Movatterモバイル変換


[0]ホーム

URL:


CN116082877A - High-reflectivity filler and inorganic thermal control coating thereof and preparation method thereof - Google Patents

High-reflectivity filler and inorganic thermal control coating thereof and preparation method thereof
Download PDF

Info

Publication number
CN116082877A
CN116082877ACN202211728205.2ACN202211728205ACN116082877ACN 116082877 ACN116082877 ACN 116082877ACN 202211728205 ACN202211728205 ACN 202211728205ACN 116082877 ACN116082877 ACN 116082877A
Authority
CN
China
Prior art keywords
potassium silicate
reflectivity
thermal control
coating
control coating
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202211728205.2A
Other languages
Chinese (zh)
Other versions
CN116082877B (en
Inventor
韩贺祥
曹康丽
周博
潘阳阳
费涛
徐骏
刘刚
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shanghai Institute of Satellite Equipment
Original Assignee
Shanghai Institute of Satellite Equipment
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shanghai Institute of Satellite EquipmentfiledCriticalShanghai Institute of Satellite Equipment
Priority to CN202211728205.2ApriorityCriticalpatent/CN116082877B/en
Publication of CN116082877ApublicationCriticalpatent/CN116082877A/en
Application grantedgrantedCritical
Publication of CN116082877BpublicationCriticalpatent/CN116082877B/en
Activelegal-statusCriticalCurrent
Anticipated expirationlegal-statusCritical

Links

Images

Classifications

Landscapes

Abstract

The invention discloses a high-reflectivity filler and a preparation method of an inorganic thermal control coating thereof; the coating comprises a finish paint and a covering layer; the finish paint uses modified high-modulus potassium silicate resin solution as a binder, and modified nano zinc oxide as a high-reflectivity filler; the coating layer is mainly modified high modulus potassium silicate resin solution. The thermal control coating of the invention has the appearance of almost white, the thickness of 100-150 mu m, the solar absorption ratio of 0.08-0.16, the hemispherical emissivity of 0.90-0.92 and the total mass loss TML<1% volatile CVCM<0.1%, volume resistivity is less than or equal to 7×107 After the coating is subjected to 100 times of high-temperature heat cycle tests at-196 ℃ to +100 ℃, the phenomena of cracking, peeling, foaming and the like are avoided, the optical performance is stable, the adhesive force is good, the requirements of the spacecraft on the antistatic heat control coating are basically met, and the problems of the space environment stability, the antistatic property and the like of the existing coating type heat control coating for the spacecraft are solved.

