CN115895360B - High-absorption stray light-eliminating coating paint with wave band of 400-1100 nm and preparation and application thereof - Google Patents
High-absorption stray light-eliminating coating paint with wave band of 400-1100 nm and preparation and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of surface engineering, and particularly relates to a 400-1100 nm-band high-absorption stray light-eliminating coating paint, and preparation and application thereof. The coating paint comprises a bottom paint and a surface paint; the primer comprises water, modified carbon aerogel and modified diatomite; the particle size of the modified diatomite is 6-12 mu m, and the pore diameter is 400-800 nm; the surface paint comprises water, an organic solvent, modified carbon aerogel and modified diatomite; the particle size of the modified diatomite is 6-12 mu m, and the pore diameter is 400-800 nm. The invention develops a diatomite aperture structure-based 400-1100 nm band high-absorption stray light eliminating coating paint. Aiming at the high-absorption stray light eliminating requirement of a spectrum band of 400-1100 nm, the coating combines diatomite with specific particle size and aperture size under the cooperation of a rough interface structure created by mixing solvents with different volatilization rates on the basis of the original high-light absorption carbon aerogel filler, so that a compact special structure capable of absorbing light is formed on the surface of the coating, and low reflection and high absorptivity are realized.
Description
Technical Field
The invention belongs to the technical field of surface engineering, and particularly relates to a 400-1100 nm-band high-absorption stray light-eliminating coating paint, and preparation and application thereof.
Background
In an optical system on a spacecraft, stray light refers to background radiation noise formed on a system detector by light rays that reach a non-imaging field of view region of the system image plane. Stray light can reduce the signal-to-noise ratio of a target, so that the imaging of an observed target is blurred, the contrast is reduced, the detection or recognition capability of the whole system is weakened, and the detection result is distorted. With the progress of space optical technology, optical devices of large aperture, long focal length, high sensitivity and the like are gradually increased, and the requirements on imaging quality are higher and higher for space cameras for earth observation satellites, telescopes for space remote sensing satellites, star sensors used for attitude control of each satellite and the like, and the devices are generally concentrated in a 400-1100 nm spectrum band, so that the stray light eliminating capability in the band also provides higher requirements.
Patent CN103276377B mentions that a black coating with reflectivity lower than 1.4% in the wavelength range of 400-2000 nm is deposited on the surface of the material by an electroless plating method, but the electroless plating technology adopted by the method has high construction difficulty and cannot be repaired secondarily when the paint effect is poor compared with the traditional paint technology. In terms of coating technology, the ultra-black coating components used at home and abroad at present mainly use carbon black, carbon nano tubes, carbon aerogel and the like as black pigments to absorb light, and use resin as a binder. The ultra-black coating prepared by adopting carbon aerosol as pigment in the patent CN110791192A has excellent light absorption performance in the wave band of 400-1100 nm, and the light absorption rate of the coating is more than 0.97 and even can reach 0.99, but in order to ensure the binding force, the surface of the substrate needs to be subjected to sand blasting treatment, complex structural parts which cannot be subjected to sand blasting and the surface of the coated substrate are difficult to implement, and the application range is limited. While the selectivity of the material substrate is improved by adopting the graphene material in the patent CN111393988B, the disclosed light absorptivity of the coating is only between 0.98 and 0.985, and the performance is slightly insufficient. Although the absorption rate of the stray light eliminating coating disclosed in the patent CN113663894A reaches 0.99 in the wave band of 200-2500 nm, in terms of an implementation case, a pure adhesive is adopted as a bottom layer to improve the bonding force between the coating and a substrate, and then the adhesive is adopted to be matched with a high-porosity carbon microsphere filler as a surface layer. It can be seen that the technology of reaching the absorption rate level of 0.99 in the existing 400-1100 nm spectrum band is still in the test stage, and further improvement is still needed from the actual realization of engineering application.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a coating technical method based on simple construction, which utilizes the microstructure characteristics of various fillers and the gradient design of a coating multilayer structure to realize the ultrahigh absorptivity, and simultaneously ensures the engineering application requirements of coating binding force, appearance and the like, and has obvious advantages in the application in the field of space optical remote sensing.
Diatomite is prepared from SiO 2 Porous powder material with the main component, the particle size range of the powder covers the range from nanometer to millimeter, the aperture range covers 50-3000 nm, and the specific surface range is 40-65 m 2 The melting point is 1650-1750 ℃, the refractive index is 1.4-1.46, and the maximum advantage of the material as a matting material compared with white carbon black matting powder is that the particle size and the pore diameter have wide selectivity, and the pore size can be processed and regulated.
The invention discovers that diatomite with the grain diameter of 6-12 mu m and the aperture range of 400-800 nm is used as a matting agent for a high-absorptivity stray light removing coating for the first time, realizes the light absorptivity of 0.993 at the wave band of 400-1100 nm, and has great effect on the capability of reducing the stray light influence and improving the imaging quality of an aerospace optical instrument.
The coating is characterized in that 400-1100 nm high-efficiency extinction performance diatomite powder and carbon aerogel with high absorption capacity are used as fillers to be added into a coating system, the coating system is designed to be a base coat and a top coat, the base coat is used for improving the binding force with a base material, the top coat is used for forming a rough interface structure by utilizing the micro morphology of the fillers and the organic solvents and the different volatilization rates of water to destroy resin film formation, extinction traps are constructed, and the light absorption capacity of the coating material in the 400-1100 nm wave band can be remarkably improved.
The first aspect of the invention provides a high absorption stray light eliminating coating paint with a wave band of 400-1100 nm, which comprises the following components: primer paint and topcoat paint;
the primer paint comprises: aqueous acrylic resin, modified carbon aerogel, modified diatomite, a dispersing aid and water. The mass ratio of the primer is (0.9-1.1), (0.1-0.2), (1-2), (0.1-0.3) and (4-6) in sequence according to the material sequence.
The topcoat paint comprises: the modified carbon aerogel comprises water-based acrylic resin, modified carbon aerogel, modified diatomite, a dispersing aid, an organic solvent and water. The mass ratio of the paint on the surface layer is (0.9-1.1), (0.2-0.4), (2-4), (0.1-0.3), (0.5-1) and (4-6) in sequence according to the material sequence.
The modified carbon aerogel is carbon aerogel modified by nitric acid, and the specific surface area of the carbon aerogel is 1500-4000m 2 Per gram, the density is 0.1-0.5 g/cm 3 And is commercially available.
The modified diatomite is obtained by purifying, alkali dissolving and reaming and grafting by a silane coupling agent, the particle size distribution of the modified diatomite after reaming and before grafting is 6-12 mu m, the main micropore pore size distribution range is 400-800 nm, and the original diatomite is commercial primary soil (2000 meshes).
The organic solvent is one or two of absolute ethyl alcohol, chloroform, acetone and tetrahydrofuran.
The aqueous acrylic resin is selected from: one of water-soluble acrylic resin, emulsion acrylic resin and water-dispersible acrylic resin.
The dispersing aid adopts one of BYK192 and AD 3016.
In a second aspect, the invention provides a method for preparing a coating paint according to the first aspect, wherein,
the preparation method of the primer comprises the following steps:
(1) Adding aqueous acrylic resin, a dispersing aid and water into a container A1 as a binder component;
(2) Adding the modified carbon aerogel and glass beads into a container A1 in the step (1);
(3) Placing the container A1 in the step (2) in a sanding and stirring device, stirring the paint, uniformly dispersing the paint, filtering glass beads, forming black color paste, and pouring the black color paste into the container B1.
(4) Adding the modified diatomite into the black color paste of the container B1 in the step (3), and mechanically stirring to obtain a bottom paint, wherein spraying and coating can be performed;
the modified carbon aerogel is carbon aerogel modified by nitric acid, and the specific surface area of the carbon aerogel is 1500-4000m 2 Per gram, the density is 0.1-0.5 g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The particle size of the modified diatomite is 6-12 mu m, and the pore diameter is 400-800 nm.
