CN113348745B - Quartz-based composite material surface composite coating and preparation method thereof - Google Patents
Quartz-based composite material surface composite coating and preparation method thereof Download PDFInfo
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- CN113348745B CN113348745B CN201418002241.0A CN201418002241A CN113348745B CN 113348745 B CN113348745 B CN 113348745B CN 201418002241 A CN201418002241 A CN 201418002241A CN 113348745 B CN113348745 B CN 113348745B
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Abstract
The invention belongs to the technical field of special functional ceramics, and relates to a composite coating on the surface of a quartz-based composite material and a preparation method thereof. The invention takes perhydropolysilazane as a precursor, so that the perhydropolysilazane is converted into a compact hole sealing layer which takes silicon dioxide as a main component and has stronger water, gas and oil resistance effects under certain conditions, thereby achieving good moisture-proof effect; a layer of organic silicon resin is further coated outside the hole sealing layer, so that double moisture-proof effects are achieved; thereby playing a great role in delaying the surface roughness damage and the wave-transmitting performance deterioration of the quartz fiber reinforced quartz-based composite material. The invention takes the product of the perhydropolysilazane as the hole sealing layer, not only has obvious water and gas blocking effect, but also has good bonding property with the substrate and the surface layer of the quartz-based composite material, and has very little influence on the dielectric property of the quartz-based composite material.
Description
Technical Field
The invention belongs to the technical field of special functional ceramics, and relates to a quartz-based composite material surface composite coating and a preparation method thereof.
Background
The continuous development of aerospace technology also puts higher and higher requirements on the performance of wave-transparent materials, and the ceramic material with a single component cannot meet the use conditions due to inherent defects (such as low toughness, high brittleness and the like), so the research of inorganic fiber fabric composite materials becomes a necessary trend. At present, the fibers used as the reinforced fabric mainly comprise quartz fibers, alumina fibers, boron nitride fibers and the like, and the composite materials of the quartz fibers, the alumina fibers, the boron nitride fibers and the like are widely used in a plurality of aviation and aerospace engineering parts such as a nose cone, a heat-proof layer, an antenna window, an antenna housing and the like in sequence.
The quartz fiber reinforced quartz-based composite material (hereinafter referred to as quartz-based composite material) overcomes the brittleness of simple substance ceramic, has higher toughness and has wide application prospect in the field of aerospace. However, the quartz fiber reinforced quartz-based composite material product has high porosity, is not compact, has low surface hardness, and has poor capability of bearing rain erosion and air flow scouring in the using process, thereby causing surface erosion and causing the surface to be rough and damaged. Meanwhile, the product absorbs moisture in the long-term storage process, so that the wave-transmitting performance of the quartz fiber reinforced quartz-based composite material is deteriorated.
Disclosure of Invention
The technical problem to be solved by the invention is to provide the quartz-based composite material surface composite coating and the preparation method thereof, which can improve the moisture resistance of the quartz-based composite material surface and delay the rough damage and wave-transmitting performance deterioration of the quartz-based composite material surface.
In order to solve the technical problem, the composite coating on the surface of the quartz-based composite material sequentially comprises a first hole sealing slurry, a second hole sealing slurry and a surface coating solution from inside to outside from the surface of the quartz-based composite material;
wherein: the first hole sealing slurry is prepared by mixing perhydropolysilazane and quartz powder, wherein the mass percent of the perhydropolysilazane is 30-60%, and the mass percent of the quartz powder is 40-70%;
the second hole sealing slurry is prepared by mixing perhydropolysilazane and n-butyl ether, wherein the mass percent of the perhydropolysilazane is 20-40%, and the mass percent of the n-butyl ether is 60-80%;
the surface coating liquid is prepared by mixing organic silicon resin and xylene, wherein the mass percent of the organic silicon resin is 30-60%, and the mass percent of the xylene is 40-70%.