Description

High-reflectivity filler and inorganic thermal control coating thereof and preparation method thereof
Technical Field
The invention belongs to the technical field of preparation of thermal control materials, and particularly relates to a high-reflectivity filler, an inorganic thermal control coating and a preparation method thereof.
Background
The thermal control coating is an important component of a spacecraft thermal control system, is coated on the outer surface of the spacecraft, and adjusts the surface thermal balance temperature of the satellite through the self thermal physical characteristic solar absorption ratio and hemispherical emissivity, so that the purpose of thermal control is achieved. In recent decades, thermal control coatings have received wide attention from the aerospace kingdoms of the world, and a plurality of series of thermal control coatings suitable for different orbital environments have been developed. The coating type white heat control coating is used as a passive heat control system, belongs to a solar reflection type coating, and mainly comprises inorganic oxide, a binder and a curing agent, wherein the inorganic filler plays a leading role in the optical performance of the coating. The coating type white thermal control coating has the characteristics of simple application process, strong adhesion, wide application range of base materials and the like, and is widely applied to satellite thermal control systems.
The high-reflectivity inorganic thermal control coating is prepared by adopting the high-reflectivity filler prepared by high-temperature sintering and the modified high-modulus potassium silicate resin binder through spraying and other processes, and the preparation method is simple and easy to implement. The obtained product has the advantages of stable and controllable quality and wide light absorption range.
Disclosure of Invention
The invention aims to provide a high-reflectivity filler, an inorganic thermal control coating and a preparation method thereof; the high-reflectivity filler is modified by silica sol to form a high-ultraviolet reflecting layer on the surface of the nano zinc oxide based on Mie scattering theory, the reflectivity advantages of zinc oxide and silicon dioxide are integrated, the amplitude of electrons is increased, and the solar spectrum reflectivity is increased; meanwhile, the potassium silicate is an inorganic binder, the performance is stable, the film forming property is obviously improved along with the increase of the modulus, and the optical performance is better. The high-reflectivity inorganic thermal control coating prepared from the coating composition has the advantages of low solar absorption ratio, high hemispherical emissivity, low volume resistivity and the like, ensures the running reliability of a spacecraft, and meets the requirements of the spacecraft on the space environment stability and antistatic property of the coating type thermal control coating.
According to one aspect of the present invention, the following technical solution is provided:
the invention provides a high-reflectivity filler, which is prepared by the following steps: respectively weighing nano zinc oxide and silica sol, and carrying out ultrasonic and high-speed stirring to obtain a mixed solution of the nano zinc oxide and the silica sol; centrifuging and drying to obtain nano-scale mixed powder; sintering to obtain filler particles with high reflectivity.
As one embodiment of the invention, the dosage ratio of the nano zinc oxide to the (30%) silica sol is 4:2-4:5; the ultrasonic treatment is carried out for 0.5 to 2 hours; the high-speed stirring is 300-500r/min.
As an embodiment of the present invention, the nano zinc oxide has a particle size of 30 to 200nm.
As one embodiment of the invention, the silica sol is one or more of acidic silica sol, neutral silica sol and alkaline silica sol.
As one embodiment of the present invention, the centrifugation speed is 6000 to 8000r/min and the centrifugation time is 5 to 10min. The drying temperature is 100-120 ℃, and the drying time is 12-24h. The sintering temperature is 600-1200 ℃ and the sintering time is 1-3h.
The invention also provides a preparation method of the high-reflectivity inorganic thermal control coating, which comprises the following steps:
s1, preparing modified high-modulus inorganic potassium silicate resin: stirring and reacting low-modulus potassium silicate with silica sol to obtain high-modulus potassium silicate solution; carrying out organic modification on the high-modulus potassium silicate solution by adopting a silane coupling agent to obtain a modified high-modulus potassium silicate resin solution;
s2, preparing a coating: taking the modified high-modulus potassium silicate resin solution as a binder, adding the high-reflectivity filler according to any one of claims 1-6, adding a solvent, and uniformly mixing and stirring to obtain a finish paint;
s3, preparing a high-reflectivity inorganic thermal control coating: spraying the finishing paint on the surface of the base material, standing and solidifying; spraying the modified high-modulus potassium silicate resin solution on the surface of the finish paint to form a covering layer, standing and curing to obtain the high-reflectivity inorganic thermal control coating.
As an embodiment of the invention, in step S1, the ratio of low modulus potassium silicate (m=2) to silica sol (30%) is 2:2-2:6.
As one embodiment of the invention, in the step S1, the reaction temperature of the stirring reaction is 30-60 ℃, and the stirring speed is 1000-1500r/min.
As an embodiment of the present invention, in step S1, the modulus of the high modulus potassium silicate solution is 3.0 to 5.0.
In step S1, the organic modification is to dilute the high modulus potassium silicate solution to 30% by mass with deionized water, and mix and modify the solution with silane coupling agent in a total amount of 0.2% -0.8%.
In step S1, the silica sol is one or more of acidic silica sol, neutral silica sol and alkaline silica sol.
In step S1, the silane coupling agent is one or more of KH550, KH560, KH570 as an embodiment of the present invention.
In step S2, as an embodiment of the present invention, the mass ratio of the binder to the filler is 10:3 to 10:9.
In step S2, the stirring speed of the mixing and stirring is 800-1200 r/min.
As an embodiment of the present invention, in step S2, an appropriate amount of deionized water is added as a solvent (the solvent satisfies the spraying conditions in order to adjust the viscosity of the paint).
As one embodiment of the present invention, in step S2, the topcoat viscosity of the topcoat paint satisfies 14 to 17S (measured by a four-coat viscometer).
As one embodiment of the present invention, in the step S3, the standing time is 6 to 12 hours, the curing temperature is 60 to 100 ℃ and the curing time is 24 to 48 hours.
As one embodiment of the present invention, the high reflectivity inorganic thermal control coating has a thickness of 100 to 150 μm.
Compared with the prior art, the invention has the following beneficial effects:
1) The nano zinc oxide is modified by silica sol, so that the optical performance of the coating is obviously improved, the solar absorption ratio is low, and the hemispherical emissivity is high;
2) The silane coupling agent is used for modifying the high-modulus potassium silicate, so that the flexibility of the coating is improved, and the adhesive force is obviously improved.
3) After the coating is subjected to a large temperature difference thermal cycle test, the adhesive force is good.
Drawings
