CN112675822B - Preparation method of high-absorption high-emissivity ultra-black molecular adsorption coating - Google Patents
Preparation method of high-absorption high-emissivity ultra-black molecular adsorption coating Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-absorption high-emissivity super-black molecular adsorption coating, and belongs to the technical field of super-black materials. The invention solves the problems of large weight and size, inflexible installation position and insufficient absorption area of the existing molecular pollution absorber taking the zeolite molecular sieve as a functional material. The invention takes carbon black and zeolite powder with large specific surface area as cores, takes functional powder with an ultrathin oxide film layer prepared by utilizing an atomic layer deposition technology as a shell as a filler, mixes the functional powder with a low-volatility resin material, and obtains a molecular adsorption coating after coating and curing. The average solar absorptivity of the coating is 95%, the hemispherical emissivity is 91%, the surface layer has the performance of eliminating stray light, and the adsorption capacity of the coating on organic gases (VOCs) such as phthalic acid ester, organic siloxane, n-butene and the like is more than or equal to 17.58mg g‑1. The coating has excellent space environment adaptability and can meet the application requirements of spacecraft and satellite imaging systems.
Description
Technical Field
The invention relates to a preparation method of a high-absorption high-emissivity super-black molecular adsorption coating, belonging to the technical field of super-black materials.
Background
With the development of spacecraft and satellite imaging systems toward high performance, high reliability and long service life, rigorous requirements on the precision and sensitivity of effective loads are provided. When the spacecraft runs in a high vacuum environment, organic small molecule pollutants released by materials such as used adhesives, plasticizers and the like can be condensed and deposited on the surface of each sensitive element, especially sensitive optical elements, so that the full exertion of the functions of the sensitive elements is influenced, and even the sensitive optical elements fail. Therefore, great attention is paid to on-orbit molecular contamination prevention and control, and corresponding measures and measures are urgently needed to reduce the influence of the on-orbit molecular contamination on sensitive elements.
At present, the porous material is used for carrying out adsorption control on organic molecular pollutants, and the method is an effective method which is simple, convenient and low in cost. The zeolite molecular sieve contains abundant micropores, has large specific surface area, selective adsorption, contains more acid sites, has certain catalytic activity, and is widely applied to the field of on-orbit pollutant control of spacecrafts. However, the existing molecular pollution adsorber using zeolite molecular sieve as functional material has the disadvantages of large weight and size, inflexible installation position and not wide enough absorption area, and can not well meet the design requirements of spacecraft. The molecular pollution adsorption coating can collect pollutants in real time in space, reduces the possibility of on-orbit pollution, and then improves the performance and the service life of the spacecraft, so the preparation method of the molecular pollution adsorption coating for the spacecraft has important significance.
Disclosure of Invention
The invention provides a preparation method of a high-absorption high-emissivity ultra-black molecular adsorption coating, aiming at solving the problems of large weight and size, inflexible installation position and insufficient absorption area of the existing molecular pollution adsorber taking a zeolite molecular sieve as a functional material.
A preparation method of a high-absorption high-emissivity ultra-black molecular adsorption coating comprises the following operation steps:
step 1, pretreating carbon black and zeolite molecular sieve powder;
step 3, carrying out periodic deposition growth of a metal oxide atomic layer on the surface of the mixed powder subjected to ball milling treatment to obtain ultra-black powder with a core-shell structure, wherein the thickness of a film layer of the metal oxide atomic layer is 30-60nm, and the metal oxide film layer is of a discrete island-shaped distribution structure;
and 5, carrying out ultrasonic treatment on the spraying diluent obtained in the step 4, then spraying the spraying diluent on the surface of the base material, and placing the base material in an oven for curing to obtain the molecular adsorption coating.
Further, the pretreatment operation process of the carbon black comprises the following steps: 100-150ml of concentrated sulfuric acid with the concentration of 95% -98% and 30-50ml of concentrated nitric acid with the concentration of 65% -68% are mixed, carbon black with the particle size of 30-50nm is added, then, the mixture is magnetically stirred, condensed and refluxed for 2-5 hours at the temperature of 70 ℃, filtered, and the obtained precipitate is washed by deionized water until the pH value is 7, and dried for later use.
