CN114262885B - Preparation method of ultralow-emissivity functional coating - Google Patents
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Abstract
The invention discloses a preparation method of an ultralow-emissivity functional coating, which comprises the following steps: (1) pretreatment; (2) chemical oxidation; (3) cleaning with clean water; (4) post-treatment; (5) hot water washing; (6) drying. The preparation process and parameters of the antenna surface coating are that the antenna is pretreated, chemically oxidized and post-treated to obtain the coating on the surface of the antenna, then the surface emissivity test and salt spray resistance test are carried out on the antenna coated with the coating, the surface emissivity is tested to be 0.06+/-0.02, the surface of the antenna is not obviously corroded after the salt spray resistance test time is 96 hours, the design requirements of high-precision ultralow emissivity and neutral salt spray resistance can be simultaneously realized, and the ground protection problem of satellite products to be transmitted and the space thermal control problem after the transmission lift-off in the sea environment are ensured.
Description
Technical Field
The invention relates to the technical field of surface engineering application, in particular to a preparation method of an ultralow-emissivity functional coating.
Background
The conventional aluminum alloy material has hemispherical emissivity of about 0.20 due to natural oxidation of the surface, has poor corrosion resistance in ground storage, and has a neutral salt spray resistance test of less than 24 hours. At present, the thermal control coating prepared by domestic methods such as organic white paint, OSR, flexible thermal control coating, aluminum alloy anodic oxidation and the like can only meet the requirement of higher hemispherical emissivity (epsilon) H 0.70 or more). Patent CN106099355A discloses a film sticking method for an aluminum alloy crack waveguide, which describes that the aluminum alloy crack waveguide is also called a crack source, and is a key piece in telecommunication, structure and process in a crack waveguide array antenna, and the design of the aluminum alloy crack waveguide antenna requires that a coating layer has ultra-low emissivity (epsilon) H Less than 0.10), and simultaneously has the function of salt fog prevention for the ground storage of coastal environment.
The aluminum alloy chemical coating is a layer of inorganic coating material generated by chemical reaction on the surface of a substrate by a chemical method, a chemical oxidation method is adopted on satellites of a certain model in China, the thermal control development of a crack waveguide antenna is carried out, the hemispherical emissivity of the obtained coating is low and is 0.12-0.13, the solar absorption ratio is high and reaches 0.35-0.40, and the requirements of low emissivity and low specific heat absorption control performance cannot be met at the same time.
Because of the special processing characteristics of the slot waveguide antenna and the multi-cavity multi-layer multi-slot complex structure form, the methods of pasting an OSR, vacuum coating, wrapping a flexible thermal control coating and the like are difficult to implement, even can not meet the communication function, and limit the use of the thermal control coating technology. Therefore, developing the ultra-low emissivity multifunctional coating of the slot waveguide antenna is an important difficult problem and key task to be solved for realizing the space thermal control and electrical performance requirements of the slot waveguide antenna and the multifunctional requirements of salt fog prevention and the like of the sea area environment storage.
Disclosure of Invention
The invention aims to solve the technical problems of space thermal control, ground protection, electrical performance and other functional requirements of a slot waveguide antenna.