A preparation method of a quartz-based composite material surface composite coating comprises the following steps:
coating the first hole sealing slurry on the surface of a quartz-based composite material, drying at room temperature, curing, and performing primary hole sealing;
coating the second hole sealing slurry on the surface of the first hole sealing slurry, and curing at 200 ℃ in a constant-temperature constant-humidity drying box;
coating surface coating liquid on the surface of the second hole sealing slurry, and curing at 200 ℃ in a constant-temperature constant-humidity drying oven;
the first hole sealing slurry is prepared by mixing perhydropolysilazane and quartz powder, wherein the mass percent of the perhydropolysilazane is 30-60%, and the mass percent of the quartz powder is 40-70%;
the second hole sealing slurry is prepared by mixing perhydropolysilazane and n-butyl ether, wherein the mass percent of the perhydropolysilazane is 20-40%, and the mass percent of the n-butyl ether is 60-80%;
the surface coating liquid is prepared by mixing organic silicon resin and xylene, wherein the mass percent of the organic silicon resin is 30-60%, and the mass percent of the xylene is 40-70%.
Further, before the surface of the quartz-based composite material is coated with the first hole sealing slurry, a quartz-based composite material substrate is pretreated: and placing the quartz-based composite material substrate in a constant-temperature constant-humidity drying box for 4-5 hours at the temperature of 100-120 ℃.
Further, in the second step of the preparation method, the second hole sealing slurry is coated on the surface of the first hole sealing slurry, and after curing is carried out in a constant temperature and humidity drying box at 200 ℃ for 45-120 minutes, the second hole sealing slurry is slowly cooled to room temperature.
In the third step of the preparation method, the surface coating liquid is coated on the surface of the second hole sealing slurry, and after curing is carried out in a constant temperature and humidity drying oven at 200 ℃ for 45-120 minutes, the second hole sealing slurry is cooled to room temperature.
Further, placing the perhydropolysilazane solution and the quartz powder on a magnetic stirrer, and stirring for 3-5 min to prepare uniform first hole sealing slurry, wherein the content of perhydropolysilazane in the perhydropolysilazane solution is more than or equal to 25.0%.
Further, placing the perhydropolysilazane solution and n-butyl ether on a magnetic stirrer, and stirring for 3-5 min to prepare uniform second hole sealing slurry, wherein the content of perhydropolysilazane in the perhydropolysilazane solution is more than or equal to 25.0%.
Further, the organic silicon resin and the dimethylbenzene are placed on a magnetic stirrer and stirred for 3-5 min, and the uniform surface coating liquid is prepared.
The invention takes perhydropolysilazane as a precursor, so that the perhydropolysilazane is converted into a compact hole sealing layer which takes silicon dioxide as a main component and has stronger water, gas and oil resistance effects under certain conditions, thereby achieving good moisture-proof effect; a layer of organic silicon resin is further coated outside the hole sealing layer, so that double moisture-proof effects are achieved; thereby playing a great role in delaying the surface roughness damage and the wave-transmitting performance deterioration of the quartz fiber reinforced quartz-based composite material. The invention takes the product of the perhydropolysilazane as the hole sealing layer, not only has obvious water and gas blocking effect, but also has good bonding property with the substrate and the surface layer of the quartz-based composite material, and has very little influence on the dielectric property of the quartz-based composite material.
Drawings
FIG. 1 is a flow chart of a method for preparing a composite coating on the surface of a quartz-based composite material.
Detailed Description
With reference to fig. 1, a method for preparing a composite coating on the surface of a quartz-based composite material includes the following steps:
coating the first hole sealing slurry on the surface of a quartz-based composite material, drying at room temperature, curing, and performing primary hole sealing;
coating the second hole sealing slurry on the surface of the first hole sealing slurry, and curing at 200 ℃ in a constant-temperature constant-humidity drying box;
coating surface coating liquid on the surface of the second hole sealing slurry, and curing at 200 ℃ in a constant-temperature constant-humidity drying oven;
the first hole sealing slurry is prepared by mixing perhydropolysilazane and quartz powder, wherein the mass percent of the perhydropolysilazane is 30-60%, and the mass percent of the quartz powder is 40-70%;
the second hole sealing slurry is prepared by mixing perhydropolysilazane and n-butyl ether, wherein the mass percent of the perhydropolysilazane is 20-40%, and the mass percent of the n-butyl ether is 60-80%;
the surface coating liquid is prepared by mixing organic silicon resin and xylene, wherein the mass percent of the organic silicon resin is 30-60%, and the mass percent of the xylene is 40-70%.