Further, the pretreatment operation process of the zeolite molecular sieve powder comprises the following steps: putting zeolite molecular sieve powder into a tubular furnace for heating, wherein the heating rate is as follows: heating to 200-; the zeolite molecular sieve powder is one or more of X type, A type and ZSM type which are mixed according to any proportion; the pore diameter of the micropore and/or mesoporous pore passage of the zeolite molecular sieve powder is less than 20 nm.
Further, the zeolite molecular sieve powder is 13X type zeolite molecular sieve powder.
Further, the specific operation process of the ball milling treatment in the step 2 is as follows: mixing the pretreated carbon black and zeolite molecular sieve powder, and then mixing the mixed powder with ZrO2Putting the grinding balls into a ball milling tank, removing air in the ball milling tank by using argon with the purity of 99.99 percent, and performing ball milling for 3-5h under the condition of the rotation speed of 400-800 rpm;
the mass ratio of the carbon black to the zeolite molecular sieve powder in the mixed powder is 1: 1-2.
Further, the specific operation process of the periodic deposition growth of the atomic layer in step 3 is as follows:
placing the mixed powder after ball milling treatment in a deposition cavity of an atomic layer deposition instrument, and pumping the deposition cavity to 4 multiplied by 10-3-6×10-3Torr, introducing carrier gas to the chamber with pressure of 0.1-0.2Torr, and setting the temperature in the deposition chamber to beRepeating 170-300 atomic layer deposition growth cycles at the temperature of 130-;
the specific operation process of each atomic layer deposition growth cycle is as follows:
(1) injecting metal source into the sinking cavity in a pulse mode for a pulse time t10.01-0.03 s;
(2) reaction is carried out by cutting off the air inlet valve and the air outlet valve, and the reaction time t2Is 1-5 s;
(3) opening the air inlet valve and the exhaust valve, purging by using nitrogen, and purging for time t3Is 30-60 s;
(4) injecting an oxygen source into the reaction cavity in a pulse mode, wherein the temperature of the oxygen source is room temperature, and the pulse time t40.01-0.03 s;
(5) reaction is carried out by cutting off the air inlet valve and the air outlet valve, and the reaction time t5Is 1-5 s;
(6) opening the air inlet valve and the exhaust valve, purging by using nitrogen, and purging for time t6Is 30-60 s;
the metal source is one or two of diethyl zinc and trimethylaluminum which are mixed in any proportion;
the oxygen source is deionized water or ozone.
Further, the specific operation process of step 4 is as follows: adding 100-200g of resin material into a liquid storage tank of an ultrasonic-assisted thermal spraying device, heating the liquid storage tank by a heating ring, controlling the temperature of the liquid storage tank to be 70-90 ℃, and melting the resin in the liquid storage tank to be liquid; and (3) sequentially adding an accelerator, a coupling agent and the ultra-black powder obtained in the step (3) into a liquid storage tank, starting a stirrer and uniformly stirring to obtain a spraying diluent.
Further, the resin material is one or more of cyanate ester resin, potassium silicate resin and silicone gel resin which are mixed in any proportion.
Still further, the accelerator is aluminum acetylacetonate.
Further, the coupling agent is KH560 silane coupling agent.
Further, the specific operation process of step 5 is as follows: and (3) carrying out ultrasonic treatment on the spraying diluent obtained in the step (4) for 10-20min under the condition that the ultrasonic power is 1000-2000W, then spraying the spraying diluent on the surface of the base material, wherein the diameter of a spray nozzle is 1-3mm, the liquid feeding pressure is 0.6-0.8Mpa, the moving speed of a spray gun is 50-100cm/s, the spraying distance is 10-20cm, after the spraying is finished, placing the spraying diluent in a vacuum drying box, preserving heat for 5-6h at 50 ℃, then raising the temperature to 100 ℃, preserving heat for 1-3h, and finally raising the temperature to 130 ℃ and preserving heat for 1-3 h.