The particle size and the pore size of the modified diatomite after reaming and before grafting are the particle size and the pore size of the modified diatomite. The grafting has no effect on the particle size and pore size of the diatomaceous earth. The grafting modification aims to uniformly disperse diatomite in a water-based acrylic resin system and reduce sedimentation and agglomeration.
Still preferably, in the step (2), the glass beads have a size of 0.5 to 0.8mm; the mass ratio of the nitric acid modified aerogel to the glass beads is 1 (20-25);
in the step (3), the rotating speed of the sanding and stirring device is 2000-2500 r/min, and the stirring time is 3-4 h;
in the step (4), the rotating speed of the mechanical stirring is 1000-1500 r/min, and the stirring time is 2-3 h.
Preferably, the preparation method of the surface layer paint comprises the following steps:
(1) Adding aqueous acrylic resin, a dispersing aid and water into a container A2 as a bonding component;
(2) Adding the modified carbon aerogel and glass beads into a container A2 in the step (1);
(3) Placing the container A2 in the step (2) in a sanding and stirring device, stirring the paint, uniformly dispersing the paint, filtering glass beads, forming black color paste, and pouring the black color paste into the container B2;
(4) Adding water, an organic solvent and modified diatomite into a container C2, stirring, adding the mixture into the black color paste of the container B2 in the step (3), and mechanically stirring to obtain a surface layer paint;
the specific surface area of the carbon aerogel is 1500-4000m 2 Per gram, the density is 0.1-0.5 g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The particle size of the modified diatomite is 6-12 mu m, and the pore diameter is 400-800 nm.
Still preferably, in the step (2), the glass beads have a size of 0.5 to 0.8mm; the mass ratio of the nitric acid modified aerogel to the glass beads is 1 (20-25);
in the step (3), the rotating speed of the sanding and stirring device is 2000-2500 r/min, and the stirring time is 3-4 h;
in the step (4), the rotating speed of the mechanical stirring is 1000-1500 r/min, and the stirring time is 2-3 h.
In the step (4), the organic solvent is acetone.
Preferably, the preparation method of the nitric acid modified carbon aerogel comprises the following steps:
(1) Adding carbon aerogel and concentrated nitric acid into a round-bottom flask, wherein 50ml of concentrated nitric acid (65% -68%) is corresponding to each 1g of carbon aerogel, refluxing at a constant temperature of 50-70 ℃ for 2-4 hours, and naturally cooling to room temperature to obtain black suspension.
(2) And (3) carrying out suction filtration on the black suspension obtained in the step (1) on a Buchner funnel to obtain black powder, and repeatedly flushing the black powder by deionized water until the flushing liquid is colorless and transparent.
(3) And (3) drying the black powder subjected to suction filtration in the step (2) to obtain the nitric acid modified carbon aerogel powder.
Preferably, the preparation method of the modified diatomite comprises the following steps:
(1) Dispersing diatomite with water, soaking for 24 hr, ultrasonic sieving (2000 mesh), and oven drying.
(2) Adding the diatomite purified in the step (1) into deionized water and heating the solution to 80 ℃.
(3) Sodium hydroxide was added to the solution of step (2) and stirred at 80℃for 40min.
(4) In the step (2) and the step (3), the mass ratio of diatomite to deionized water to sodium hydroxide is (1-1.2): (5-10), and (0.5-1).
(5) Filtering the solution in the step (3), washing the diatomite to be neutral, and finishing the alkali-dissolution reaming of the diatomite.
(6) Adding the diatomite subjected to alkali dissolution and hole expansion in the step (5) into deionized water again, and then adding a silane coupling agent to form a solution.
(7) The silane coupling agent added in the step (6) can be 1 or 2 of KH-792, KH-570, KH-590 and KH-560, and the mass ratio of the silane coupling agent to the diatomite is (0.5-1): 10.
(9) And (3) carrying out ultrasonic treatment on the solution in the step (6) at 40 ℃ for 2 hours, filtering and drying to obtain the alkali-soluble hole-enlarging diatomite grafted by the silane coupling agent.
In the preparation method, the modified diatomite provides microscopic extinction characteristics for the coating, and the organic solvent contained in the surface layer paint is mixed with water to cause the surface of the coating to be rough, so that extinction traps are provided by the modified diatomite. The carbon aerogel with high specific surface area can be better dispersed in an organic resin system through nitric acid modification, so that the coating has excellent light absorption performance.
The aqueous acrylic resin serves as a binder, the auxiliary agent provides dispersion, and promotes curing, and water serves as a solvent.
The third aspect of the invention provides a 400-1100 nm band high-absorption stray light eliminating coating, which is prepared by the following steps: spraying the primer paint and the top coat paint of any one of the first aspects on a substrate test piece in sequence, and curing to obtain the stray light eliminating coating.
The substrate test pieces include, but are not limited to, aluminum alloys, magnesium alloys, stainless steel, titanium alloys, carbon fiber composites, polyetheretherketone composites, and the like. Preferably, an aluminum alloy is used.
The curing mode is normal temperature curing, preferably, the temperature is 25 ℃ for 18 hours.
In a fourth aspect the invention provides the use of a stray light removing coating according to the third aspect for absorbing stray light in the 400-1100 nm band.
In a fifth aspect the invention provides the use of a coating according to the third aspect for absorbing stray light in the 400-1100 nm band in a spatial optical system.
The absorbance increase amplitude of the coating affects the optical properties:
the space stray light has a role in overruling the optical remote sensing imaging quality of the spacecraft, and the existing space optical remote sensing equipment such as a star sensor, a spectrometer, a space camera and the like all adopt a light shield structure and are coated with stray light eliminating coatings on the inner surface to inhibit the stray light. The wave band of 400-1100 nm is the main working wave band of the optical equipment, the absorption rate of the currently used stray light eliminating coating in the wave band of 400-1100 nm is at the level of 0.98 at the highest, and a large-size light shield is still needed to be matched with the light shield to realize the absolute inhibition of stray light. Along with the increasing width of the existing optical remote sensing equipment, the remote sensing precision is higher and higher, the size of the lens of the space optical equipment is obviously increased, the caliber can reach more than 1m, the maximum caliber size of the light shield breaks through two meters according to the original coating absorptivity level of 0.98, the whole satellite weight is greatly increased, and the space optical equipment is difficult to store in a rocket fairing.
When the solar absorptivity of the coating reaches 0.99, the incident stray light can enter the lens energy detection surface through at least more than 2 times of scattering in the existing product design, and the stray light with the incident energy of 1 is absorbed by the 0.97 absorptivity coating for 2 times to obtain the scattered energy with the (1-0.97) 2=9×10 -4 The method comprises the steps of carrying out a first treatment on the surface of the After 2 absorption with a 0.98 absorption coating, the scattered energy is (1-0.98) 2=4×10 -4 . If the absorptivity of the coating is increased to 0.99, the energy is scattered to be (1-0.99) 2=1×10 after the coating is absorbed for 2 times by the 0.99 absorptivity coating -4 . The scattering energy with the coating absorptivity of 0.99 is 25% of the scattering energy with the coating absorptivity of 0.98, and is 11% of the coating absorptivity of 0.97, the scattering energy is obviously reduced, and the size of the light shield can be greatly reduced and the whole weight of the satellite can be lightened under the same stray light inhibition requirement.
However, the development difficulty of the coating in the wave band of 400-1100 nm is very high, namely the absorption rate level of the filler in the paint, which is responsible for the absorption capacity, is less than 0.99, and after the filler becomes the coating, the film forming substance in the coating can enhance the specular reflection of the interface, and the absorption rate can be further reduced.