Other features, objects and advantages of the present invention will become more apparent upon reading of the detailed description of non-limiting embodiments, given with reference to the accompanying drawings in which:
FIG. 1 is a schematic structural view of a high reflectivity inorganic thermal control coating of the present invention;
FIG. 2 is a flow chart of the preparation of the high reflectivity inorganic thermal control coating of the present invention;
FIG. 3 is a graph of the spectral reflectance of the high reflectance inorganic thermal control coating of example 4;
FIG. 4 is a graph showing the morphology of the high-reflectivity inorganic thermal control coating of example 4 before and after a high-temperature test; wherein, the left graph is before the high-low temperature test, and the right graph is after the high-low temperature test.
Detailed Description
The invention is described in detail below with reference to the accompanying drawings and detailed description. The following examples will assist those skilled in the art in further understanding the present invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications could be made by those skilled in the art without departing from the inventive concept. These are all within the scope of the present invention.
The high reflectivity filler and its inorganic thermal control coating are shown in figure 1, which is composed of a cover layer and a top coat, the cover layer is coated after the top coat is coated on the base material. The preparation flow of the high-reflection inorganic thermal control coating is shown in figure 2, and comprises the following steps:
step one, preparing a high-reflectivity filler: respectively weighing a certain amount of nano zinc oxide and different types of silica sol, and performing ultrasonic and high-speed stirring and other processes to obtain a mixed solution of the nano zinc oxide and the silica sol; centrifuging and drying the mixed solution to obtain nanoscale mixed powder; sintering the dried mixed powder at a certain temperature and for a certain time to obtain filler particles with high reflectivity;
step two, preparing modified high-modulus inorganic potassium silicate resin: reacting the low-modulus potassium silicate solution with silica sol with different mass ratios at a certain temperature and a certain stirring speed to obtain high-modulus potassium silicate solutions with different moduli; carrying out organic modification on the prepared high-modulus potassium silicate solution by adopting different silane coupling agents to obtain a modified high-modulus potassium silicate resin solution;
step three, preparing a coating: adding high-reflectivity filler powder with different mass ratios into the modified high-modulus potassium silicate resin binder, mixing and stirring, adding a solvent, mixing and stirring uniformly;
step four, preparing a high-reflectivity inorganic thermal control coating: spraying finishing paint, spraying the paint on a substrate, standing for 6-12h, curing for 12-24h at 60-100 ℃, and testing the thickness of the finishing paint with 100-130 mu m by a non-magnetic thickness gauge; spraying the coating layer, standing for 6-12h, spraying the modified high-modulus potassium silicate resin solution, and curing for 12-24h at 60-100 ℃; the high-reflectivity inorganic thermal control coating can be prepared, the total thickness of the coating is 110-150 mu m, the solar absorption ratio is tested by ultraviolet-visible light-near infrared equipment, the hemispherical emissivity is tested by an emissivity tester, the adhesive force is tested by a cross-cut method, and the appearance of the pattern layer is observed through eyes under the irradiation of a flashlight.
Example 1
The embodiment relates to a high-reflectivity filler, an inorganic thermal control coating thereof and a preparation method thereof.
The high-reflectivity inorganic thermal control coating of the embodiment consists of high-reflectivity filler powder and a modified high-modulus potassium silicate resin binder.
Preparation of high reflectance filler: respectively weighing nano zinc oxide and acidic silica sol, wherein the dosage ratio is 4:2, and obtaining a mixed solution of the nano zinc oxide and the acidic silica sol through the processes of 0.5h ultrasonic treatment, 300r/min stirring and the like; centrifuging the mixed solution at 6000r/min for 10min, and drying at 100 ℃ for 24h to obtain nanoscale mixed powder; and sintering the dried mixed powder for 1h at 600 ℃ to obtain the filler particles with high reflectivity.
Preparing modified high-modulus inorganic potassium silicate resin: mixing a low-modulus potassium silicate solution with an acidic silica sol, reacting at a dosage ratio of 1:1 and a temperature of 30 ℃ under a condition of 1000r/min, and supplementing deionized water to obtain a high-modulus potassium silicate solution with a mass fraction of 30% and M=3; adding KH550 accounting for 0.2 percent of the total amount to carry out organic modification (directly adding and stirring uniformly) on the prepared high modulus potassium silicate solution, thus obtaining the modified high modulus potassium silicate resin solution.
Preparing a coating: the dosage ratio of the modified high-modulus potassium silicate resin with M=3 to the high-reflectivity filler is 10:3, a proper amount of deionized water is added, the mixture is uniformly mixed and stirred, the stirring speed is 800r/min, and the viscosity of the finish paint is 14s.
Preparing a high-reflectivity inorganic thermal control coating: in the process of preparing the coating, spraying the finishing paint, standing for 6 hours, and curing for 24 hours at 60 ℃ to obtain the finishing paint with the thickness of about 100 mu m; spraying a coating layer, namely spraying the modified high-modulus potassium silicate resin solution, standing for 6 hours, and curing for 24 hours at 60 ℃; the high-reflectivity inorganic thermal control coating can be prepared, and the total thickness of the coating is about 115 mu m.
Example 2
The embodiment relates to a high-reflectivity filler, an inorganic thermal control coating thereof and a preparation method thereof.
This embodiment is basically the same as embodiment 1 except that:
preparation of high reflectance filler: respectively weighing nano zinc oxide and neutral silica sol, wherein the dosage ratio is 4:3, and obtaining a mixed solution of the nano zinc oxide and the neutral silica sol through the processes of 1h ultrasonic treatment, high-speed stirring at 350r/min and the like; centrifuging the mixed solution at 7000r/min for 8min, and drying at 110 ℃ for 18h to obtain nanoscale mixed powder; and sintering the dried mixed powder for 2 hours at 800 ℃ to obtain the filler particles with high reflectivity.
Preparing modified high-modulus inorganic potassium silicate resin: mixing a low-modulus potassium silicate solution with neutral silica sol, reacting at 40 ℃ under 1100r/min with the dosage ratio of 1:2, and supplementing deionized water to obtain a high-modulus potassium silicate solution with the mass fraction of 30% and M=4; adding KH560 accounting for 0.4 percent of the total weight to carry out organic modification on the prepared high modulus potassium silicate solution, thus obtaining modified high modulus potassium silicate resin solution.
Preparing a coating: the dosage ratio of the modified high-modulus potassium silicate resin with M=4 to the high-reflectivity filler powder is 10:5, a proper amount of deionized water is added, the mixture is uniformly mixed and stirred, the stirring speed is 800r/min, and the viscosity of the finish paint is 15s.