Further, the base material is an aluminum plate, a magnesium plate, a tantalum plate or a high aluminum silicon alloy plate.
The invention has the following beneficial effects: the invention takes carbon black and zeolite powder with large specific surface area as cores, takes functional powder with an ultrathin oxide film layer prepared by utilizing an atomic layer deposition technology as a shell as a filler, mixes the functional powder with a low-volatility resin material, and obtains a molecular adsorption coating after coating and curing. The average solar absorptivity of the coating is 95%, the hemispherical emissivity is 91%, the surface layer has the performance of eliminating stray light, and the adsorption capacity of the coating on organic gases (VOCs) such as phthalic acid ester, organic siloxane, n-butene and the like is more than or equal to 17.58mg g-1. The coating has excellent space environment adaptability and can meet the application requirements of spacecraft and satellite imaging systems. In addition, the present application has the following advantages:
(1) the carbon black has extremely high solar absorptivity and irradiation resistance, and can effectively eliminate space stray light;
(2) the method has the advantages that the stable chemical bonding is formed between the oxide film layer prepared by the atomic layer deposition technology and the surface of the carbon black, so that the structural stability and the dispersibility of the functional powder material can be improved, and the problem of low light absorption performance caused by powder agglomeration is effectively solved;
(3) the high-energy dispersion diluent treated by the ultrasonic-assisted thermal spraying process is sprayed on the surface of a base material, so that a surface layer with rich pores can be formed, a large number of light trap holes are generated, and the absorption capacity of the coating on visible light and infrared light is improved.
Drawings
FIG. 1 is a spectrum of solar absorptance of a molecular adsorption coating prepared in accordance with embodiment 1;
FIG. 2 is a graph of hemispherical emissivity of the molecular adsorption coating prepared in accordance with embodiment 1;
FIG. 3 is a diagram of the molecular adsorption coating prepared in embodiment 1 before the cold-hot alternation test;
fig. 4 is a diagram showing the molecular adsorption coating prepared in embodiment 1 after a hot-cold alternation test.
Detailed Description
The experimental procedures used in the following examples are conventional unless otherwise specified. The materials, reagents, methods and apparatus used, unless otherwise specified, are conventional in the art and are commercially available to those skilled in the art.
Embodiment mode 1:
(1) acidifying carbon black with particle size of 30-50 nm. The specific operation process is as follows: adding 80mL of concentrated sulfuric acid with the concentration of 97% and 40mL of concentrated nitric acid with the concentration of 67% into carbon black, carrying out magnetic stirring, condensing, refluxing and reacting for 3h at 70 ℃, washing with deionized water until the pH value is about 7, and drying for later use.
The acidification treatment can lead the oxygen-containing groups on the surface of the carbon black to be dissociated, for example, -COOH groups to be dissociated into-COO-, thereby increasing the electric potential of a double electric layer and increasing the electrostatic repulsion, and simultaneously, the surface of the carbon black is surrounded by a layer of volume due to the acid groups, thus playing a certain steric hindrance role. Meanwhile, the surface of the carbon black powder subjected to acidification treatment becomes fluffy, so that the diffuse reflection and scattering effects of the optical fiber on the surface can be increased, and the light absorption performance of the optical fiber is improved.
(2) The zeolite molecular sieve powder with the aperture of 13X type, micropore and/or mesopore pore canal less than 20nm is heated and dried to discharge the redundant water vapor in the zeolite, and the rapid air extraction in the atomic layer deposition process is convenient. The specific operation process is as follows: putting zeolite molecular sieve powder into a tube furnace for heating, heating to 200 ℃ within 0.5h, vacuumizing to-0.1 MPa, preserving heat for 2h, and naturally cooling to room temperature.