The invention solves the technical problems by the following technical means:
a preparation method of an ultralow-emissivity functional coating comprises the following steps:
(1) Pretreatment of
a. Acid etching: placing the antenna into an acid etching solution, and performing acid etching treatment at 70-80 ℃ for 3-5min, wherein the acid etching solution comprises the following formula: sulfuric acid (H) 2 SO 4 ) 100-120mL/L chromic anhydride (CrO) 3 )30-40g/L；
b. And (3) cleaning: taking out the antenna subjected to acid etching treatment in the step a, and then cleaning by using flowing tap water;
c. alkali etching: c, placing the antenna washed in the step b into an alkaline etching solution, and performing alkaline etching treatment at the temperature of 60-70 ℃ for 10-60 seconds, wherein the alkaline etching solution comprises the following formula: 10-20g/L sodium hydroxide (NaOH), sodium carbonate (Na) 2 CO 3 ) 30-40g/L sodium phosphate (Na) 3 PO 4 )40-50g/L；
d, washing with clear water: taking out the antenna subjected to the alkali etching treatment in the step c, and then cleaning by using flowing tap water;
e. and (3) light emitting: and d, placing the antenna washed in the step d into a light-emitting liquid for light-emitting treatment, wherein the light-emitting temperature is 10-30 ℃, the light-emitting time is 5-15s, and the formula of the light-emitting liquid is as follows: HNO (HNO) 3 :H 2 SO 4 :HF＝60:35:5(V:V:V)；
f. And (3) cleaning: taking out the antenna subjected to the light-emitting treatment in the step e, and then cleaning by using flowing tap water;
(2) Chemical oxidation
Placing the pretreated antenna into a chemical oxidation solution for oxidation; the chemical oxidation process formula comprises the following steps: 10-20g/L phosphoric acid (H) 3 PO 4 ) 1-2g/L diammonium phosphate (NH) 4 ) 2 HPO 4 2-4g/L sodium chromate (Na) 2 CrO 4 ) 1-3g/L boric acid (H) 3 BO 3 ) 2-5g/L tannic acid; the oxidation parameters are: pH is 2-4.5, temperature is 25-35 ℃, and time is 2-8min;
(3) Cleaning with water
Placing the antenna subjected to the chemical oxidation treatment in the step (2) into flowing tap water for cleaning;
(4) Post-treatment
Placing the antenna washed by the clean water in the step (3) into a post-treatment solution, and treating the antenna at 25-35 ℃ for 30-60s, wherein the post-treatment solution is chromic anhydride (CrO) with the concentration of 5-10g/L 3 )；
(5) Hot water washing
Putting the processed antenna into hot water for cleaning;
(6) Drying
And (3) drying the antenna washed by the hot water on the upper surface of a blower, and then putting the antenna into an oven to dry the whole antenna.
The preparation process and parameters of the antenna surface coating are that the antenna is pretreated, chemically oxidized and post-treated to obtain the coating on the surface of the antenna, then the surface emissivity test and salt spray resistance test are carried out on the antenna coated with the coating, the surface emissivity is tested to be 0.06+/-0.02, the surface of the antenna is not obviously corroded after the salt spray resistance test time is 96 hours, the design requirements of high-precision ultralow emissivity and neutral salt spray resistance can be simultaneously realized, and the ground protection problem of satellite products to be transmitted and the space thermal control problem after the transmission lift-off in the sea environment are ensured.
Preferably, the washing time in the step b is 10-60s.
Preferably, the washing time in the step d is 10-60s.
Preferably, the cleaning time in the step f is 10-60s.
Preferably, the washing time in the step (3) is 10-30s.
Preferably, the temperature of the hot water in the step (5) is 45-55 ℃.
Preferably, the hot water cleaning time in the step (5) is 10-30s.
Preferably, the temperature of the drying in the step (6) is 45-55 ℃ and the drying time is 10-12h.
Preferably, the method further comprises the following steps: the surface emissivity epsilon of an antenna which had been completely dried and cooled was tested H Performing tolerationSalt spray test.
Preferably, the salt spray resistance test method is performed as specified by NSS in GJB150.11A.
The invention has the following beneficial effects:
1. the preparation process and parameters of the antenna surface coating are that the antenna is pretreated, chemically oxidized and post-treated to obtain the coating on the surface of the antenna, then the surface emissivity test and salt spray resistance test are carried out on the antenna coated with the coating, the surface emissivity is tested to be 0.06+/-0.02, the surface of the antenna is not obviously corroded after the salt spray resistance test time is 96 hours, the design requirements of high-precision ultralow emissivity and neutral salt spray resistance can be simultaneously realized, and the ground protection problem of satellite products to be transmitted and the space thermal control problem after the transmission lift-off in the sea environment are ensured.
2. The coating obtained on the surface of the antenna is subjected to a space-resistant atomic oxygen simulation acceleration identification test, and after the test, the coating is free from phenomena such as falling, skinning, color change and the like, the index change is less than +/-0.02, and the space performance is stable.