Compared with the prior art, the invention has the following beneficial effects:
1. The invention develops a diatomite aperture structure-based 400-1100 nm band high-absorption stray light eliminating coating paint. The coating paint takes carbon aerogel and diatomite as fillers, and can be cured to form a high-absorption coating with a bottom layer and surface layer structure. Aiming at the high-absorption stray light eliminating requirement of a spectrum band of 400-1100 nm, the coating combines diatomite with specific particle size and aperture size under the cooperation of a rough interface structure created by mixing solvents with different volatilization rates on the basis of the original high-light absorption carbon aerogel filler, so that the surface of the coating forms a compact special structure capable of absorbing light, incident light is subjected to multiple reflection and absorption in a concave, the reflectivity is further reduced, the light absorption performance of the coating is optimized, and low reflection and high absorptivity are realized. The invention can be used for space earth observation cameras, spectrometers, space telescopes, star sensors and other spacecraft optical remote sensing products with imaging function in the 400-1100 nm spectrum.
2. The solar absorptivity of the coating prepared by the invention can reach 0.993 at the wave band of 400-1100 nm, and the hemispherical emissivity can reach 0.93 (the hemispherical emissivity is high and the heat dissipation is good, and the hemispherical emissivity is low and the heat dissipation is poor). The coating binding force is superior to grade 1 by using a cross-hatch test.
Drawings
Fig. 1 is a schematic diagram of a coating structure.
Fig. 2 shows absorption spectrum curves of the coatings of example 1, example 2 and example 3.
FIG. 3 is a photograph of the local pore diameter microscopic morphology of diatomite particles after alkali-dissolution reaming and before silane coupling agent grafting.
Description of the drawings:
1. and the substrate test piece, 2, the coating primer layer, 3, the coating top-coat layer, 4, the modified diatomite, 5, the modified carbon nano aerogel, 6, water and an organic solvent are used for promoting the acrylate to be solidified to form a coating interface coarse structure.
Detailed Description
The present invention will be described with reference to specific examples, but embodiments of the present invention are not limited thereto. Experimental methods, in which specific conditions are not specified in examples, are generally available commercially according to conventional conditions as well as those described in handbooks, or according to general-purpose equipment, materials, reagents, etc. used under conditions suggested by manufacturers, unless otherwise specified. The raw materials required in the following examples and comparative examples are all commercially available.
Example 1
A 400-1100 nm band high absorption stray light removing coating paint, the coating paint comprising: primer paint and topcoat paint.
The preparation method of the primer comprises the following steps:
(1) 100g of aqueous emulsion acrylic resin, 10g of AD3016 dispersing auxiliary and 500g of water are added into A as a binder component;
(2) 15g of nitric acid modified carbon aerogel and 300g of glass beads are added into a container A1 in the step (1);
(3) And (3) placing the container A1 in the step (2) in a sanding and stirring device, sanding and dispersing for 4 hours at 2400r/min, filtering glass beads, forming black color paste, and pouring the black color paste into the container B1.
(4) 200g of modified diatomite is added into the black color paste of the container B1 in the step (3), and is mechanically stirred for 2 hours at 1000r/min to obtain a bottom paint, and spray coating can be carried out.
The preparation method of the surface paint comprises the following steps:
(5) 100g of aqueous emulsion acrylic resin, 20g of AD3016 dispersing auxiliary and 250g of water are added into A as a binder component;
(6) Adding 30g of nitric acid modified carbon aerogel and 600g of glass beads into a container A2 in the step (1);
(7) And (3) placing the container A2 in the step (5) in a sanding and stirring device, sanding and dispersing for 4 hours at 2400r/min, filtering glass beads, forming black color paste, and pouring the black color paste into the container B2.
(8) 250g of water, 50g of acetone and 400g of modified diatomite are added into a container C2, stirred and then added into the black color paste of the container B2 in the step (3), and mechanically stirred for 2 hours at 1000r/min to obtain a surface paint, and spray coating can be carried out.
A preparation method of a 400-1100 nm band high-absorption stray light eliminating coating comprises the following steps:
Uniformly spraying the bottom paint in the step (4) on an aluminum alloy substrate test piece in an air spraying mode by a spray gun for 5 times, wherein the spraying thickness of each time is 5-10 mu m; uniformly spraying the surface layer paint in the step (8) on the bottom paint in an air spraying mode by using a spray gun for 3 times, wherein the spraying thickness of each time is 5-10 mu m;
the test piece obtained in the above step was cured at 25℃for 18 hours to obtain a stray light eliminating coating SC-1.
In this embodiment, the preparation method of the nitric acid modified carbon aerogel comprises the following steps:
(1) Adding 10g of carbon aerogel and 500ml of 68% concentrated nitric acid into a round-bottom flask, refluxing at a constant temperature of 70 ℃ for 3 hours, and naturally cooling to room temperature to obtain black suspension; the specific surface area of the selected carbon aerogel is 2200m 2 Per gram, density 0.1g/cm 3 ;
(2) And (3) carrying out suction filtration on the black suspension obtained in the step (1) on a Buchner funnel to obtain black powder, and repeatedly flushing the black powder by deionized water until the flushing liquid is colorless and transparent.
(3) And (3) drying the black powder subjected to suction filtration in the step (2) to obtain nitric acid modified carbon aerogel powder which is used for preparing the paint.
In the embodiment, the preparation method of the modified diatomite comprises the following steps:
(1) 550g of diatomite is dispersed by water and then is soaked for 24 hours, and then is dried through the mesh (2000 meshes) after ultrasonic treatment.
(2) 500g of the purified diatomaceous earth from step (1) was added to 3000g of deionized water and the solution was heated to 80 ℃.
(3) 400g of sodium hydroxide was added to the solution of step (2) and stirred at 80℃for 40min.
(4) Filtering the solution in the step (3), washing the diatomite to be neutral, and finishing the alkali-dissolution reaming of the diatomite.
(5) 400g of the diatomite subjected to alkali dissolution and hole expansion in the step (4) is taken and added into deionized water again, and 20g of KH-792 silane coupling agent is added to form a solution.
(6) And (3) carrying out ultrasonic treatment on the solution obtained in the step (5) at 40 ℃ for 2 hours, filtering and drying to obtain alkali-soluble hole-enlarging diatomite grafted by a silane coupling agent, namely the modified diatomite. Fig. 3 is a microscopic morphology photograph of the local pore diameter of the diatomite particles after alkali-dissolution reaming and before silane coupling agent grafting, and the pore diameter of the diatomite particles after alkali-dissolution reaming is 400-800 nm. And the measured diatomite particle size after alkali dissolution and reaming is 6-12 mu m.
The coating (SC-1) obtained in this example 1 had an optical absorptivity of 0.993 at the 400-1100 nm band, and a hemispherical emissivity (. Epsilon H ) The binding force of the coating is better than grade 1, the average thickness of the coating is 80 mu m, the appearance is rough and compact, and the powder cannot be dropped to touch.
A schematic representation of the coating structure of the coating (SC-1) is shown in FIG. 1. The coating structure comprises: the paint comprises a substrate test piece 1, a coating primer layer 2 formed by curing a bottom paint, a coating finish paint layer 3 formed by curing a top paint, modified diatomite 4 and modified carbon nano aerogel 5. In addition, the water and organic solvent promote the curing of the acrylate to form the coating interface roughness 6.
The coating is designed as a bottom layer and a surface layer, the bottom layer has the function of providing enough bonding performance, ensuring the bonding force between the coating and the base material, and the surface layer has the function of forming a special structure on the surface, reducing light reflection and further enhancing the light absorption performance of the coating.
Example 2
Nitric acid modified carbon aerogel prepared in example 1 and modified diatomaceous earth were used.