The preparation method and the beneficial effects of the invention are illustrated by the following specific examples:
example 1
Firstly, matrix pretreatment: the quartz-based composite material substrate is placed in a constant temperature and humidity drying box and is placed for 4 hours at the temperature of 120 ℃.
Step two, preparing the components of the composite coating:
a, preparing first hole sealing slurry: 24g of perhydropolysilazane solution with the perhydropolysilazane content of 25.0% and 14g of quartz powder were stirred on a magnetic stirrer for 3min to be uniformly mixed, and the first hole sealing slurry was prepared.
b, preparing second hole sealing slurry: 20g of perhydropolysilazane solution with the perhydropolysilazane content of 25.0% and 20g of n-butyl ether were stirred for 3min on a magnetic stirrer to be uniformly mixed, and second hole sealing slurry was prepared.
c, preparing a surface coating liquid: 6g of organic silicon resin and 14g of dimethylbenzene are weighed and stirred for 3min on a magnetic stirrer to be uniformly mixed, so that the surface coating liquid is prepared.
Step three, a coating process:
coating the first hole sealing slurry on the surface of a quartz-based composite material by adopting a brushing process, drying at room temperature for 30min, curing, and performing primary hole sealing;
and b, coating the second hole sealing slurry on the surface of the first hole sealing slurry, and curing for 1h at 200 ℃ in a constant-temperature constant-humidity drying box to obtain a hole sealing layer.
c, coating surface coating liquid on the surface of the second hole sealing slurry, and curing for 1h at 200 ℃ in a constant-temperature constant-humidity drying oven to obtain the composite coating.
And (3) carrying out effect inspection on the composite coating prepared by the process.
And (3) testing results: the thickness of the composite coating is 4 microns, the composite coating is placed in a constant temperature and humidity box with the temperature of 60 ℃ and the relative humidity of 90% for 72 hours, the weight of the composite coating is increased by 1.976%, the hardness of the composite coating is 5H, the adhesive force grade is 1 grade, the dielectric constant is 3.02, and the requirements of the wave-transmitting materials for aviation and aerospace on the moisture-proof coating are met.
Example 2
Firstly, matrix pretreatment: the quartz-based composite material substrate is placed in a constant temperature and humidity drying box and is placed for 5 hours at the temperature of 100 ℃.
Step two, preparing the components of the composite coating:
a, preparing first hole sealing slurry: taking 16g of perhydropolysilazane solution with the perhydropolysilazane content of 50.0% and 12g of quartz powder, stirring for 3min on a magnetic stirrer, and uniformly mixing to obtain first hole sealing slurry.
b, preparing second hole sealing slurry: and (3) stirring 24g of perhydropolysilazane solution with the perhydropolysilazane content of 50.0% and 18g of n-butyl ether on a magnetic stirrer for 5min to uniformly mix to prepare second hole sealing slurry.
c, preparing a surface coating liquid: 6g of organic silicon resin and 12g of dimethylbenzene are weighed and stirred for 3min on a magnetic stirrer to be uniformly mixed, so that the surface coating liquid is prepared.
Step three, a coating process:
coating the first hole sealing slurry on the surface of the quartz-based composite material by adopting a brushing process, drying at room temperature for 45min, curing, and performing primary hole sealing;
and b, coating the second hole sealing slurry on the surface of the first hole sealing slurry, and curing for 90min at 200 ℃ in a constant-temperature constant-humidity drying box to obtain a hole sealing layer.
c, coating surface coating liquid on the surface of the second hole sealing slurry, and curing for 45min at 200 ℃ in a constant-temperature constant-humidity drying oven to obtain the composite coating.
And (3) carrying out effect inspection on the composite coating prepared by the process.
And (3) testing results: the thickness of the composite coating is 3 microns, the composite coating is placed in a constant temperature and humidity box with the temperature of 60 ℃ and the relative humidity of 90% for 72 hours, the weight gain is 2.101%, the hardness of the composite coating is 5H, the adhesive force grade is 1 grade, the dielectric constant is 2.97, and the requirements of aviation and aerospace wave-transmitting materials on moisture-proof coatings are met.