3. The method of the invention has been applied to sea wire 01-04 star, WWB015 and other multi-type satellites, and realizes the engineering practice of preparing the surface coating of a plurality of batches of antennas, thereby solving the difficult problem of preparing the multifunctional coating of the on-board SAR antenna
Drawings
FIG. 1 is a surface micro-topography of an antenna with a surface-coating obtained in example 1 of the present invention after a high temperature heat treatment under specific conditions;
FIG. 2 is a photograph showing the appearance of an antenna having a surface obtained coating layer obtained in example 1 according to the present invention after 96 hours of salt spray resistance test;
FIG. 3 is a photograph showing the appearance of a conventional aluminum alloy sample according to the comparative example of the present invention after 24 hours of salt spray resistance test.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings and the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The test materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
Those of skill in the art, without any particular mention of the techniques or conditions, may follow the techniques or conditions described in the literature in this field or follow the product specifications.
Example 1
A preparation method of an ultralow-emissivity functional coating comprises the following steps:
(1) Pretreatment of
a. Acid etching: the antenna is put into acid etching solution, and acid etching treatment is carried out for 4min at the temperature of 73 ℃, wherein the formula of the acid etching solution is as follows: sulfuric acid (H) 2 SO 4 ) 110mL/L, chromic anhydride (CrO) 3 )30g/L；
b. And (3) cleaning: taking out the antenna subjected to acid etching treatment in the step a, and then cleaning the antenna for 30s by using flowing tap water;
c. alkali etching: c, placing the antenna washed in the step b into an alkaline etching solution, and performing alkaline etching treatment at the temperature of 62 ℃ for 48 seconds, wherein the alkaline etching solution comprises the following formula: 12g/L sodium hydroxide (NaOH), sodium carbonate (Na) 2 CO 3 ) 36g/L, sodium phosphate (Na) 3 PO 4 )48g/L；
d, washing with clear water: taking out the antenna subjected to the alkali etching treatment in the step c, and then cleaning the antenna for 30s by using flowing tap water;
e. and (3) light emitting: and d, placing the antenna washed in the step in a light-emitting liquid for light-emitting treatment, wherein the light-emitting temperature is 15 ℃, the light-emitting time is 10s, and the formula of the light-emitting liquid is as follows: HNO (HNO) 3 :H 2 SO 4 :HF＝60:35:5(V:V:V)；
f. And (3) cleaning: taking out the antenna subjected to the light-emitting treatment in the step e, and then cleaning the antenna for 40s by using flowing tap water;
(2) Chemical oxidation
Placing the pretreated antennaOxidizing in a chemical oxidizing solution; the chemical oxidation process formula comprises the following steps: 12g/L phosphoric acid (H) 3 PO 4 ) 1.5g/L diammonium hydrogen phosphate (NH) 4 ) 2 HPO 4 3g/L sodium chromate (Na) 2 CrO 4 ) 2g/L boric acid (H) 3 BO 3 ) 5g/L tannic acid; the oxidation parameters are: pH 2.5, temperature 30 ℃ and time 5min;
(3) Cleaning with water
Placing the antenna subjected to the chemical oxidation treatment in the step (3) into flowing tap water for cleaning for 30s;
(4) Post-treatment
Placing the antenna washed by the clean water in the step (4) into a post-treatment solution, and treating the antenna at 30 ℃ for 40s, wherein the post-treatment solution is chromic anhydride (CrO) with the concentration of 6g/L 3 )；
(5) Hot water washing
Putting the treated antenna into hot water for cleaning, wherein the temperature of the hot water is 51 ℃, and the cleaning time is 30s;
(6) Drying
And (3) drying the antenna after hot water washing on the upper surface of a blower, and then placing the antenna into an oven to dry the whole antenna completely, wherein the drying temperature is 50-55 ℃ and the drying time is 10 hours.
The surface emissivity epsilon of the antenna with the surface obtained coating prepared in this example was tested H 0.05.