(3) Mixing the treated carbon black, zeolite molecular sieve powder and certain amount of ZrO2Grinding balls are put into the ball milling tank together, and the grinding balls are covered by the cover and then reserved on the tank coverAnd (3) filling argon with the purity of 99.99% into the two air filling holes by adopting proper airflow for 10min to completely exhaust air, and finally fixing the ball milling tank in a ball mill, wherein the rotating speed of the ball mill is set to be 600rpm, and the ball milling time is set to be 4 h.
(4) Placing the mixed powder after ball milling treatment in a deposition cavity of an atomic layer deposition instrument, and pumping the deposition cavity to 5 × 10-3And Torr, then introducing carrier gas to the cavity with the pressure of 0.15Torr and the temperature in the deposition cavity of 150 ℃, and repeatedly executing 230 atomic layer deposition growth cycles to perform the periodic deposition growth of the metal oxide atomic layer on the surface of the powder.
The specific operation process of each atomic layer deposition growth cycle is as follows: 1) injecting metal source (diethyl zinc) into the sinking cavity in a pulse mode, wherein the pulse time t10.015 s; 2) the reaction is carried out by cutting off the air inlet valve and the exhaust valve, and the reaction time t2Is 5 s; 3) opening the air inlet valve and the air outlet valve, purging by using nitrogen, and purging for time t3Is 60 s; 4) injecting oxygen source (water) into the reaction cavity in a pulse mode, wherein the oxygen source temperature is room temperature, and the pulse time t4Is 0.02 s; 5) the reaction is carried out by cutting off the air inlet valve and the exhaust valve, and the reaction time t55s, 6) opening the air inlet valve and the air outlet valve, and purging by using nitrogen for a purging time t6For 60s, one deposition growth cycle was completed.
The thickness of the obtained metal oxide atomic layer film is 30nm, and the film is in a discrete island distribution structure.
(5) Adding 150g of low-volatility cyanate ester resin into a liquid storage tank of an ultrasonic-assisted thermal spraying device, heating the liquid storage tank by a heating ring, controlling the temperature of the liquid storage tank to be 80 ℃, and melting the resin in the liquid storage tank to form a liquid state; and then sequentially adding an accelerator aluminum acetylacetonate, a coupling agent KH560 silane coupling agent and the ultra-black powder obtained in the step 4 into a liquid storage tank, starting a stirrer to stir, and uniformly mixing the accelerator and the molten resin to obtain a spraying diluent. Wherein the mass ratio of the cyanate ester resin, the aluminum acetylacetonate, the KH560 silane coupling agent and the ultra-black powder is 10:1: 0.5.
Then starting an ultrasonic generator, adjusting the ultrasonic power to 1500W, performing ultrasonic action for 15min, and pausing for 5min, removing bubbles of a molten polymer system by utilizing the vibration characteristic of ultrasonic, spraying the spraying diluent on the surface of the high-aluminum-silicon alloy base material, wherein the spraying conditions are as follows: the diameter of the nozzle is 2mm, the liquid feeding pressure is 0.8Mpa, the moving speed of the spray gun is 100cm/s, and the spray distance is 17 cm.
And finally, further curing in an oven, specifically, putting the molecular adsorption coating in a vacuum drying oven, heating to 50 ℃ for 6h, heating to 100 ℃ for 1h, and heating to 130 ℃ for 1h to obtain the high-absorption high-emissivity ultra-black molecular adsorption coating. The curing mode adopts segmented curing to prevent the film layer from cracking.
The solar absorptivity test result of the high-absorption high-emissivity ultra-black molecular adsorption coating obtained by the embodiment is shown in fig. 1, the average absorptivity is 96% calculated in the wavelength range of 200-2500 nm, and the light in the ultraviolet, visible light, infrared and other wave bands is absorbed, so that the coating has good extinction performance.
The emissivity curve of the high-absorption high-emissivity ultra-black molecular adsorption coating obtained by the embodiment is shown in fig. 2, and the average emissivity of the coating is 91% in the wavelength range of 2-16 μm through calculation, which shows that the coating can quickly radiate heat to achieve the temperature control effect.