A 400-1100 nm band high absorption stray light removing coating paint, the coating paint comprising: primer paint and topcoat paint.
The preparation method of the primer comprises the following steps:
(1) 100g of aqueous emulsion acrylic resin, 10g of AD3016 dispersing auxiliary and 500g of water are added into A as a binder component;
(2) Adding 10g of nitric acid modified carbon aerogel and 200g of glass beads into a container A1 in the step (1);
(3) And (3) placing the container A1 in the step (2) in a sanding and stirring device, sanding and dispersing for 4 hours at 2400r/min, filtering glass beads, forming black color paste, and pouring the black color paste into the container B1.
(4) 200g of modified diatomite is added into the black color paste of the container B1 in the step (3), and is mechanically stirred for 2 hours at 1000r/min to obtain a bottom paint, and spray coating can be carried out.
The preparation method of the surface paint comprises the following steps:
(5) 100g of aqueous emulsion acrylic resin, 20g of AD3016 dispersing auxiliary and 250g of water are added into A as a binder component;
(6) Adding 20g of nitric acid modified carbon aerogel and 500g of glass beads into a container A2 in the step (1);
(7) And (3) placing the container A2 in the step (5) in a sanding and stirring device, sanding and dispersing for 4 hours at 2400r/min, filtering glass beads, forming black color paste, and pouring the black color paste into the container B2.
(8) 250g of water, 50g of acetone and 400g of modified diatomite are added into a container C2, stirred and then added into the black color paste of the container B2 in the step (3), and mechanically stirred for 2 hours at 1000r/min to obtain a surface paint, and spray coating can be carried out.
A preparation method of a 400-1100 nm band high-absorption stray light eliminating coating comprises the following steps:
uniformly spraying the bottom paint in the step (4) on an aluminum alloy substrate test piece in an air spraying mode by a spray gun for 5 times, wherein the spraying thickness of each time is 5-10 mu m; uniformly spraying the surface layer paint in the step (8) on the bottom paint in an air spraying mode by using a spray gun for 3 times, wherein the spraying thickness of each time is 5-10 mu m;
the test piece obtained in the above step was cured at 25℃for 18 hours to obtain a stray light eliminating coating SC-2.
The coating (SC-2) obtained in this example 2 had an optical absorptivity of 0.991 at a wavelength band of 400 to 1100nm, and a hemispherical emissivity (. Epsilon H ) The binding force of the coating is 0.92, which is superior to grade 1, the average thickness of the coating is 80 mu m, the appearance is rough and compact, and the powder cannot be dropped to touch.
Example 3
Nitric acid modified carbon aerogel prepared in example 1 and modified diatomaceous earth were used.
A 400-1100 nm band high absorption stray light removing coating paint, the coating paint comprising: primer paint and topcoat paint.
The preparation method of the primer comprises the following steps:
(1) 100g of aqueous emulsion acrylic resin, 10g of AD3016 dispersing auxiliary and 500g of water are added into A as a binder component;
(2) 15g of nitric acid modified carbon aerogel and 300g of glass beads are added into a container A1 in the step (1);
(3) And (3) placing the container A in the step (2) in a sanding and stirring device, sanding and dispersing for 4 hours at 2400r/min, filtering glass beads, forming black color paste, and pouring the black color paste into the container B1.
(4) 100g of modified diatomite is added into the black color paste of the container B1 in the step (3), and is mechanically stirred for 2 hours at 1000r/min to obtain a bottom paint, and spray coating can be carried out.
The preparation method of the surface paint comprises the following steps:
(5) 100g of aqueous emulsion acrylic resin, 20g of AD3016 dispersing auxiliary and 250g of water are added into A as a binder component;
(6) Adding 30g of nitric acid modified carbon aerogel and 600g of glass beads into a container A2 in the step (1);
(7) And (3) placing the container A2 in the step (5) in a sanding and stirring device, sanding and dispersing for 4 hours at 2400r/min, filtering glass beads, forming black color paste, and pouring the black color paste into the container B2.
(8) 250g of water, 50g of acetone and 200g of modified diatomite are added into a container C2, stirred and then added into the black color paste of the container B2 in the step (3), and mechanically stirred for 2 hours at 1000r/min to obtain a surface paint, and spray coating can be carried out.
A preparation method of a 400-1100 nm band high-absorption stray light eliminating coating comprises the following steps:
uniformly spraying the bottom paint in the step (4) on an aluminum alloy substrate test piece in an air spraying mode by a spray gun for 5 times, wherein the spraying thickness of each time is 5-10 mu m; uniformly spraying the surface layer paint in the step (8) on the bottom paint in an air spraying mode by using a spray gun for 3 times, wherein the spraying thickness of each time is 5-10 mu m;
the test piece obtained in the above step is cured for 18 hours at 25 ℃ to obtain the stray light removing coating SC-3.
The coating (SC-3) obtained in example 3 had an optical absorptivity of 0.990 at a wavelength band of 400 to 1100nm, and a hemispherical emissivity (. Epsilon H ) The binding force of the coating is better than grade 1, the average thickness of the coating is 80 mu m, the appearance is rough and compact, and the powder cannot be dropped to touch.
Comparative example 1 excessive powder of topcoat
Nitric acid modified carbon aerogel prepared in example 1 and modified diatomaceous earth were used. The quality of the nitric acid modified carbon aerogel and modified diatomaceous earth was increased in the topcoat paint as compared to example 1.
A 400-1100 nm band high absorption stray light removing coating paint, the coating paint comprising: primer paint and topcoat paint.
The preparation method of the primer comprises the following steps:
(1) 100g of aqueous emulsion acrylic resin, 10g of AD3016 dispersing auxiliary and 500g of water are added into A as a binder component;
(2) 15g of nitric acid modified carbon aerogel and 300g of glass beads are added into a container A1 in the step (1);
(3) And (3) placing the container A1 in the step (2) in a sanding and stirring device, sanding and dispersing for 4 hours at 2400r/min, filtering glass beads, forming black color paste, and pouring the black color paste into the container B1.
(4) 200g of modified diatomite is added into the black color paste of the container B in the step (3), and is mechanically stirred for 2 hours at 1000r/min to obtain a bottom paint, and spray coating can be carried out.
The preparation method of the surface paint comprises the following steps:
(5) 100g of aqueous emulsion acrylic resin, 20g of AD3016 dispersing auxiliary and 350g of water are added into A as a binder component;
(6) Adding 50g of nitric acid modified carbon aerogel and 1000g of glass beads into a container A2 in the step (1);
(7) And (3) placing the container A2 in the step (5) in a sanding and stirring device, sanding and dispersing for 4 hours at 2400r/min, filtering glass beads, forming black color paste, and pouring the black color paste into the container B2.
(8) 250g of water, 50g of acetone and 500g of modified diatomite are added into a container C2, stirred and then added into the black color paste of the container B2 in the step (3), and mechanically stirred for 2 hours at 1000r/min to obtain a surface paint, and spray coating can be carried out.
A preparation method of a 400-1100 nm band high-absorption stray light eliminating coating comprises the following steps:
uniformly spraying the bottom paint in the step (4) on an aluminum alloy substrate test piece in a spray gun air spraying mode for 5 times, wherein the spraying thickness of each time is 5-10 mu m; uniformly spraying the surface layer paint in the step (8) on the bottom paint in an air spraying mode by using a spray gun for 3 times, wherein the spraying thickness of each time is 5-10 mu m;
the test piece obtained in the above step was cured at 25℃for 18 hours to obtain a stray light eliminating coating SC-4.
The coating (SC-4) obtained in comparative example 1 had an optical absorptivity of 0.983 at a wavelength band of 400 to 1100nm, and a hemispherical emissivity (. Epsilon.) H ) The average thickness of the coating is 0.93 mu m, the powder falling phenomenon of the coating is obvious, the binding force of the coating cannot be tested, the binding performance of the coating is at risk of cracking and powder falling, the coating is easy to pollute high-precision optical instruments, and the coating cannot be practically applied.