The antenna with the surface obtained coating prepared in this example was subjected to high temperature treatment under specific conditions, and then the antenna after the high temperature treatment was subjected to SEM electron microscopy analysis, and the analysis results are shown in fig. 1.
Salt spray resistance test was performed on the prepared antenna with the surface obtained coating: the test method is carried out according to NSS in GJB150.11A, and the appearance picture after 24 hours of test time is shown in figure 2, so that no obvious corrosion on the antenna surface can be seen, and after the test time is up to 96 hours, no obvious corrosion on the antenna surface can be detected.
Example 2
A preparation method of an ultralow-emissivity functional coating comprises the following steps:
(1) Pretreatment of
a. Acid etching: the antenna is put into acid etching solution, and acid etching treatment is carried out for 3min at the temperature of 75 ℃, wherein the formula of the acid etching solution is as follows: sulfuric acid (H) 2 SO 4 ) 120mL/L, chromic anhydride (CrO) 3 )40g/L；
b. And (3) cleaning: taking out the antenna subjected to acid etching treatment in the step a, and then cleaning the antenna for 30s by using flowing tap water;
c. alkali etching: c, placing the antenna washed in the step b into an alkaline etching solution, and performing alkaline etching treatment at the temperature of 65 ℃ for 50 seconds, wherein the alkaline etching solution comprises the following formula: sodium hydroxide (NaOH) 18g/L, sodium carbonate (Na) 2 CO 3 ) 34g/L, sodium phosphate (Na) 3 PO 4 )45g/L；
d, washing with clear water: taking out the antenna subjected to the alkali etching treatment in the step c, and then cleaning the antenna for 30s by using flowing tap water;
e. and (3) light emitting: and d, placing the antenna washed in the step in a light-emitting liquid for light-emitting treatment, wherein the light-emitting temperature is 15 ℃, the light-emitting time is 10s, and the formula of the light-emitting liquid is as follows: HNO (HNO) 3 :H 2 SO 4 :HF＝60:35:5(V:V:V)；
f. And (3) cleaning: taking out the antenna subjected to the light-emitting treatment in the step e, and then cleaning the antenna for 30s by using flowing tap water;
(2) Chemical oxidation
Placing the pretreated antenna into a chemical oxidation solution for oxidation; the chemical oxidation process formula comprises the following steps: 10g/L phosphoric acid (H) 3 PO 4 ) 1.2g/L diammonium phosphate (NH) 4 ) 2 HPO 4 2.4g/L sodium chromate (Na) 2 CrO 4 ) 1.8g/L boric acid (H) 3 BO 3 ) 2.5g/L tannic acid; the oxidation parameters are: pH 3.5, temperature 28 ℃ and time 6min;
(3) Cleaning with water
Placing the antenna subjected to the chemical oxidation treatment in the step (3) into flowing tap water to be cleaned for 50s;
(4) Post-treatment
Placing the antenna washed by the clean water in the step (4) into a post-treatment solution, and treating the antenna at 25 ℃ for 45 seconds, wherein the post-treatment solution is chromic anhydride (CrO) with the concentration of 7g/L 3 )；
(5) Hot water washing
Placing the treated antenna into hot water for cleaning, wherein the temperature of the hot water is 50 ℃, and the cleaning time is 20s;
(6) Drying
And (3) drying the antenna after hot water washing on the upper surface of a blower, and then placing the antenna into an oven to dry the whole antenna completely, wherein the drying temperature is 50-55 ℃ and the drying time is 12 hours.
The surface emissivity epsilon of the antenna with the surface obtained coating prepared in this example was tested H 0.06.
Salt spray resistance test was performed on the prepared antenna with the surface obtained coating: the test method is carried out according to the NSS in GJB150.11A, the test time is 96 hours, and the surface of the antenna is checked to have no obvious corrosion after the test.