Example 3
Firstly, matrix pretreatment: the quartz-based composite material substrate is placed in a constant temperature and humidity drying box and is placed for 5 hours at the temperature of 100 ℃.
Step two, preparing the components of the composite coating:
a, preparing first hole sealing slurry: 15g of perhydropolysilazane solution with the perhydropolysilazane content of 80.0% and 12g of quartz powder were stirred for 3min on a magnetic stirrer to be uniformly mixed, and the first hole sealing slurry was prepared.
b, preparing second hole sealing slurry: 12g of perhydropolysilazane solution with the perhydropolysilazane content of 50.0% and 21g of n-butyl ether were taken and stirred for 5min on a magnetic stirrer to be uniformly mixed, and second hole sealing slurry was prepared.
c, preparing a surface coating liquid: weighing 12g of organic silicon resin and 10g of dimethylbenzene, and stirring for 3min on a magnetic stirrer to uniformly mix to prepare the surface coating liquid.
Step three, a coating process:
coating the first hole sealing slurry on the surface of the quartz-based composite material by adopting a brushing process, drying at room temperature for 45min, curing, and performing primary hole sealing;
and b, coating the second hole sealing slurry on the surface of the first hole sealing slurry, and curing for 120min at 200 ℃ in a constant-temperature constant-humidity drying box to obtain a hole sealing layer.
c, coating surface coating liquid on the surface of the second hole sealing slurry, and curing for 120min at 200 ℃ in a constant-temperature constant-humidity drying oven to obtain the composite coating.
And (3) carrying out effect inspection on the composite coating prepared by the process.
And (3) testing results: the thickness of the composite coating is 3 microns, the composite coating is placed in a constant temperature and humidity box with the temperature of 60 ℃ and the relative humidity of 90% for 72 hours, the weight gain is 2.021%, the hardness of the composite coating is 5H, the adhesive force grade is 1 grade, the dielectric constant is 3.07, and the requirements of aviation and aerospace wave-transmitting materials on moisture-proof coatings are met.
Example 4
Firstly, matrix pretreatment: the quartz-based composite material substrate is placed in a constant temperature and humidity drying box and is placed for 5 hours at the temperature of 100 ℃.
Step two, preparing the components of the composite coating:
a, preparing first hole sealing slurry: 12g of perhydropolysilazane solution with the perhydropolysilazane content of 95.0% and 8g of quartz powder are taken and stirred on a magnetic stirrer for 3min to be uniformly mixed, so that the first hole sealing slurry is prepared.
b, preparing second hole sealing slurry: and (3) taking 6g of perhydropolysilazane solution with the perhydropolysilazane content of 95.0% and 18g of n-butyl ether, and stirring for 5min on a magnetic stirrer to uniformly mix to obtain second hole sealing slurry.
c, preparing a surface coating liquid: weighing 18g of organic silicon resin and 12g of dimethylbenzene, and stirring for 3min on a magnetic stirrer to uniformly mix to prepare the surface coating liquid.
Step three, a coating process:
coating the first hole sealing slurry on the surface of the quartz-based composite material by adopting a brushing process, drying at room temperature for 45min, curing, and performing primary hole sealing;
and b, coating the second hole sealing slurry on the surface of the first hole sealing slurry, and curing for 45min at 200 ℃ in a constant-temperature constant-humidity drying box to obtain a hole sealing layer.
c, coating surface coating liquid on the surface of the second hole sealing slurry, and curing for 90min at 200 ℃ in a constant-temperature constant-humidity drying oven to obtain the composite coating.
And (3) carrying out effect inspection on the composite coating prepared by the process.
And (3) testing results: the thickness of the composite coating is 4 microns, the composite coating is placed in a constant temperature and humidity box with the temperature of 60 ℃ and the relative humidity of 90% for 72 hours, the weight gain is 2.011 percent, the hardness of the composite coating is 5H, the adhesion grade is 1 grade, the dielectric constant is 3.12, and the requirements of aviation and aerospace wave-transmitting materials on moisture-proof coatings are met.
The above detailed description is provided for the purpose of illustrating the invention and the accompanying claims, it being understood that the above description is only exemplary of the invention and is not intended to limit the scope of the invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the invention should be included in the scope of the invention.
