the tetraethoxysilane into the flask, measuring corresponding amounts of ammonia water and distilled water respectively, uniformly mixing, placing the mixture into a dropping funnel, connecting the dropping funnel with the three-neck flask, adjusting the dropping speed of the dropping funnel to be 1-2 drops/second, continuously stirring, controlling the concentration of tetraethoxysilane to be 0.05-0.1 mol/L, controlling the water-silicon ratio R to be 16, controlling the concentration of catalyst ammonia water to be 0.02-0.2 mol/L, centrifugally washing after the reaction is finished, and drying to obtain the silver-plated aluminum powder coated by silicon dioxide.
In a preferred embodiment, the surfactant in S3 is one or more of polyether, polyglycerol, sulfate, carboxylate, phosphonate and phosphate.
The technical scheme of the invention has the beneficial effects that:
the composite pigment prepared by the scheme has good compatibility and stealth performance in visible light and infrared bands. The emissivity is regulated and controlled through the thickness of the silver coating on the surface of the aluminum powder, the infrared stealth requirement is met, and compared with the method of using pure silver powder as a substrate, the cost of silver coating of the aluminum powder is lower. The silver layer is protected by the silicon dioxide, so that oxidation is prevented, the weather resistance is improved, and the hydrophilicity of the silicon dioxide layer and pits on the surface are beneficial to compounding of pigments, so that the invisible light is realized.
Drawings
FIG. 1 is the emissivity of different silver plating thicknesses at a wavelength band of 2-14 μm according to the present invention;
FIG. 2 shows the effect of the low emissivity color composite pigment of the present invention after spraying;
FIG. 3 is a plot of the visible/NIR reflectance of SE3948 according to the present invention;
FIG. 4 is a graph of visible/near infrared spectral reflectance for MG1151 of the present invention;
FIG. 5 is a DG0648 visible/near infrared spectral reflectance curve of the present invention;
FIG. 6 is a chart of visible/near infrared spectral reflectance curves for YG1560 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments. The embodiments of the present invention have been presented for purposes of illustration and description, and are not intended to be exhaustive or limited to the invention in the form disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art. The embodiment was chosen and described in order to best explain the principles of the invention and the practical application, and to enable others of ordinary skill in the art to understand the invention for various embodiments with various modifications as are suited to the particular use contemplated.
The technical scheme of the invention provides a preparation method of a low-emissivity color composite pigment, which comprises the following steps: s1, magnetron sputtering silver plating: the scaly aluminum powder with the grain diameter of 60-70 microns is spread on the sputtering base material; putting the sputtering base material into a magnetron sputtering anode cover, adjusting sputtering parameters, performing sputtering reaction for 5-40min, cooling to room temperature after sputtering is finished, and taking out; s2: coating a silver layer by a sol-gel method: through the hydrolysis-polycondensation reaction of ethyl orthosilicate, hydrated silicon dioxide precipitate is generated and deposited on the surface of the silver-plated aluminum powder, and the silver-plated aluminum powder coated with silicon dioxide is obtained. S3: coloring by a coprecipitation method.
Example 1
The preparation steps of S1-S3 are adopted, and specific implementation parameters are defined. The magnetron sputtering parameters in the S1 are as follows: background pressure: 3*10 -4 Pa; the sputtering parameters are as follows: the purity of Ar gas is 99.9 percent, the flow value of the Ar gas is 35sccm, the deposition pressure is 0.2Pa, the deposition temperature is 50 ℃, the target working current is 0.3A, and the target working voltage is 450V. The thickness of the silver layer of the magnetron sputtering silver plating in the S1 is 5nm;
the step of coating the silver layer by the sol-gel method in the S2 is as follows: weighing silver-plated aluminum powder, placing the silver-plated aluminum powder into isopropanol, pouring the silver-plated aluminum powder into a three-neck flask after ultrasonic dispersion, placing the three-neck flask into a constant-temperature water bath tank at 40 ℃ for stirring, measuring a certain amount of tetraethoxysilane, adding the tetraethoxysilane into the flask, measuring corresponding amounts of ammonia water and distilled water respectively, uniformly mixing, placing the mixture into a dropping funnel, connecting the dropping funnel with the three-neck flask, adjusting the dropping speed of the dropping funnel to be 1 drop/second, continuously stirring, controlling the concentration of tetraethoxysilane to be 0.05mol/L, controlling the water-silicon ratio R to be 16, controlling the concentration of catalyst ammonia water to be 0.02mol/L, centrifugally washing after the reaction is finished, and drying to obtain the silver-plated aluminum powder coated by silicon dioxide.