Comparative example 2 paint powder too little
Nitric acid modified carbon aerogel prepared in example 1 and modified diatomaceous earth were used. The quality of the nitric acid modified carbon aerogel and modified diatomaceous earth was reduced in the topcoat paint compared to example 1.
A 400-1100 nm band high absorption stray light removing coating paint, the coating paint comprising: primer paint and topcoat paint.
The preparation method of the primer comprises the following steps:
(1) 100g of aqueous emulsion acrylic resin, 10g of AD3016 dispersing auxiliary and 500g of water are added into A as a binder component;
(2) 15g of nitric acid modified carbon aerogel and 300g of glass beads are added into a container A1 in the step (1);
(3) And (3) placing the container A1 in the step (2) in a sanding and stirring device, sanding and dispersing for 4 hours at 2400r/min, filtering glass beads, forming black color paste, and pouring the black color paste into the container B1.
(4) 200g of modified diatomite is added into the black color paste of the container B in the step (3), and is mechanically stirred for 2 hours at 1000r/min to obtain a bottom paint, and spray coating can be carried out.
The preparation method of the surface paint comprises the following steps:
(5) 100g of aqueous emulsion acrylic resin, 20g of AD3016 dispersing auxiliary and 250g of water are added into A as a binder component;
(6) 15g of nitric acid modified carbon aerogel and 600g of glass beads are added into a container A2 in the step (1);
(7) And (3) placing the container A2 in the step (5) in a sanding and stirring device, sanding and dispersing for 4 hours at 2400r/min, filtering glass beads, forming black color paste, and pouring the black color paste into the container B2.
(8) 250g of water, 50g of acetone and 150g of modified diatomite are added into a container C2, stirred and then added into the black color paste of the container B2 in the step (3), and mechanically stirred for 2 hours at 1000r/min to obtain a surface paint, and spray coating can be carried out.
A preparation method of a 400-1100 nm band high-absorption stray light eliminating coating comprises the following steps:
uniformly spraying the bottom paint in the step (4) on an aluminum alloy substrate test piece in an air spraying mode by a spray gun for 5 times, wherein the spraying thickness of each time is 5-10 mu m; uniformly spraying the surface paint in the step (8) on the bottom paint by adopting a spray gun air spraying mode, wherein the spraying thickness is 5-10 mu m in each spraying time for 3 times;
and curing the test piece obtained in the step at 25 ℃ for 18 hours to obtain the stray light eliminating coating SC-5.
The coating (SC-5) obtained in comparative example 2 had an optical absorptivity of 0.980 at a wavelength band of 400 to 1100nm, and a hemispherical emissivity (. Epsilon.) H ) The binding force of the coating is better than grade 1, the average thickness of the coating is 80 mu m, the appearance is rough and compact, and the powder cannot be dropped to touch. It can be seen that the filler content is too low and has a large influence on the absorption rate of the coating in the 400-1100 nm band.
Comparative example 3-topcoat without solvent blend
Nitric acid modified carbon aerogel prepared in example 1 and modified diatomaceous earth were used. In comparison with example 1, no organic solvent was added in the topcoat paint preparation step (8).
A 400-1100 nm band high absorption stray light removing coating paint, the coating paint comprising: primer paint and topcoat paint.
The preparation method of the primer comprises the following steps:
(1) 100g of aqueous emulsion acrylic resin, 10g of AD3016 dispersing auxiliary and 500g of water are added into A as a binder component;
(2) 15g of nitric acid modified carbon aerogel and 300g of glass beads are added into a container A1 in the step (1);
(3) And (3) placing the container A1 in the step (2) in a sanding and stirring device, sanding and dispersing for 4 hours at 2400r/min, filtering glass beads, forming black color paste, and pouring the black color paste into the container B1.
(4) 200g of modified diatomite is added into the black color paste of the container B1 in the step (3), and is mechanically stirred for 2 hours at 1000r/min to obtain a bottom paint, and spray coating can be carried out.
The preparation method of the surface paint comprises the following steps:
(5) 100g of aqueous emulsion acrylic resin, 20g of AD3016 dispersing auxiliary and 250g of water are added into A as a binder component;
(6) Adding 30g of nitric acid modified carbon aerogel and 600g of glass beads into a container A2 in the step (1);
(7) And (3) placing the container A2 in the step (4) in a sanding and stirring device, sanding and dispersing for 4 hours at 2400r/min, filtering glass beads, forming black color paste, and pouring the black color paste into the container B2.
(8) 250g of water and 400g of modified diatomite are added into a container C2, stirred and then added into the black color paste of the container B2 in the step (3), and mechanically stirred for 2 hours at 1000r/min to obtain a surface paint, and spray coating can be carried out.
A preparation method of a 400-1100 nm band high-absorption stray light eliminating coating comprises the following steps:
uniformly spraying the bottom paint in the step (4) on an aluminum alloy substrate test piece in an air spraying mode by a spray gun for 5 times, wherein the spraying thickness of each time is 5-10 mu m; uniformly spraying the surface layer paint in the step (8) on the bottom paint in an air spraying mode by using a spray gun for 3 times, wherein the spraying thickness of each time is 5-10 mu m;
the test piece obtained in the above step is cured for 18 hours at 25 ℃ to obtain the stray light removing coating SC-6.
The coating (SC-6) obtained in comparative example 3 had an optical absorptivity of 0.983 at a wavelength band of 400 to 1100nm, and a hemispherical emissivity (. Epsilon.) H ) The binding force of the coating is 0.92, which is superior to grade 1, the average thickness of the coating is 80 mu m, the appearance is rough and compact, and the powder cannot be dropped to touch. The interference of the fast volatile solvent is absent, the film forming performance of the acrylic resin on the surface of the coating is improved, the interface reflection capability is enhanced, but the light absorption performance of the filler is weakened.
Comparative example 4-carbon aerogel unmodified
Modified diatomaceous earth and unmodified carbon aerogel prepared in example 1 were used.
A 400-1100 nm band high absorption stray light removing coating paint, the coating paint comprising: primer paint and topcoat paint.
The preparation method of the primer comprises the following steps:
(1) 100g of aqueous emulsion acrylic resin, 10g of AD3016 dispersing auxiliary and 500g of water are added into A as a binder component;
(2) Adding 15g of carbon aerogel and 300g of glass beads into a container A1 in the step (1);
(3) And (3) placing the container A1 in the step (2) in a sanding and stirring device, sanding and dispersing for 4 hours at 2400r/min, filtering glass beads, forming black color paste, and pouring the black color paste into the container B1.
(4) 200g of modified diatomite is added into the black color paste of the container B in the step (3), and is mechanically stirred for 2 hours at 1000r/min to obtain a bottom paint, and spray coating can be carried out.
The preparation method of the surface paint comprises the following steps:
(5) 100g of aqueous emulsion acrylic resin, 20g of AD3016 dispersing auxiliary and 250g of water are added into A as a binder component;
(6) Adding 30g of carbon aerogel and 600g of glass beads into a container A2 in the step (1);
(7) And (3) placing the container A2 in the step (5) in a sanding and stirring device, sanding and dispersing for 4 hours at 2400r/min, filtering glass beads, forming black color paste, and pouring the black color paste into the container B2.
(8) 250g of water, 50g of acetone and 400g of modified diatomite are added into a container C2, stirred and then added into the black color paste of the container B2 in the step (3), and mechanically stirred for 2 hours at 1000r/min to obtain a surface paint, and spray coating can be carried out.