Example 3
A preparation method of an ultralow-emissivity functional coating comprises the following steps:
(1) Pretreatment of
a. Acid etching: the antenna is put into acid etching solution, and acid etching treatment is carried out for 5min at the temperature of 78 ℃, wherein the formula of the acid etching solution is as follows: sulfuric acid (H) 2 SO 4 ) 100mL/L, chromic anhydride (CrO) 3 )30g/L；
b. And (3) cleaning: taking out the antenna subjected to acid etching treatment in the step a, and then cleaning the antenna for 30s by using flowing tap water;
c. alkali etching: c, placing the antenna washed in the step b into an alkaline etching solution, and performing alkaline etching treatment at 68 ℃ for 40 seconds, wherein the alkaline etching solution comprises the following formula: sodium hydroxide (NaOH) 16g/L, sodium carbonate (Na 2 CO 3 ) 36g/L, sodium phosphate (Na) 3 PO 4 )47g/L；
d, washing with clear water: taking out the antenna subjected to the alkali etching treatment in the step c, and then cleaning the antenna for 30s by using flowing tap water;
e. and (3) light emitting: and d, placing the antenna washed in the step in a light-emitting liquid for light-emitting treatment, wherein the light-emitting temperature is 25 ℃, the light-emitting time is 20s, and the formula of the light-emitting liquid is as follows: HNO (HNO) 3 :H 2 SO 4 :HF＝60:35:5(V:V:V)；
f. And (3) cleaning: taking out the antenna subjected to the light-emitting treatment in the step e, and then cleaning the antenna for 30s by using flowing tap water;
(2) Chemical oxidation
Placing the pretreated antenna into a chemical oxidation solution for oxidation; the chemical oxidation process formula comprises the following steps: 17g/L phosphoric acid (H) 3 PO 4 ) 1.6g/L diammonium hydrogen phosphate (NH) 4 ) 2 HPO 4 3g/L sodium chromate (Na) 2 CrO 4 ) 3g/L boric acid (H) 3 BO 3 ) 4g/L tannic acid; the oxidation parameters are: pH 4, temperature 32 ℃ and time 6min;
(3) Cleaning with water
Placing the antenna subjected to the chemical oxidation treatment in the step (3) into flowing tap water to be cleaned for 50s;
(4) Post-treatment
Placing the antenna washed by the clean water in the step (4) into a post-treatment solution, and treating the antenna at 28 ℃ for 50s, wherein the post-treatment solution is chromic anhydride (CrO) with the concentration of 6g/L 3 )；
(5) Hot water washing
Putting the treated antenna into hot water for cleaning, wherein the temperature of the hot water is 55 ℃, and the cleaning time is 25s;
(6) Drying
And (3) drying the antenna after hot water washing on the upper surface of a blower, and then placing the antenna into an oven to dry the whole antenna completely, wherein the drying temperature is 50-55 ℃ and the drying time is 12 hours.
The surface emissivity epsilon of the antenna with the surface obtained coating prepared in this example was tested H 0.05.
Salt spray resistance test was performed on the prepared antenna with the surface obtained coating: the test method is carried out according to the NSS in GJB150.11A, the test time is 96 hours, and the surface of the antenna is checked to have no obvious corrosion after the test.
Comparative example
The comparative example is an existing aluminum alloy sample purchased in the market, the aluminum alloy sample is subjected to a salt spray resistance test, the test method is carried out according to the NSS specification in GJB150.11A, the appearance picture after the test time is 24 hours is shown in fig. 3, and it can be seen that the surface of the existing aluminum alloy sample purchased in the market is corroded.