The coloring step of the coprecipitation method in the S3 comprises the following steps: and (3) simultaneously adding the color pigment and the silver-plated aluminum powder coated with silicon dioxide obtained in the step (S2) into a solvent, dropwise adding 1/L of alkali solution until the pH value is 7.5, then adding a surfactant, continuously stirring for 1h, centrifugally collecting precipitates after the reaction is finished, respectively washing the precipitates for 2 times by using distilled water and ethanol, drying the obtained product at 100 ℃ for 1.5h, and cooling to room temperature to obtain the low-emissivity color composite pigment. The surfactant in S3 is polyglycerol.
Example 2
The magnetron sputtering parameters in the S1 are as follows: background pressure: 4*10 -4 Pa; the sputtering parameters are as follows: the purity of Ar gas is 99.9 percent, the flow value of the Ar gas is 40sccm, the deposition pressure is 0.4Pa, the deposition temperature is 60 ℃, the target working current is 0.6A, and the target working voltage is 500V. The thickness of the silver layer of the magnetron sputtering silver plating in the S1 is 10nm.
The step of coating the silver layer by the sol-gel method in the S2 is as follows: weighing silver-plated aluminum powder, placing the silver-plated aluminum powder into isopropanol, pouring the silver-plated aluminum powder into a three-neck flask after ultrasonic dispersion, placing the three-neck flask into a constant-temperature water bath tank at 45 ℃ for stirring, measuring a certain amount of tetraethoxysilane, adding the tetraethoxysilane into the flask, measuring corresponding amounts of ammonia water and distilled water respectively, uniformly mixing, placing the mixture into a dropping funnel, connecting the dropping funnel with the three-neck flask, adjusting the dropping speed of the dropping funnel to be 2 drops/second, continuously stirring, controlling the concentration of the tetraethoxysilane to be 0.1mol/L, controlling the water-silicon ratio R to be 16, controlling the concentration of catalyst ammonia water to be 0.2mol/L, centrifugally washing after the reaction is finished, and drying to obtain the silver-plated aluminum powder coated by silicon dioxide.
The coloring step of the coprecipitation method in the S3 comprises the following steps: and (3) simultaneously adding the color pigment and the silver-plated aluminum powder coated with silicon dioxide obtained in the step (S2) into a solvent, dropwise adding 1-1.5mol/L alkali solution until the pH value is 8, then adding a surfactant, continuously stirring for 1-2h, after the reaction is finished, centrifugally collecting precipitates, washing the precipitates for 2-3 times respectively by using distilled water and ethanol, drying the obtained product at 100-120 ℃ for 1.5-2h, and cooling to room temperature to obtain the low-emissivity color composite pigment. The surfactant in S3 is polyether-based.
Example 3
The magnetron sputtering parameters in the S1 are as follows: background pressure: 3.5*10 -4 Pa; the sputtering parameters are as follows: the purity of Ar gas is 99.9 percent, the flow value of the Ar gas is 37sccm, the deposition pressure is 0.3Pa, the deposition temperature is 55 ℃, the target working current is 0.4A, and the target working voltage is 480V. The thickness of the silver layer of the magnetron sputtering silver plating in the S1 is 20nm.
The step of coating the silver layer by the sol-gel method in the S2 is as follows: weighing silver-plated aluminum powder, placing the silver-plated aluminum powder into isopropanol, pouring the silver-plated aluminum powder into a three-neck flask after ultrasonic dispersion, placing the three-neck flask into a constant-temperature water bath tank at 45 ℃, stirring, measuring a certain amount of tetraethoxysilane, adding the tetraethoxysilane into the flask, measuring corresponding amounts of ammonia water and distilled water respectively, uniformly mixing, placing the mixture into a dropping funnel, connecting the dropping funnel with the three-neck flask, adjusting the dropping speed of the dropping funnel to be 1-2 drops/second, continuously stirring, controlling the concentration of the tetraethoxysilane to be 0.07mol/L, controlling the water-silicon ratio R to be 16, controlling the concentration of catalyst ammonia water to be 0.1mol/L, centrifugally washing after the reaction is finished, and drying to obtain the silver-plated aluminum powder coated by silicon dioxide.
The coloring method by the coprecipitation method in the S3 comprises the following steps: and (3) simultaneously adding the color pigment and the silver-plated aluminum powder coated with silicon dioxide obtained in the step (S2) into a solvent, dropwise adding 1.2mol/L alkali solution until the pH value is 8, then adding a surfactant, continuously stirring for 1.5h, after the reaction is finished, centrifugally collecting precipitates, respectively washing the precipitates with distilled water and ethanol for 2 times, drying the obtained product at the temperature of 110 ℃ for 1.5h, and then cooling to the room temperature to obtain the low-emissivity color composite pigment. The surfactant in S3 is a mixture of phosphonate and phosphate.