A preparation method of a 400-1100 nm band high-absorption stray light eliminating coating comprises the following steps:
uniformly spraying the bottom paint in the step (4) on an aluminum alloy substrate test piece in an air spraying mode by a spray gun for 5 times, wherein the spraying thickness of each time is 5-10 mu m; uniformly spraying the surface layer paint in the step (8) on the bottom paint in an air spraying mode by using a spray gun for 3 times, wherein the spraying thickness of each time is 5-10 mu m;
the test piece obtained in the above step was cured at 25℃for 18 hours to obtain a stray light eliminating coating SC-7.
The coating (SC-7) obtained in comparative example 4 had an optical absorptivity of 0.980 at a wavelength band of 400 to 1100nm, and a hemispherical emissivity (. Epsilon.) H ) The binding force of the coating is better than grade 3, the average thickness of the coating is 80 mu m, the appearance is rough and compact, and the powder cannot be dropped to touch. The carbon aerogel is not modified by nitric acid, has poor compatibility with organic resin, and the specific surface area is reduced due to the agglomeration phenomenon, so that the absorption capacity of the coating is reduced.
Comparative example 5-primer-less paint, top coat only paint
The preparation method of the surface paint comprises the following steps:
(1) 100g of aqueous emulsion acrylic resin, 20g of AD3016 dispersing auxiliary and 250g of water are added into A as a binder component;
(2) Adding 30g of nitric acid modified carbon aerogel and 600g of glass beads into a container A2 in the step (1);
(3) And (3) placing the container A2 in the step (2) in a sanding and stirring device, sanding and dispersing for 4 hours at the rotating speed of 2400r/min, filtering glass beads, forming black color paste, and pouring the black color paste into the container B2.
(4) 250g of water, 50g of acetone and 400g of modified diatomite are added into a container C2, stirred and then added into the black color paste of the container B2 in the step (3), and mechanically stirred for 2 hours at 1000r/min to obtain a surface paint, and spray coating can be carried out.
A preparation method of a 400-1100 nm band high-absorption stray light eliminating coating comprises the following steps:
and (3) uniformly spraying the paint in the step (4) on an aluminum alloy substrate test piece in a spray gun air spraying mode, wherein the spraying is performed for 8 times, and the spraying thickness is 5-10 mu m each time.
The test piece obtained in the above step is cured for 18 hours at 25 ℃ to obtain the stray light removing coating SC-8.
The coating (SC-8) prepared in comparative example 5 was cracked and peeled off on the test piece of the aluminum alloy substrate, and the absorptivity, thickness and binding force could not be measured.
Comparative example 6- (diatomaceous earth having a suitable particle size and a small pore diameter)
Nitric acid modified carbon aerogel prepared using example 1
The pore size distribution range of the modified diatomaceous earth of comparative example 6 is smaller than that of the modified diatomaceous earth of example 1.
Comparative example 6 preparation method of modified diatomaceous earth:
(1) 550g of diatomite is dispersed by water and then is soaked for 24 hours, and then is dried through the mesh (2000 meshes) after ultrasonic treatment.
(2) 500g of the purified diatomaceous earth from step (1) was added to 3000g of deionized water and the solution was heated to 80 ℃.
(3) 250g of sodium hydroxide was added to the solution of step (2) and stirred at 60℃for 40min.
(4) Filtering the solution in the step (3), washing the diatomite to be neutral, and finishing the alkali-dissolution reaming of the diatomite.
(5) 400g of the diatomite subjected to alkali dissolution and hole expansion in the step (4) is taken and added into deionized water again, and 20g of KH-792 silane coupling agent is added to form a solution.
(6) And (3) carrying out ultrasonic treatment on the solution in the step (5) at 40 ℃ for 2 hours, filtering and drying to obtain alkali-soluble hole-enlarging diatomite grafted by a silane coupling agent, namely modified diatomite, which is used for the experiment of the comparative example 6, wherein the particle size distribution of the modified diatomite is 6-12 mu m, and the main micropore size distribution range is 100-300 nm. The pore size distribution range of the modified diatomaceous earth of comparative example 6 is smaller than that of the modified diatomaceous earth of example 1.
A 400-1100 nm band high absorption stray light removing coating paint, the coating paint comprising: primer paint and topcoat paint.
The preparation method of the primer comprises the following steps:
(1) 100g of aqueous emulsion acrylic resin, 10g of AD3016 dispersing auxiliary and 500g of water are added into A as a binder component;
(2) 15g of nitric acid modified carbon aerogel and 300g of glass beads are added into a container A1 in the step (1);
(3) And (3) placing the container A1 in the step (2) in a sanding and stirring device, sanding and dispersing for 4 hours at 2400r/min, filtering glass beads, forming black color paste, and pouring the black color paste into the container B1.
(4) 200g of modified diatomite is added into the black color paste of the container B1 in the step (3), and is mechanically stirred for 2 hours at 1000r/min to obtain a bottom paint, and spray coating can be carried out.
The preparation method of the surface paint comprises the following steps:
(5) 100g of aqueous emulsion acrylic resin, 20g of AD3016 dispersing auxiliary and 250g of water are added into A as a binder component;
(6) Adding 30g of nitric acid modified carbon aerogel and 600g of glass beads into a container A2 in the step (1);
(7) And (3) placing the container A2 in the step (5) in a sanding and stirring device, sanding and dispersing for 4 hours at 2400r/min, filtering glass beads, forming black color paste, and pouring the black color paste into the container B2.
(8) 250g of water, 50g of acetone and 400g of modified diatomite are added into a container C2, stirred and then added into the black color paste of the container B2 in the step (3), and mechanically stirred for 2 hours at 1000r/min to obtain a surface paint, and spray coating can be carried out.
A preparation method of a 400-1100 nm band high-absorption stray light eliminating coating comprises the following steps:
uniformly spraying the bottom paint in the step (4) on an aluminum alloy substrate test piece in an air spraying mode by a spray gun for 5 times, wherein the spraying thickness of each time is 5-10 mu m; uniformly spraying the surface layer paint in the step (8) on the bottom paint in a spray gun air spraying mode for 3 times, wherein the spraying thickness of each time is 5-10 mu m;
And curing the test piece obtained in the step at 25 ℃ for 18 hours to obtain the stray light eliminating coating SC-9.
The coating (SC-9) obtained in comparative example 6 had an optical absorptivity of 0.985 at a wavelength band of 400 to 1100nm, and a hemispherical emissivity (. Epsilon.) H ) The binding force of the coating is 0.93, the average thickness of the coating is 80 mu m, the appearance is rough and compact, the powder is not dropped when touching, the aperture of the diatomite is not matched with the wavelength of the wave band of 400-1100 nm, and the extinction performance is reduced.
Comparative example 7- (modified diatomaceous earth having a large particle size and a large pore diameter)
Nitric acid modified carbon aerogel prepared using example 1
Comparative example 7 the modified diatomaceous earth had a particle size and pore size distribution range greater than that of example 1.
The preparation method of the modified diatomite in comparative example 7 comprises the following steps:
(1) 550g of diatomite is dispersed by water and then is soaked for 24 hours, and then is dried through the mesh (500 meshes) after ultrasonic treatment.
(2) 500g of the purified diatomaceous earth from step (1) was added to 3000g of deionized water and the solution was heated to 80 ℃.
(3) 500g of sodium hydroxide was added to the solution of step (2) and stirred at 80℃for 40min.
(4) Filtering the solution in the step (3), washing the diatomite to be neutral, and finishing the alkali-dissolution reaming of the diatomite.
(5) 400g of the diatomite subjected to alkali dissolution and hole expansion in the step (4) is taken and added into deionized water again, and 20g of KH-792 silane coupling agent is added to form a solution.