In summary, the preparation process and parameters of the antenna surface coating designed by the invention are that the antenna is pretreated, chemically oxidized and post-treated to obtain the coating on the surface of the antenna, then the surface emissivity test and salt spray resistance test are carried out on the antenna coated with the coating, the surface emissivity is tested to be 0.06+/-0.02, the salt spray resistance test time is 96 hours, the surface of the antenna is not obviously corroded, the design requirements of high-precision ultralow emissivity and neutral salt spray resistance can be simultaneously realized, and the ground protection problem of satellite products to be transmitted and the space thermal control problem after the transmission lift-off under the sea area environment are ensured.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. The preparation method of the ultra-low emissivity functional coating is characterized by comprising the following steps of:
(1) Pretreatment of
a. Acid etching: placing the antenna into an acid etching solution, and performing acid etching treatment at 70-80 ℃ for 3-5min, wherein the acid etching solution comprises the following formula: 100-120mL/L sulfuric acid and 30-40g/L chromic anhydride;
b. and (3) cleaning: taking out the antenna subjected to acid etching treatment in the step a, and then cleaning by using flowing tap water;
c. alkali etching: c, placing the antenna washed in the step b into an alkaline etching solution, and performing alkaline etching treatment at the temperature of 60-70 ℃ for 10-60 seconds, wherein the alkaline etching solution comprises the following formula: 10-20g/L of sodium hydroxide, 30-40g/L of sodium carbonate and 40-50g/L of sodium phosphate;
d, washing with clear water: taking out the antenna subjected to the alkali etching treatment in the step c, and then cleaning by using flowing tap water;
e. and (3) light emitting: and d, placing the washed antenna in the step D into a light-emitting liquid for light-emitting treatment, wherein the light-emitting temperature is 10-30 ℃, the light-emitting time is 5-15s, and the formula of the light-emitting liquid is as follows: HNO (HNO) 3 :H 2 SO 4 :HF/v:v:v＝60:35:5；
f. And (3) cleaning: taking out the antenna subjected to the light-emitting treatment in the step e, and then cleaning by using flowing tap water;
(2) Chemical oxidation
Placing the pretreated antenna into a chemical oxidation solution for oxidation; the chemical oxidation process formula comprises the following steps: 10-20g/L phosphoric acid, 1-2g/L diammonium hydrogen phosphate, 2-4g/L sodium chromate, 1-3g/L boric acid and 2-5g/L tannic acid; the oxidation parameters are: pH is 2-4.5, temperature is 25-35 ℃, and time is 2-8min;
(3) Cleaning with water
Placing the antenna subjected to the chemical oxidation treatment in the step (2) into flowing tap water for cleaning;
(4) Post-treatment
Placing the antenna washed by the clean water in the step (3) into a post-treatment solution, and treating the antenna at 25-35 ℃ for 30-60s, wherein the post-treatment solution is chromic anhydride (CrO) with the concentration of 5-10g/L 3 )；
(5) Hot water washing
Putting the processed antenna into hot water for cleaning;
(6) Drying
And (3) drying the antenna washed by the hot water on the upper surface of a blower, and then putting the antenna into an oven to dry the whole antenna.
2. The method for preparing the ultra-low emissivity functional coating of claim 1, wherein the method comprises the steps of: the cleaning time in the step b is 10-60s.
3. The method for preparing the ultra-low emissivity functional coating of claim 1, wherein the method comprises the steps of: the cleaning time in the step d is 10-60s.
4. The method for preparing the ultra-low emissivity functional coating of claim 1, wherein the method comprises the steps of: the cleaning time in the step f is 10-60s.
5. The method for preparing the ultra-low emissivity functional coating of claim 1, wherein the method comprises the steps of: the cleaning time in the step (3) is 10-30s.
6. The method for preparing the ultra-low emissivity functional coating of claim 1, wherein the method comprises the steps of: the temperature of the hot water in the step (5) is 45-55 ℃.
7. The method for preparing the ultra-low emissivity functional coating of claim 1, wherein the method comprises the steps of: and (5) cleaning the hot water in the step (5) for 10-30s.
8. The method for preparing the ultra-low emissivity functional coating of claim 1, wherein the method comprises the steps of: the drying temperature in the step (6) is 45-55 ℃.
9. The method for preparing the ultra-low emissivity functional coating of claim 1, wherein the method comprises the steps of: the method also comprises the following steps: the surface emissivity epsilon of an antenna which had been completely dried and cooled was tested H And (5) performing a salt spray resistance test.
10. The method for preparing the ultra-low emissivity functional coating of claim 9, wherein the method comprises the steps of: the salt spray resistance test method was performed as specified by NSS in GJB150.11A.
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