Example 4
The magnetron sputtering parameters in the S1 are as follows: background pressure: 3.8*10 -4 Pa; the sputtering parameters are as follows: the purity of Ar gas is 99.9 percent, the flow value of the Ar gas is 40sccm, the deposition pressure is 0.2Pa, the deposition temperature is 60 ℃, the target working current is 0.6A, and the target working voltage is 450V. The thickness of the silver layer of the magnetron sputtering silver plating in the S1 is 50nm.
The step of coating the silver layer by the sol-gel method in the S2 is as follows: weighing silver-plated aluminum powder, placing the silver-plated aluminum powder into isopropanol, pouring the silver-plated aluminum powder into a three-neck flask after ultrasonic dispersion, placing the three-neck flask into a constant-temperature water bath tank at 42 ℃, stirring, measuring a certain amount of tetraethoxysilane, adding the tetraethoxysilane into the flask, measuring corresponding amounts of ammonia water and distilled water respectively, uniformly mixing, placing the mixture into a dropping funnel, connecting the dropping funnel with the three-neck flask, adjusting the dropping speed of the dropping funnel to be 1 drop/second, continuously stirring, controlling the concentration of tetraethoxysilane to be 0.07mol/L, controlling the water-silicon ratio R to be 16, controlling the concentration of catalyst ammonia water to be 0.12mol/L, centrifugally washing after the reaction is finished, and drying to obtain the silver-plated aluminum powder coated by silicon dioxide.
The coloring step of the coprecipitation method in the S3 comprises the following steps: and (3) simultaneously adding the color pigment and the silver-plated aluminum powder coated by the silicon dioxide obtained in the step (S2) into a solvent, dropwise adding 1.3mol/L alkali solution until the pH value is 8, then adding a surfactant, continuously stirring for 2h, after the reaction is finished, centrifugally collecting precipitates, respectively washing the precipitates for 3 times by using distilled water and ethanol, drying the obtained product at 100 ℃ for 2h, and cooling to room temperature to obtain the low-emissivity color composite pigment. The surfactant in S3 is a mixture based on sulfate and carboxylate.
Example 5
The magnetron sputtering parameters in the S1 are as follows: background pressure: 4*10 -4 Pa; the sputtering parameters are as follows: the purity of Ar gas is 99.9 percent, the flow value of Ar gas is 38sccm, the deposition pressure is 0.4Pa, the deposition temperature is 55 ℃, and the target working current isFlow 0.45A, target operating voltage 460V. The thickness of the silver layer of the magnetron sputtering silver plating in the S1 is 80nm.
The step of coating the silver layer by the sol-gel method in the S2 is as follows: weighing silver-plated aluminum powder, placing the silver-plated aluminum powder into isopropanol, pouring the silver-plated aluminum powder into a three-neck flask after ultrasonic dispersion, placing the three-neck flask into a 43 ℃ constant-temperature water bath for stirring, measuring a certain amount of tetraethoxysilane, adding the tetraethoxysilane into the flask, measuring corresponding amounts of ammonia water and distilled water respectively, uniformly mixing, placing the mixture into a dropping funnel, connecting the dropping funnel with the three-neck flask, adjusting the dropping speed of the dropping funnel to be 1-2 drops/second, continuously stirring, controlling the concentration of tetraethoxysilane to be 0.09mol/L, the water-silicon ratio R to be 16, and the concentration of catalyst ammonia water to be 0.08mol/L, centrifugally washing after the reaction is finished, and drying to obtain the silver-plated aluminum powder coated by silicon dioxide.
The coloring method by the coprecipitation method in the S3 comprises the following steps: and (3) simultaneously adding the color pigment and the silver-plated aluminum powder coated with silicon dioxide obtained in the step (S2) into a solvent, dropwise adding 1mol/L alkali solution until the pH value is 7.5, then adding a surfactant, continuously stirring for 2h, after the reaction is finished, centrifugally collecting precipitates, respectively washing the precipitates for 3 times by using distilled water and ethanol, drying the obtained product at the temperature of 110 ℃ for 1.5h, and cooling to the room temperature to obtain the low-emissivity color composite pigment. The surfactant in S3 is a mixture based on polyether and polyglycerol.