Preparing a high-reflectivity inorganic thermal control coating: in the process of preparing the coating, spraying the finishing paint, standing for 8 hours, and curing for 18 hours at 80 ℃ to obtain the finishing paint with the thickness of about 110 mu m; spraying a coating layer, namely spraying the modified high-modulus potassium silicate resin solution, standing for 6 hours, and curing for 18 hours at 80 ℃; the high-reflectivity inorganic thermal control coating can be prepared, and the total thickness of the coating is about 130 mu m.
Example 3
The embodiment relates to a high-reflectivity filler, an inorganic thermal control coating thereof and a preparation method thereof.
This embodiment is basically the same as embodiment 1 except that:
preparation of high reflectance filler: respectively weighing a certain amount of nano zinc oxide and alkaline silica sol, wherein the mass ratio is 4:2, and obtaining a mixed solution of the nano zinc oxide and the alkaline silica sol through the processes of 1.5h ultrasonic treatment, 400r/min stirring and the like; centrifuging the mixed solution for 5min at 8000r/min, and drying at 120 ℃ for 12h to obtain nanoscale mixed powder; and sintering the dried mixed powder for 3 hours at the temperature of 1000 ℃ to obtain the filler particles with high reflectivity.
Preparing modified high-modulus inorganic potassium silicate resin: mixing a low-modulus potassium silicate solution with alkaline silica sol at a dosage ratio of 1:3, reacting at 50 ℃ and 1200r/min, and supplementing deionized water to obtain a high-modulus potassium silicate solution with mass fraction of 30% and M=5; adding KH570 accounting for 0.6 percent of the total weight to carry out organic modification on the prepared high modulus potassium silicate solution, thus obtaining modified high modulus potassium silicate resin solution.
Preparing a coating: the dosage ratio of the modified high-modulus potassium silicate resin with M=5 to the high-reflectivity filler powder is 10:7, a proper amount of deionized water is added, the mixture is uniformly mixed and stirred, the stirring speed is 1200r/min, and the viscosity of the finish paint is 16s.
Preparing a high-reflectivity inorganic thermal control coating: in the process of preparing the coating, spraying the finishing paint, standing for 10 hours, and curing for 12 hours at 100 ℃ to obtain the finishing paint with the thickness of about 120 mu m; spraying a coating layer, namely spraying the modified high-modulus potassium silicate resin solution, standing for 10 hours, and curing for 12 hours at 100 ℃; the high-reflectivity inorganic thermal control coating can be prepared, and the total thickness of the coating is about 130 mu m.
Example 4
The embodiment relates to a high-reflectivity filler, an inorganic thermal control coating thereof and a preparation method thereof.
This embodiment is basically the same as embodiment 1 except that:
preparation of high reflectance filler: respectively weighing a certain amount of nano zinc oxide and alkaline silica sol, wherein the mass ratio is 4:4, and obtaining a mixed solution of the nano zinc oxide and the alkaline silica sol through the processes of 2h ultrasonic treatment, 500r/min stirring and the like; centrifuging the mixed solution for 5min at 8000r/min, and drying at 120 ℃ for 12h to obtain nanoscale mixed powder; and sintering the dried mixed powder for 3 hours at 1200 ℃ to obtain the filler particles with high reflectivity.
Preparing modified high-modulus inorganic potassium silicate resin: mixing a low-modulus potassium silicate solution with alkaline silica sol in a dosage ratio of 1:3, and reacting at 60 ℃ under the condition of 1200r/min to obtain a high-modulus potassium silicate solution with modulus M=5; adding KH570 accounting for 0.8 percent of the total weight to carry out organic modification on the prepared high modulus potassium silicate solution, thus obtaining modified high modulus potassium silicate resin solution.
Preparing a coating: the dosage ratio of the modified high-modulus potassium silicate resin with M=5 to the high-reflectivity filler powder is 10:9, a proper amount of deionized water is added, the mixture is uniformly mixed and stirred, the stirring speed is 1200r/min, and the viscosity of the finish paint is 17s.
Preparing a high-reflectivity inorganic thermal control coating: in the process of preparing the coating, spraying the finishing paint, standing for 12 hours, and curing for 12 hours at 100 ℃ so that the thickness of the finishing paint is about 130 mu m; spraying a coating layer, namely spraying the modified high-modulus potassium silicate resin solution, standing for 12 hours, and curing for 12 hours at 100 ℃; the high-reflectivity inorganic thermal control coating can be prepared, and the total thickness of the coating is about 150 mu m.
Comparative example 1
The comparative example relates to a high-reflectivity filler, an inorganic thermal control coating and a preparation method thereof.
This comparative example is basically the same as example 4, except that:
preparing modified high-modulus inorganic potassium silicate resin: mixing a low-modulus potassium silicate solution with alkaline silica sol in a dosage ratio of 1:3, and reacting at 60 ℃ under the condition of 1200r/min to obtain a high-modulus potassium silicate solution with modulus M=5; adding KH570 accounting for 0.8 percent of the total weight to carry out organic modification on the prepared high modulus potassium silicate solution, thus obtaining modified high modulus potassium silicate resin solution.
Preparing a coating: the dosage ratio of the modified high-modulus potassium silicate resin with M=5 to the nano zinc oxide is 10:9, a proper amount of deionized water is added, the mixture is uniformly mixed and stirred, the stirring speed is 1200r/min, and the viscosity of the finish paint is 17s.
Preparing a high-reflectivity inorganic thermal control coating: in the process of preparing the coating, spraying the finishing paint, standing for 12 hours, and curing for 12 hours at 100 ℃ so that the thickness of the finishing paint is about 130 mu m; spraying a coating layer, namely spraying the modified high-modulus potassium silicate resin solution, standing for 12 hours, and curing for 12 hours at 100 ℃; the high-reflectivity inorganic thermal control coating can be prepared, and the total thickness of the coating is about 150 mu m.
Comparative example 2
The comparative example relates to a high-reflectivity filler, an inorganic thermal control coating and a preparation method thereof.
This comparative example is basically the same as example 4, except that:
preparation of high reflectance filler: respectively weighing a certain amount of nano zinc oxide and alkaline silica sol, wherein the mass ratio is 4:4, and obtaining a mixed solution of the nano zinc oxide and the alkaline silica sol through the processes of 2h ultrasonic treatment, 500r/min stirring and the like; centrifuging the mixed solution for 5min at 8000r/min, and drying at 120 ℃ for 12h to obtain nanoscale mixed powder; and sintering the dried mixed powder for 3 hours at 1200 ℃ to obtain the filler particles with high reflectivity.
Preparing modified high-modulus inorganic potassium silicate resin: mixing the low-modulus potassium silicate solution with alkaline silica sol in the dosage ratio of 1:3, and reacting at 60 ℃ under the condition of 1200r/min to obtain the high-modulus potassium silicate solution with modulus M=5.
Preparing a coating: the dosage ratio of the high-modulus potassium silicate resin with M=5 to the high-reflectivity filler powder is 10:9, a proper amount of deionized water is added, the mixture is uniformly mixed and stirred, the stirring speed is 1200r/min, and the viscosity of the finish paint is 17s.