Claims (8)
1. A composite coating on the surface of a quartz-based composite material is characterized in that the composite coating sequentially comprises a first hole sealing slurry, a second hole sealing slurry and a surface coating liquid from inside to outside from the surface of the quartz-based composite material;
the first hole sealing slurry is prepared by mixing perhydropolysilazane and quartz powder, wherein the mass percent of the perhydropolysilazane is 30-60%, and the mass percent of the quartz powder is 40-70%;
the second hole sealing slurry is prepared by mixing perhydropolysilazane and n-butyl ether, wherein the mass percent of the perhydropolysilazane is 20-40%, and the mass percent of the n-butyl ether is 60-80%;
the surface coating liquid is prepared by mixing organic silicon resin and xylene, wherein the mass percent of the organic silicon resin is 30-60%, and the mass percent of the xylene is 40-70%.
2. A preparation method of a quartz-based composite material surface composite coating is characterized by comprising the following steps:
coating the first hole sealing slurry on the surface of a quartz-based composite material, drying at room temperature, curing, and performing primary hole sealing;
coating the second hole sealing slurry on the surface of the first hole sealing slurry, and curing at 200 ℃ in a constant-temperature constant-humidity drying box;
coating surface coating liquid on the surface of the second hole sealing slurry, and curing at 200 ℃ in a constant-temperature constant-humidity drying oven;
the first hole sealing slurry is prepared by mixing perhydropolysilazane and quartz powder, wherein the mass percent of the perhydropolysilazane is 30-60%, and the mass percent of the quartz powder is 40-70%;
the second hole sealing slurry is prepared by mixing perhydropolysilazane and n-butyl ether, wherein the mass percent of the perhydropolysilazane is 20-40%, and the mass percent of the n-butyl ether is 60-80%;
the surface coating liquid is prepared by mixing organic silicon resin and xylene, wherein the mass percent of the organic silicon resin is 30-60%, and the mass percent of the xylene is 40-70%.
3. The method for preparing the composite coating on the surface of the quartz-based composite material according to claim 2, wherein the perhydropolysilazane solution and the quartz powder are placed on a magnetic stirrer and stirred for 3-5 min to prepare uniform first hole sealing slurry, wherein the perhydropolysilazane content in the perhydropolysilazane solution is not less than 25.0%.
4. The method for preparing the composite coating on the surface of the quartz-based composite material according to claim 2, wherein the perhydropolysilazane solution and n-butyl ether are placed on a magnetic stirrer and stirred for 3-5 min to prepare uniform second hole sealing slurry; wherein the content of perhydropolysilazane in the perhydropolysilazane solution is not less than 25.0%.
5. The method for preparing the composite coating on the surface of the quartz-based composite material according to claim 2, wherein the organic silicon resin and the xylene are placed on a magnetic stirrer and stirred for 3-5 min to prepare uniform surface coating liquid.
6. The method for preparing the composite coating on the surface of the quartz-based composite material according to claim 2, wherein in the second step, the second hole sealing slurry is coated on the surface of the first hole sealing slurry, and after curing for 45-120 minutes at 200 ℃ in a constant temperature and humidity drying oven, the mixture is slowly cooled to room temperature.
7. The method for preparing the composite coating on the surface of the quartz-based composite material according to the claim 2 or 6, wherein in the third step, the surface coating liquid is coated on the surface of the second hole sealing slurry, cured at 200 ℃ for 45-120 minutes in a constant temperature and humidity drying oven, and then cooled to room temperature.
8. The method for preparing the composite coating on the surface of the quartz-based composite material as claimed in claim 2, wherein before the first hole sealing slurry is coated on the surface of the quartz-based composite material, a quartz-based composite material substrate is pretreated: and placing the quartz-based composite material substrate in a constant-temperature constant-humidity drying box for 4-5 hours at the temperature of 100-120 ℃.
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| CN115625099A (en) * | 2022-12-08 | 2023-01-20 | 北京玻钢院复合材料有限公司 | Hydrophobic moisture-proof layer of wave-transmitting material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115625099A (en) * | 2022-12-08 | 2023-01-20 | 北京玻钢院复合材料有限公司 | Hydrophobic moisture-proof layer of wave-transmitting material and preparation method thereof |
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