(1) By reflection detection, emissivity of 5, 10, 20, 50 and 80um silver plating thickness in examples 1 to 5 at 2 to 14 μm wavelength band is measured, and infrared emissivity curve is plotted as shown in fig. 1, and average emissivity at 8 to 14 μm wavelength band at different thickness is calculated as shown in table 1 below:
TABLE 1 emissivity for different coating thicknesses
As shown in Table 1, the test shows that the average emissivity of the infrared band (wavelength 8-14 μm) is as low as 0.1, and can be controlled between 0.1 and 0.5 according to the requirement. The requirement of low emissivity of the infrared stealth coating is met.
(2) SE3948, YG1560, MG1151 and DG0648 are prepared and respectively sprayed on a test substrate by four national military standard colors prepared in examples 1 to 4, the spraying thickness is 20 to 40 μm, the spraying result is shown in figure 2 (YG 1560, MG1151, DG0648 and SE3948 are sequentially arranged from left to right), the color index requirement required by the visible light stealth field is met, the spectrum detection data (the wavelength is 0.3 to 1.4 μm) is shown in figures 3 to 6, the reflectivity is 0.05 to 0.6, and the requirement for hiding under light is met.
It should be apparent that the described embodiments are only some of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by one of ordinary skill in the art and related arts based on the embodiments of the present invention without any creative effort, shall fall within the protection scope of the present invention. Structures, devices, and methods of operation not specifically described or illustrated herein are generally practiced in the art without specific recitation or limitation.
Claims (5)
1. The preparation method of the low-emissivity color composite pigment is characterized by comprising the following steps of:
s1, magnetron sputtering silver plating: the scaly aluminum powder with the grain diameter of 60-70 microns is spread on the sputtering base material; putting the sputtering base material into a magnetron sputtering anode cover, adjusting sputtering parameters, performing sputtering reaction for 5-40min, cooling to room temperature after sputtering is finished, and taking out;
s2: coating a silver layer by a sol-gel method: through the hydrolysis-polycondensation reaction of ethyl orthosilicate, hydrated silicon dioxide precipitate is generated and deposited on the surface of the silver-plated aluminum powder, and the silver-plated aluminum powder coated with silicon dioxide is obtained;
s3: coloring by a coprecipitation method: and (3) simultaneously adding the color pigment and the silver-plated aluminum powder coated by the silicon dioxide obtained in the step (S2) into a solvent, dropwise adding 1-1.5mol/L of alkali solution until the pH value is 7.5-8, then adding a surfactant, continuously stirring for 1-2h, centrifugally collecting precipitates after the reaction is finished, respectively washing the precipitates for 2-3 times by using distilled water and ethanol, drying the obtained product at 100-120 ℃ for 1.5-2h, and cooling to room temperature to obtain the low-emissivity color composite pigment.
2. The preparation method of the low-emissivity color composite pigment according to claim 1, wherein the magnetron sputtering parameters in S1 are as follows: background pressure: 3*10 -4 -4*10 -4 Pa; the sputtering parameters are as follows: the purity of Ar gas is 99.9 percent, the flow value of Ar gas is 35-40sccm, the deposition pressure is 0.2-0.4Pa, the deposition temperature is 50-60 ℃, the target working current is 0.3-0.6A, and the target working voltage is 450-500V.
3. The method for preparing the low-emissivity color composite pigment of claim 1, wherein the method comprises the following steps: and in S1, the thickness of the silver layer plated with silver by magnetron sputtering is 5-80nm.
4. The preparation method of the low-emissivity colored composite pigment according to claim 1, wherein the step of coating the silver layer by a sol-gel method in S2 comprises: weighing silver-plated aluminum powder, placing the silver-plated aluminum powder into isopropanol, pouring the silver-plated aluminum powder into a three-neck flask after ultrasonic dispersion, placing the three-neck flask into a constant-temperature water bath at 40-45 ℃, stirring, measuring a certain amount of tetraethoxysilane, adding the tetraethoxysilane into the flask, measuring corresponding amounts of ammonia water and distilled water respectively, uniformly mixing, placing the mixture into a dropping funnel, connecting the dropping funnel with the three-neck flask, adjusting the dropping speed of the dropping funnel to be 1-2 drops/second, continuously stirring, controlling the concentration of the tetraethoxysilane to be 0.05-0.1 mol/L, controlling the water-silicon ratio R to be 16, controlling the concentration of catalyst ammonia water to be 0.02-0.2 mol/L, centrifugally washing after the reaction is finished, and drying to obtain the silicon dioxide coated silver-plated aluminum powder.
5. The method for preparing a low-emissivity color composite pigment according to claim 1, wherein the surfactant in S3 is one or more selected from polyether, polyglycerol, sulfate, carboxylate, phosphonate and phosphate.
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