Preparing a high-reflectivity inorganic thermal control coating: in the process of preparing the coating, spraying the finishing paint, standing for 12 hours, and curing for 12 hours at 100 ℃ so that the thickness of the finishing paint is about 130 mu m; spraying a coating layer, namely spraying the modified high-modulus potassium silicate resin solution, standing for 12 hours, and curing for 12 hours at 100 ℃; the high-reflectivity inorganic thermal control coating can be prepared, and the total thickness of the coating is about 150 mu m.
The high reflectivity inorganic thermal control coatings of example 1, example 2, example 3, example 4, comparative example 1 and comparative example 2 above were subjected to performance testing as follows:
coating thickness test
The thickness of the coating was measured using a MiniTest600 thickness gauge manufactured by EPK company, germany. The measurement range is 0-300 μm, and the error is + -2 μm. The thickness of the tested coating is between 110 and 140 mu m, and the requirements of technical indexes of 100 to 150 mu m are met.
Adhesion test
The general specification test requirements of the GJB2704A-2006 spacecraft thermal control coating are met. And (3) tightly attaching the adhesive tape with the peel strength of 2-4N/cm to the middle area of the coating, wherein the distance from the edge is not less than 3mm. One end of the tape was pulled up by hand and the tape was set at 90 ° to the surface. After the tape was pulled slowly (about 5 mm/s) off the surface, the adhesion test results are shown in the following table.
As can be seen from table 1, the silane coupling agent of comparative example 4 and comparative example 2 can significantly improve the adhesion of the coating; comparative examples 1 to 4, the adhesion properties of the coating were gradually improved as the amount of coupling modifier added was increased.
Table 1 coating adhesion rating
Sample numberingExample 1Example 2Example 3Example 4Comparative example 1Comparative example 2
Adhesion rating221002
Solar absorptance test
This test uses an LAMBDA950 ultraviolet-visible-near infrared spectrophotometer (UV/VIS/NIR Spectrophotometer) from America, eimer (Perkin Elmer) to measure the solar absorption ratio of high reflectance inorganic thermal control coatings. The measurable wavelength range is 200nm to 2500nm, the resolution of the instrument is 0.1nm, the bandwidth is less than or equal to 0.05nm, the stray light is less than or equal to 0.00008 percent A, the noise is less than 0.0008A, the photometer repeatability is less than 0.0001A, the baseline drift is less than 0.0002A/h, and the baseline is flat: 0.001A, good stability, high baseline flatness, and extremely low stray light. In the experiment, the step length was set to 5nm and the slit width was set to 4nm.
Hemispherical emissivity test
The hemispherical emissivity of the sample in the 3-35 μm band at room temperature was measured using a TEMP 2000A emissivity measuring instrument developed by AZ techenology corporation, usa, with a measurement accuracy of ±3% and a full band repeatability of ±0.5%.
As can be seen from table 2, in comparative example 4 and comparative example 1, modification of the nano zinc oxide by the silica sol can significantly improve the optical performance of the coating, the solar absorption ratio is significantly reduced (as shown in fig. 3, the reflectance of the coating is improved in the whole band range, especially in the ultraviolet band, the hemispherical emissivity is significantly improved; in comparative examples 1 to 4, as the modification amount of the silica sol to the nano zinc oxide is increased, the optical performance of the coating is gradually improved, the solar absorption ratio is reduced, and the hemispherical emissivity is increased.
TABLE 2 solar absorption and emissivity of the coating
Figure BDA0004026908590000081
Figure BDA0004026908590000093
Volume resistivity test
The volume resistivity of the spacecraft thermal control coating is tested by referring to the standard GB/T1410-2006, and the test conditions are as follows:
test voltage 100V;
TABLE 3 conductivity of coatings
Figure BDA0004026908590000094
Vacuum gassing property test
Vacuum bleed test was performed with reference to standard GJB2704A-2006, under the following conditions:
sample pretreatment: maintaining at 23+ -1deg.C and humidity 45%RH+ -10%RH for 24 hr; the heated temperature of the sample is 125+/-1 ℃; the collection temperature of the condensable volatile is 25 ℃; the test pressure is less than or equal to 7 multiplied by 10-3 Pa; the heat preservation time is 24 hours;
balance test sensitivity: l μg.
Testing to calculate Total Mass Loss (TML), condensable Volatiles (CVCM) of the material in vacuum; as shown in table 3.
TABLE 4 vacuum gassing performance of coatings
Sample numberingExample 1Example 2Example 3Example 4Comparative example 1Comparative example 2
TML0.840.760.720.770.0760.067
CVCM0.0100.0110.0160.0120.0120.013
Thermal cycle testing
The method adopts a temperature impact box (model ZTS010, shanghai up to environmental test equipment Co., ltd.) and under the standard requirement of GJB2704A-2006, the test conditions are as follows after 100 times of thermal cycles at the temperature ranging fromminus 100 ℃ to plus 100 ℃ under the normal atmospheric condition:
test temperature: the high temperature end temperature is-196 ℃, and the low temperature end temperature is-100 ℃; cycling for 100 times; temperature control error: high temperature + -5 ℃ and low temperature + -10 ℃; the thermal cycling device should have two constant temperature zones of different temperatures, with the sample 10s being transferred from one constant temperature zone to the other; preserving heat for 10min at the high temperature and low temperature ends to ensure that the temperature of the test piece is the same as the ambient temperature; dehumidifying measures should be taken during the test to prevent frosting on the surface of the test piece.
The test results of example 4 are shown in fig. 4: the modified coating has good appearance after 100 times of high-temperature heat cycle at-196 ℃ to +100 ℃, stable optical performance and good adhesive force, and meets the technical index requirement.
In combination with table 1, table 2 and test results, the properties of the high reflectivity inorganic thermal control coating of the present invention are as follows:
appearance: white, even coating surface, no bubble, no crack, no peeling and no falling off;
thickness: 100 μm to 150 μm;
solar absorption ratio: 0.08-0.16;
hemispherical emissivity: 0.91-0.92;
the volume resistivity is less than or equal to 1 multiplied by 107 Ω·m
Thermal cycle test: after the coating meets the high-temperature low-temperature heat cycle test for 100 times at the temperature of minus 196 ℃ to plus 100 ℃, the phenomena of cracking, peeling, foaming and color change are avoided, the optical performance is stable, and the adhesive force is good;
vacuum air release performance: all satisfy TML <1%, CVCM <0.1%.
In conclusion, the high-reflectivity inorganic thermal control coating has good coating adhesive force on the basis of ensuring good thermal control performance (solar absorption ratio and hemispherical emissivity) of the coating, is simple and easy to learn in coating construction, has strong feasibility, and has good adhesive force after being subjected to 100-time temperature impact test at-196 ℃ to +100 ℃.
The foregoing describes specific embodiments of the present invention. It is to be understood that the invention is not limited to the particular embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the claims without affecting the spirit of the invention.