(6) And (3) carrying out ultrasonic treatment on the solution in the step (5) at 40 ℃ for 2 hours, filtering and drying to obtain the alkali-soluble hole-enlarging diatomite grafted by the silane coupling agent, wherein the particle size distribution after modification is 20-25 mu m, and the main micropore size distribution range is 1-2 mu m.
A 400-1100 nm band high absorption stray light removing coating paint, the coating paint comprising: primer paint and topcoat paint.
The preparation method of the primer comprises the following steps:
(1) 100g of aqueous emulsion acrylic resin, 10g of AD3016 dispersing auxiliary and 500g of water are added into A as a binder component;
(2) 15g of nitric acid modified carbon aerogel and 300g of glass beads are added into a container A1 in the step (1);
(3) And (3) placing the container A1 in the step (2) in a sanding and stirring device, sanding and dispersing for 4 hours at 2400r/min, filtering glass beads, forming black color paste, and pouring the black color paste into the container B1.
(4) 200g of modified diatomite is added into the black color paste of the container B1 in the step (3), and is mechanically stirred for 2 hours at 1000r/min to obtain a bottom paint, and spray coating can be carried out.
The preparation method of the surface paint comprises the following steps:
(5) 100g of aqueous emulsion acrylic resin, 20g of AD3016 dispersing auxiliary and 250g of water are added into A as a binder component;
(6) Adding 30g of nitric acid modified carbon aerogel and 600g of glass beads into a container A2 in the step (1);
(7) And (3) placing the container A2 in the step (5) in a sanding and stirring device, sanding and dispersing for 4 hours at 2400r/min, filtering glass beads, forming black color paste, and pouring the black color paste into the container B2.
(8) 250g of water, 50g of acetone and 400g of modified diatomite are added into a container C2, stirred and then added into the black color paste of the container B2 in the step (3), and mechanically stirred for 2 hours at 1000r/min to obtain a surface paint, and spray coating can be carried out.
A preparation method of a 400-1100 nm band high-absorption stray light eliminating coating comprises the following steps:
uniformly spraying the bottom paint in the step (5) on an aluminum alloy substrate test piece in an air spraying mode by using a spray gun, wherein the spraying is performed for 5 times, and the spraying thickness of each time is 5-10 mu m; uniformly spraying the surface layer paint in the step (8) on the bottom paint in an air spraying mode by using a spray gun for 3 times, wherein the spraying thickness of each time is 5-10 mu m;
the test piece obtained in the above step was cured at 25℃for 18 hours to obtain a stray light-free coating SC-10.
The coating (SC-10) obtained in this comparative example 7 had an optical absorptivity of 0.983 at a wavelength band of 400 to 1100nm, and a hemispherical emissivity (. Epsilon H ) 0.93, the binding force of the coating is better than grade 1, and the average coating isThe thickness is 80 mu m, the appearance is rough and compact, the powder cannot be dropped when touching, the particle size and the aperture of the diatomite are not matched with the wavelength of the wave band of 400-1100 nm, and the extinction performance is reduced.
Comparative example 8- (diatomaceous earth having small particle diameter and small pore diameter)
Nitric acid modified carbon aerogel prepared using example 1
Comparative example 8 the modified diatomaceous earth was smaller in particle size and pore size distribution range than the modified diatomaceous earth of example 1.
The preparation method of the modified diatomite in comparative example 8 comprises the following steps:
(1) 550g of diatomite is dispersed by water and then is soaked for 24 hours, and is dried through the mesh (5000 meshes) after ultrasonic treatment.
(2) 500g of the purified diatomaceous earth from step (1) was added to 3000g of deionized water and the solution was heated to 80 ℃.
(3) 500g of sodium hydroxide was added to the solution of step (2) and stirred at 80℃for 40min.
(4) Filtering the solution in the step (3), washing the diatomite to be neutral, and finishing the alkali-dissolution reaming of the diatomite.
(5) 400g of the diatomite subjected to alkali dissolution and hole expansion in the step (4) is taken and added into deionized water again, and 20g of KH-792 silane coupling agent is added to form a solution.
(6) And (3) carrying out ultrasonic treatment on the solution in the step (5) at 40 ℃ for 2 hours, filtering and drying to obtain the alkali-soluble hole-enlarging diatomite grafted by the silane coupling agent, wherein the particle size distribution after modification is 1-2 mu m, and the main micropore size distribution range is 100-200 nm.
A 400-1100 nm band high absorption stray light removing coating paint, the coating paint comprising: primer paint and topcoat paint.
The preparation method of the primer comprises the following steps:
(1) 100g of aqueous emulsion acrylic resin, 10g of AD3016 dispersing auxiliary and 500g of water are added into A as a binder component;
(2) 15g of nitric acid modified carbon aerogel and 300g of glass beads are added into a container A1 in the step (1);
(3) And (3) placing the container A1 in the step (2) in a sanding and stirring device, sanding and dispersing for 4 hours at 2400r/min, filtering glass beads, forming black color paste, and pouring the black color paste into the container B1.
(4) 200g of modified diatomite is added into the black color paste of the container B1 in the step (3), and is mechanically stirred for 2 hours at 1000r/min to obtain a bottom paint, and spray coating can be carried out.
The preparation method of the surface paint comprises the following steps:
(5) 100g of aqueous emulsion acrylic resin, 20g of AD3016 dispersing auxiliary and 250g of water are added into A as a binder component;
(6) Adding 30g of nitric acid modified carbon aerogel and 600g of glass beads into a container A2 in the step (1);
(7) And (3) placing the container A2 in the step (5) in a sanding and stirring device, sanding and dispersing for 4 hours at 2400r/min, filtering glass beads, forming black color paste, and pouring the black color paste into the container B2.
(8) 250g of water, 50g of acetone and 400g of modified diatomite are added into a container C2, stirred and then added into the black color paste of the container B2 in the step (3), and mechanically stirred for 2 hours at 1000r/min to obtain a surface paint, and spray coating can be carried out.
A preparation method of a 400-1100 nm band high-absorption stray light eliminating coating comprises the following steps:
uniformly spraying the bottom paint in the step (4) on an aluminum alloy substrate test piece in an air spraying mode by a spray gun for 5 times, wherein the spraying thickness of each time is 5-10 mu m; uniformly spraying the surface layer paint in the step (8) on the bottom paint in an air spraying mode by using a spray gun for 3 times, wherein the spraying thickness of each time is 5-10 mu m;
the test piece obtained in the above step was cured at 25℃for 18 hours to obtain a stray light-free coating SC-11.
The coating (SC-11) obtained in this comparative example 8 had an optical absorption of 0.977 at a wavelength band of 400 to 1100nm, and a hemispherical emissivity (. Epsilon H ) The bonding force of the coating is 0.92, the bonding force of the coating is better than that of the coating of grade 1, the average thickness of the coating is 80 mu m, the appearance is rough and compact, powder is not dropped when touching, the particle size and the aperture of the diatomite are smaller than those of the wavelength of the wave band of 400-1100 nm, the extinction structure is not effective, and the light absorption performance is seriously reduced.
Comparative example 9-unmodified diatomaceous earth
Nitric acid modified carbon aerogel and unmodified carbon aerogel of example 1 were used.
A 400-1100 nm band high absorption stray light removing coating paint, the coating paint comprising: primer paint and topcoat paint.
The preparation method of the primer comprises the following steps:
(1) 100g of aqueous emulsion acrylic resin, 10g of AD3016 dispersing auxiliary and 500g of water are added into A as a binder component;
(2) 15g of nitric acid modified carbon aerogel and 300g of glass beads are added into a container A1 in the step (1);
(3) And (3) placing the container A1 in the step (2) in a sanding and stirring device, sanding and dispersing for 4 hours at 2400r/min, filtering glass beads, forming black color paste, and pouring the black color paste into the container B1.