South Dai 703 silicone rubber is known to release gases such as phthalate, organosiloxane, n-butene, etc. at high temperatures and can be used to simulate steric molecular contaminants. The specific test process is as follows: the molecular adsorption coating material obtained in example 1 and 703 silicone rubber were placed in a space molecular contamination vacuum test system, and the temperature of a heating table was set to 125 ℃. The adsorption experiment is carried out on a heating table, sampling is carried out once every 10min, the sample is placed in a precision balance for ectopic weighing, and the adsorption quantity is obtained by calculating the difference between the front and the back of weighing. The results are shown in the following table:
| adsorption time (min) | Adsorption amount (mg. g)-1) |
| 30 | 13.36294988 |
| 60 | 15.22255986 |
| 90 | 16.08275677 |
| 120 | 16.51632544 |
| 150 | 17.39237754 |
| 180 | 17.58914390 |
As shown in the table above, the molecular adsorption coating has strong adsorption capacity within 3 hours, and the adsorption capacity is 13.3-17.58 mg/g-1. The adsorption is saturated in 3h, and the adsorbability is 17.58mg g-1。
The high-absorption high-emissivity super-black molecular adsorption coating obtained by the embodiment is used for testing the binding force, and the specific test process is as follows: the coating is placed in a vacuum high-low temperature tester to be subjected to a cold and hot alternating test at the temperature of-170-130 ℃, and the comparison between the graph in fig. 3 and the graph in fig. 4 shows that the tested coating does not crack, fall off powder and the like on a base material and still has excellent interface binding force.
Claims (9)
1. A preparation method of a high-absorption high-emissivity ultra-black molecular adsorption coating is characterized by comprising the following operation steps:
step 1, pretreating carbon black and zeolite molecular sieve powder;
step 2, mixing the pretreated carbon black and zeolite molecular sieve powder, and then carrying out ball milling treatment on the obtained mixed powder;
step 3, carrying out periodic deposition growth of a metal oxide atomic layer on the surface of the mixed powder subjected to ball milling treatment to obtain ultra-black powder with a core-shell structure, wherein the thickness of a film layer of the metal oxide atomic layer is 30-60 nm;
step 4, heating the resin to melt the resin into a liquid state, adding an accelerator, a coupling agent and ultra-black powder, and uniformly stirring to obtain a spraying diluent;
step 5, carrying out ultrasonic treatment on the spraying diluent obtained in the step 4, then spraying the spraying diluent on the surface of the base material, and placing the base material in an oven for curing to obtain a molecular adsorption coating;
the pretreatment operation process of the carbon black comprises the following steps: 100-150ml of concentrated sulfuric acid with the concentration of 95-98% and 30-50ml of concentrated nitric acid with the concentration of 65-68% are mixed, carbon black with the particle size of 30-50nm is added, then, the mixture is magnetically stirred, condensed and refluxed for 2-5 hours at the temperature of 70 ℃, filtered, and the obtained precipitate is washed by deionized water until the pH value is 7 and dried for later use.
2. The method for preparing the high-absorption high-emissivity ultra-black molecular adsorption coating according to claim 1, wherein the pretreatment operation process of the zeolite molecular sieve powder comprises: putting zeolite molecular sieve powder into a tubular furnace for heating, wherein the heating rate is as follows: heating to 200-; the zeolite molecular sieve powder is one or more of X type, A type and ZSM type which are mixed according to any proportion; the pore diameter of the micropore and/or mesoporous pore passage of the zeolite molecular sieve powder is less than 20 nm.
3. The method of claim 2, wherein the zeolite molecular sieve powder is 13X zeolite molecular sieve powder.
4. The method for preparing a high absorption high emissivity ultra black molecular adsorption coating according to claim 1, wherein the ball milling process in step 2 comprises the following specific steps: mixing the pretreated carbon black and zeolite molecular sieve powder, and then mixing the mixed powder with ZrO2Putting the grinding balls into a ball milling tank, removing air in the ball milling tank by using argon with the purity of 99.99 percent, and performing ball milling for 3-5h under the condition of the rotation speed of 400-800 rpm;
the mass ratio of the carbon black to the zeolite molecular sieve powder in the mixed powder is 1: 1-2.