Claims (10)

1. A high reflectance filler, characterized in that it is prepared by the steps of: respectively weighing nano zinc oxide and silica sol, and carrying out ultrasonic and high-speed stirring to obtain a mixed solution of the nano zinc oxide and the silica sol; centrifuging and drying to obtain nano-scale mixed powder; sintering to obtain filler particles with high reflectivity.
2. The high reflectance filler according to claim 1, wherein the ratio of nano zinc oxide to 30% silica sol is 4:2-4:5; the ultrasonic treatment is carried out for 0.5 to 2 hours; the high-speed stirring is 300-500r/min.
3. The high reflectance filler according to claim 1, wherein the nano zinc oxide has a particle size of between 30 and 200nm; the silica sol is one or more of acidic silica sol, neutral silica sol and alkaline silica sol.
4. The high-reflectivity filler of claim 1, characterized in that the centrifugation speed is 6000-8000r/min and the centrifugation time is 5-10min; the drying temperature is 100-120 ℃ and the drying time is 12-24 hours; the sintering temperature is 600-1200 ℃ and the sintering time is 1-3h.
5. A method for preparing a high-reflectivity inorganic thermal control coating, which is characterized by comprising the following steps:
s1, preparing modified high-modulus inorganic potassium silicate resin: stirring and reacting low-modulus potassium silicate with silica sol to obtain high-modulus potassium silicate solution; carrying out organic modification on the high-modulus potassium silicate solution by adopting a silane coupling agent to obtain a modified high-modulus potassium silicate resin solution;
s2, preparing a coating: taking the modified high-modulus potassium silicate resin solution as a binder, adding the high-reflectivity filler according to any one of claims 1-4, adding a solvent, and uniformly mixing and stirring to obtain a finish paint;
s3, preparing a high-reflectivity inorganic thermal control coating: spraying the finishing paint on the surface of the base material, standing and solidifying; spraying the modified high-modulus potassium silicate resin solution on the surface of the finish paint to form a covering layer, standing and curing to obtain the high-reflectivity inorganic thermal control coating.
6. The method of producing a high reflectance inorganic thermal control coating according to claim 5, wherein in step S1, the ratio of low modulus potassium silicate to silica sol is 2:2-2:6; the reaction temperature of the stirring reaction is 30-60 ℃, and the stirring speed is 1000-1500r/min; the modulus of the high modulus potassium silicate solution is 3.0-5.0.
7. The method for preparing the high-reflectivity inorganic thermal control coating according to claim 5, wherein in the step S1, the organic modification is to add deionized water into a high-modulus potassium silicate solution to dilute the solution to 30% by mass, and the silane coupling agent accounting for 0.2% -0.8% of the total mass is adopted for mixed modification; the silane coupling agent is one or more of KH550, KH560 and KH 570.
8. The method for preparing a high-reflectivity inorganic thermal control coating according to claim 5, wherein in step S2, the mass ratio of the binder to the filler is 10:3-10:9; the stirring speed of the mixing and stirring is 800-1200 r/min.
9. The method for preparing a high-reflectivity inorganic thermal control coating according to claim 5, wherein deionized water is added as a solvent in step S2; the viscosity of the finish paint measured by the four-viscosity meter is 14-17 s.
10. The method for preparing a high-reflectivity inorganic thermal control coating according to claim 5, wherein in the step S3, the standing time is 6-12 hours, the curing temperature is 60-100 ℃, and the curing time is 12-24 hours; the thickness of the high-reflectivity inorganic thermal control coating is 100-150 mu m.
CN202211728205.2A2022-12-292022-12-29High-reflectivity filler and inorganic thermal control coating thereof and preparation method thereofActiveCN116082877B (en)