(4) 200g of diatomite is added into the black color paste of the container B1 in the step (3), and is mechanically stirred for 2 hours at 1000r/min to obtain a bottom paint, and spray coating can be carried out.
The preparation method of the surface paint comprises the following steps:
(5) 100g of aqueous emulsion acrylic resin, 20g of AD3016 dispersing auxiliary and 250g of water are added into A as a binder component;
(6) Adding 30g of nitric acid modified carbon aerogel and 600g of glass beads into a container A2 in the step (1);
(7) And (3) placing the container A2 in the step (5) in a sanding and stirring device, sanding and dispersing for 4 hours at 2400r/min, filtering glass beads, forming black color paste, and pouring the black color paste into the container B2.
(8) 250g of water, 50g of acetone and 400g of diatomite are added into a container C2, stirred and then added into the black color paste of the container B2 in the step (3), and mechanically stirred for 2 hours at 1000r/min to obtain a surface paint, and spray coating can be carried out.
A preparation method of a 400-1100 nm band high-absorption stray light eliminating coating comprises the following steps:
Uniformly spraying the bottom paint in the step (4) on an aluminum alloy substrate test piece in an air spraying mode by a spray gun for 5 times, wherein the spraying thickness of each time is 5-10 mu m; uniformly spraying the surface layer paint in the step (8) on the bottom paint in an air spraying mode by using a spray gun for 3 times, wherein the spraying thickness of each time is 5-10 mu m;
the test piece obtained in the above step was cured at 25℃for 18 hours to obtain a stray light-free coating SC-11.
The coating (SC-12) obtained in comparative example 9 had an optical absorption of 0.976 at a wavelength band of 400 to 1100nm, and a hemispherical emissivity (. Epsilon H ) The binding force of the coating is 0.90, the coating is better than grade 2, the average thickness of the coating is 80 mu m, the appearance is rough and compact, the diatomite is slightly powder-falling after touching, the diatomite is not modified, the wetting and bonding performance of the diatomite by resin is reduced, the filler is agglomerated and powder-falling, and the microstructure performance cannot be reflected.
Application example 1: coating performance test
1. Coating stray light eliminating performance detection
The coatings prepared in examples 1-3 and each comparative example had an average thickness of about 80 μm, and the coating reflectivity (i.e., absorbance in the 400-1100nm band in the table below) and the coating hemispherical emissivity were measured using an ultraviolet-visible near infrared spectrophotometer, with the results shown in tables 1 and 2 below.
2. Adhesion force
The coatings prepared in examples 1-3 and each comparative example were scored with an average thickness of about 80 μm, reference standard GB/T5210-2006 color paint and varnish pull-off test, and then adhered to the scored place using a 3M tape and pulled up quickly, the coating was observed for peeling and the coating adhesion was verified with reference to the standard rating, and the results are shown in tables 1 and 2 below.
TABLE 1
TABLE 2
It can be seen from tables 1 and 2 that the combination properties of examples 1 to 3 are superior to those of the comparative examples, especially the 400-1100nm band absorption and coating emissivity.
Claims (6)
1. The utility model provides a 400 ~ 1100nm wave band high absorption stray light eliminating coating paint which characterized in that, the coating paint includes: primer paint and topcoat paint;
the primer paint comprises: water, modified carbon aerogel and modified diatomaceous earth; the modified carbon aerogel is nitric acid modified carbon aerogel, and the specific surface area of the carbon aerogel is 1500-4000m 2 Per gram, the density is 0.1-0.5 g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The particle size of the modified diatomite is 6-12 mu m, the pore diameter is 400-800 nm, wherein the mass ratio of the modified carbon aerogel to the modified diatomite is (0.1-0.2): 1-2;
the topcoat paint comprises: water, organic solvent, modified carbon aerogel and modified diatomite; the modified carbon aerogel is nitric acid modified carbon aerogel, and the specific surface area of the carbon aerogel is 1500-4000m 2 Per gram, the density is 0.1-0.5 g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The particle size of the modified diatomite is 6-12 mu m, the pore diameter is 400-800 nm, wherein the mass ratio of the modified carbon aerogel to the modified diatomite is (0.2-0.4): 2-4;
the primer further comprises: aqueous acrylic resin, dispersing aid; the primer paint comprises the following aqueous acrylic resin, modified carbon aerogel, modified diatomite, a dispersing aid and water in mass ratio: (0.9-1.1): (0.1-0.2): (1-2): (0.1-0.3): (4-6);
The topcoat paint further includes: aqueous acrylic resin, dispersing aid; the mass ratio of the water-borne acrylic resin to the modified carbon aerogel to the modified diatomite to the dispersing aid to the organic solvent to the water in the surface paint is (0.9-1.1): (0.2-0.4): (2-4): (0.1-0.3): (0.5-1): (4-6);
the modified diatomite is obtained by performing alkali-dissolution reaming and silane coupling agent modification on raw diatomite, and the particle size and the pore diameter of the modified diatomite refer to the particle size and the pore diameter of the diatomite after alkali-dissolution reaming and before silane coupling agent modification.
2. The method of preparing a coating paint according to claim 1, wherein the method of preparing a primer paint comprises the steps of:
(1) Adding an aqueous acrylic resin, a dispersing aid and water into a container A1 as a binder component;
(2) Adding the modified carbon aerogel and glass beads into a container A1 in the step (1);
(3) Placing the container A1 in the step (2) in a sanding and stirring device, stirring the paint, uniformly dispersing the paint, filtering glass beads, forming black color paste, and pouring the black color paste into the container B1;
(4) Adding the modified diatomite into the black color paste of the container B1 in the step (3), and stirring to prepare a bottom paint;
The mass ratio of the water-based acrylic resin to the nitric acid modified carbon aerogel to the modified diatomite to the dispersing aid to the water is as follows: (0.9-1.1): (0.1-0.2): (1-2): (0.1-0.3): (4-6);
the modified carbon aerogel is nitric acid modified carbon aerogel, and the specific surface area of the carbon aerogel is 1500-4000m 2 Per gram, the density is 0.1-0.5 g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The particle size of the modified diatomite is 6-12 mu m, and the pore diameter is 400-800 nm.
3. The method of preparing a coating paint according to claim 1, wherein the method of preparing a top coat paint comprises the steps of:
(1) Adding an aqueous acrylic resin, a dispersing aid and water into a container A2 as a binder component;
(2) Adding the modified carbon aerogel and glass beads into a container A2 in the step (1);
(3) Placing the container A2 in the step (2) in a sanding and stirring device, stirring the paint, uniformly dispersing the paint, filtering glass beads, forming black color paste, and pouring the black color paste into the container B2;
(4) Adding water, an organic solvent and modified diatomite into a container C2, stirring, adding the mixture into the black color paste of the container B2 in the step (3), and uniformly mixing and stirring to prepare a surface layer paint;
the mass ratio of the water-borne acrylic resin to the modified carbon aerogel to the modified diatomite to the dispersing aid to the organic solvent to the water in the surface paint is (0.9-1.1): (0.2-0.4): (2-4): (0.1-0.3): (0.5-1): (4-6);
The said modificationThe carbon aerogel is nitric acid modified carbon aerogel, and the specific surface area of the carbon aerogel is 1500-4000m 2 Per gram, the density is 0.1-0.5 g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The particle size of the modified diatomite is 6-12 mu m, and the pore diameter is 400-800 nm.
4. The high-absorption stray light eliminating coating with the wave band of 400-1100 nm is characterized by comprising the following preparation method: the primer paint and the top paint of claim 1 are sprayed on a test piece substrate in sequence, and cured to obtain the stray light eliminating coating.
5. Use of a stray light removing coating according to claim 4 for absorbing stray light in the 400-1100 nm band.
6. Use of a coating according to claim 4 for absorbing stray light in the wavelength band of 400-1100 nm in a spatial optical system.
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