5. The method for preparing a high-absorption high-emissivity ultra-black molecular adsorption coating according to claim 1, wherein the specific operation process of the periodic deposition growth of the atomic layer in step 3 comprises:
placing the mixed powder after ball milling treatment in a deposition cavity of an atomic layer deposition instrument, and pumping the deposition cavity to 4 multiplied by 10-3-6×10-3Torr, then introducing carrier gas to the pressure of the cavity body being 0.1-0.2Torr, setting the temperature in the deposition cavity body to be 130-;
the specific operation process of each atomic layer deposition growth cycle is as follows:
(1) injecting metal source into the sinking cavity in a pulse mode for a pulse time t10.01-0.03 s;
(2) reaction is carried out by cutting off the air inlet valve and the air outlet valve, and the reaction time t2Is 1-5 s;
(3) opening the air inlet valve and the exhaust valve, purging by using nitrogen, and purging for time t3Is 30-60 s;
(4) injecting oxygen source into the reaction cavity in a pulse mode, wherein the temperature of the oxygen source is room temperature, and the pulse time t40.01-0.03 s;
(5) reaction is carried out by cutting off the air inlet valve and the air outlet valve, and the reaction time t5Is 1-5 s;
(6) opening the inlet and outlet valves to use nitrogenPurging is carried out for a time t6Is 30-60 s;
the metal source is one or two of diethyl zinc and trimethylaluminum which are mixed in any proportion;
the oxygen source is deionized water or ozone.
6. The method for preparing the high-absorption high-emissivity ultra-black molecular adsorption coating according to claim 1, wherein the specific operation process of the step 4 is as follows:
adding 100-200g of resin material into a liquid storage tank of an ultrasonic-assisted thermal spraying device, heating the liquid storage tank by a heating ring, controlling the temperature of the liquid storage tank to be 70-90 ℃, and melting the resin in the liquid storage tank to be liquid; and (3) sequentially adding an accelerator, a coupling agent and the ultra-black powder obtained in the step (3) into a liquid storage tank, starting a stirrer and uniformly stirring to obtain a spraying diluent.
7. The method for preparing a high absorption high emissivity ultra black molecular adsorption coating according to claim 6, wherein the resin material is one or more of cyanate ester resin, potassium silicate resin, silicone gel resin mixed in any proportion; the accelerant is aluminum acetylacetonate; the coupling agent is KH560 silane coupling agent.
8. The method for preparing the high-absorption high-emissivity ultra-black molecular adsorption coating according to claim 1, wherein the specific operation process of the step 5 is as follows:
and (3) carrying out ultrasonic treatment on the spraying diluent obtained in the step (4) for 10-20min under the condition that the ultrasonic power is 1000-2000W, then spraying the spraying diluent on the surface of the base material, wherein the diameter of a spray nozzle is 1-3mm, the liquid feeding pressure is 0.6-0.8Mpa, the moving speed of a spray gun is 50-100cm/s, the spraying distance is 10-20cm, after the spraying is finished, placing the spraying diluent in a vacuum drying box, preserving heat for 5-6h at 50 ℃, then raising the temperature to 100 ℃, preserving heat for 1-3h, and finally raising the temperature to 130 ℃ and preserving heat for 1-3 h.
9. The method for preparing a high absorption high emissivity ultra black molecular adsorption coating according to claim 8, wherein the substrate material is aluminum plate, magnesium plate, tantalum plate or high aluminum silicon alloy plate.
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Inventor after: Li Yang Inventor after: Zhou Yan Inventor after: Lu Songtao Inventor after: Hong Yang Inventor after: Wu Xiaohong Inventor after: Qin Wei Inventor before: Li Yang Inventor before: Lu Songtao Inventor before: Hong Yang Inventor before: Wu Xiaohong Inventor before: Qin Wei |