Priority Applications (1)

Application NumberPriority DateFiling DateTitle
CN202211728205.2ACN116082877B (en)2022-12-292022-12-29High-reflectivity filler and inorganic thermal control coating thereof and preparation method thereof

Applications Claiming Priority (1)

Application NumberPriority DateFiling DateTitle
CN202211728205.2ACN116082877B (en)2022-12-292022-12-29High-reflectivity filler and inorganic thermal control coating thereof and preparation method thereof

Publications (2)

Publication NumberPublication Date
CN116082877Atrue CN116082877A (en)2023-05-09
CN116082877B CN116082877B (en)2024-04-09

Family

ID=86186321

Family Applications (1)

Application NumberTitlePriority DateFiling Date
CN202211728205.2AActiveCN116082877B (en)2022-12-292022-12-29High-reflectivity filler and inorganic thermal control coating thereof and preparation method thereof

Country Status (1)

CountryLink
CN (1)CN116082877B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication numberPriority datePublication dateAssigneeTitle
CN117126560A (en)*2023-08-242023-11-28上海卫星装备研究所Low-resistance inorganic thermal control coating and preparation method thereof
CN119592110A (en)*2024-12-032025-03-11哈尔滨工业大学SiO prepared based on step-by-step sol-gel method2White dustproof coating of @ ZnO and preparation method thereof

Citations (12)

* Cited by examiner, † Cited by third party
Publication numberPriority datePublication dateAssigneeTitle
JP2013199415A (en)*2012-03-262013-10-03Kyocera CorpCeramic sintered compact, electronic component mounting substrate using the same, and electronic device
CN103421368A (en)*2013-08-222013-12-04武汉武大巨成加固实业有限公司Preparation method of high-modulus potassium silicate inorganic nano-resin
CN104087092A (en)*2014-05-302014-10-08航天材料及工艺研究所Preparation method for aqueous low-solar-absorptance antistatic coating
DE102013009881B3 (en)*2013-06-132014-12-11Ferro Gmbh Process for the preparation of an SiO 2 antireflective coating, SiO 2 antireflective coated substrate and its use
CN106661345A (en)*2014-07-072017-05-10爱尔兰国立大学都柏林大学学院Thermal control coatings
CN106752906A (en)*2016-12-072017-05-31上海卫星装备研究所The preparation method of low-resistivity filler and its antistatic thermal control coating
CN107746590A (en)*2017-09-222018-03-02南京洞见环境科技有限公司A kind of organo-mineral complexing insulating moulding coating and preparation method thereof
CN110804753A (en)*2019-12-042020-02-18中国电子科技集团公司第十二研究所 A kind of preparation method of alloy surface composite thermal control coating
CN110835474A (en)*2019-11-222020-02-25上海卫星装备研究所Low-absorption-ratio pigment particles for star and preparation method thereof
CN111393882A (en)*2020-03-242020-07-10哈尔滨工业大学Ultraviolet radiation resistant low-absorptivity inorganic white thermal control coating and preparation method thereof
CN111763077A (en)*2020-07-102020-10-13天津城建大学 A kind of manufacturing method of alumina ceramic concentrating cavity with high reflectivity
CN113881259A (en)*2021-11-122022-01-04亚士创能科技(上海)股份有限公司Inorganic coating and preparation method and application thereof

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication numberPriority datePublication dateAssigneeTitle
JP2013199415A (en)*2012-03-262013-10-03Kyocera CorpCeramic sintered compact, electronic component mounting substrate using the same, and electronic device
DE102013009881B3 (en)*2013-06-132014-12-11Ferro Gmbh Process for the preparation of an SiO 2 antireflective coating, SiO 2 antireflective coated substrate and its use
CN103421368A (en)*2013-08-222013-12-04武汉武大巨成加固实业有限公司Preparation method of high-modulus potassium silicate inorganic nano-resin
CN104087092A (en)*2014-05-302014-10-08航天材料及工艺研究所Preparation method for aqueous low-solar-absorptance antistatic coating
CN106661345A (en)*2014-07-072017-05-10爱尔兰国立大学都柏林大学学院Thermal control coatings
CN106752906A (en)*2016-12-072017-05-31上海卫星装备研究所The preparation method of low-resistivity filler and its antistatic thermal control coating
CN107746590A (en)*2017-09-222018-03-02南京洞见环境科技有限公司A kind of organo-mineral complexing insulating moulding coating and preparation method thereof
CN110835474A (en)*2019-11-222020-02-25上海卫星装备研究所Low-absorption-ratio pigment particles for star and preparation method thereof
CN110804753A (en)*2019-12-042020-02-18中国电子科技集团公司第十二研究所 A kind of preparation method of alloy surface composite thermal control coating
CN111393882A (en)*2020-03-242020-07-10哈尔滨工业大学Ultraviolet radiation resistant low-absorptivity inorganic white thermal control coating and preparation method thereof
CN111763077A (en)*2020-07-102020-10-13天津城建大学 A kind of manufacturing method of alumina ceramic concentrating cavity with high reflectivity
CN113881259A (en)*2021-11-122022-01-04亚士创能科技(上海)股份有限公司Inorganic coating and preparation method and application thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
JUNGE CHEN等: "Optical properties and radiation stability of SiO2/ZnO composite pigment prepared by co-sintering method", CERAMICS INTERNATIONAL, vol. 48, pages 755*

Cited By (2)

* Cited by examiner, † Cited by third party
Publication numberPriority datePublication dateAssigneeTitle
CN117126560A (en)*2023-08-242023-11-28上海卫星装备研究所Low-resistance inorganic thermal control coating and preparation method thereof
CN119592110A (en)*2024-12-032025-03-11哈尔滨工业大学SiO prepared based on step-by-step sol-gel method2White dustproof coating of @ ZnO and preparation method thereof

Also Published As

Publication numberPublication date
CN116082877B (en)2024-04-09

Similar Documents

PublicationPublication DateTitle
CN116082877B (en)High-reflectivity filler and inorganic thermal control coating thereof and preparation method thereof
Huang et al.Green preparation of a cellulose nanocrystals/polyvinyl alcohol composite superhydrophobic coating
US10647885B2 (en)High performance silicon based coatings
EP3553141B1 (en)Polymer composition having antifreeze and self-cleaning properties
Bhat et al.Low-temperature sintering of highly conductive silver ink for flexible electronics
CN104277713B (en)The preparation method of a kind of POSS cross-linking modified fluorine silicon coating and hydrophobic anti-icing application
Hong et al.Facile one-step fabrication of PHC/PDMS anti-icing coatings with mechanical properties and good durability
US20090136741A1 (en)Nanoscopically modified superhydrophobic coating
Lei et al.Fabrication of durable superhydrophobic coatings with hierarchical structure on inorganic radome materials
CN102807803A (en)Method for preparing organic and inorganic composite super-hydrophobic coatings
KR102481351B1 (en) surface reactivation agent
CN113372815B (en)Preparation method and application of biomass-based super-hydrophobic coating
CN104774510B (en)Antistatic thermal control coating composition, preparation method and applications thereof
CN111808312A (en)Refrigeration film
CN117126560A (en)Low-resistance inorganic thermal control coating and preparation method thereof
CN107353796A (en)A kind of anti-fog coating and preparation method thereof
CN108137944A (en)The highly durable anti-reflection coating containing nano-particle of room temperature curing
KR20080070853A (en)Methods for reducing the time to produce a mar and/or scratch resistant coating on a substrate
KR20200036362A (en)Composition for release layer and release film comprising cured product of the same
CN105111910B (en)A kind of method of the isocyanate component of anionic method synthesis aqueous polyurethane coating with bi component
KR102558640B1 (en)A protective film having a heat-resistant function and a method for manufacturing the same
CN115975491B (en)High-barrier coating for soft-coated aluminum-plastic film of lithium battery and preparation method of high-barrier coating
CN106590221A (en)POSS-modified long life thermal control coating combination and preparation method thereof
CN112280414A (en)High-iron solvent type anti-icing coating in alpine region and production method thereof
JP2025027464A (en) Insert sheet, transfer film, and method for producing insert sheet

Legal Events

DateCodeTitleDescription
PB01Publication
PB01Publication
SE01Entry into force of request for substantive examination
SE01Entry into force of request for substantive examination
GR01Patent grant
GR01Patent grant

[8]ページ先頭

©2009-2025 Movatter.jp