CN114031419B - Preparation method of inorganic moisture-proof layer of quartz ceramic radome - Google Patents
Preparation method of inorganic moisture-proof layer of quartz ceramic radome Download PDFInfo
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- CN114031419B CN114031419B CN202111383774.3A CN202111383774A CN114031419B CN 114031419 B CN114031419 B CN 114031419B CN 202111383774 A CN202111383774 A CN 202111383774A CN 114031419 B CN114031419 B CN 114031419B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5025—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
- C04B41/5035—Silica
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01Q—ANTENNAS, i.e. RADIO AERIALS
- H01Q1/00—Details of, or arrangements associated with, antennas
- H01Q1/42—Housings not intimately mechanically associated with radiating elements, e.g. radome
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Abstract
The invention discloses a preparation method of an inorganic moisture-proof layer of a quartz ceramic radome, which comprises the following steps: 1) preparing vitrification glue: uniformly mixing organic silicon resin, silicon oxide powder, low-melting-point glass powder, a silane coupling agent and a solvent, and removing bubbles; 2) antenna housing surface treatment: polishing the surface of a quartz ceramic antenna housing to be smooth, blowing off dust, brushing a silane coupling agent on the surface once, cleaning with ethanol, naturally volatilizing, and carrying out forced air drying in a forced air drying oven; 3) spraying glue on the surface; 4) curing, including precuring, medium temperature curing and high temperature curing; 5) and (5) aging treatment. According to the invention, the organic silicon resin is added, so that the effective components of the moisture-proof layer can be promoted to be adhered to the surface of the antenna housing, and the bonding force between the effective components and the antenna housing interface is improved. Through pre-curing and medium-temperature curing, a silica compound is formed, then through high-temperature curing, the low-melting-point glass powder is melted, gaps are filled to form a continuous phase, and a vitrified film layer is formed, so that the coating is high-temperature resistant and has good moisture resistance.
Description
Technical Field
The invention belongs to the technical field of wave-transparent ceramic composite materials for aerospace, and particularly relates to a preparation method of a quartz ceramic radome moisture-proof layer.
Background
At present, microwave radar guidance is mostly adopted for high-speed aircrafts, and a high-temperature resistant ceramic antenna housing is an important part of the high-speed aircrafts. The high-temperature resistant ceramic radome seriously affects the wave transmission performance due to moisture absorption, so the moisture resistance is critical. Along with the improvement of the flying speed of an aircraft, the requirement of the high temperature resistance (over 800 ℃) of the antenna housing is improved, and the antenna housing is required to be reusable. At present, the ceramic radome, especially the quartz ceramic radome is dampproof, mainly adopts an organic resin coating to prevent moisture, and is carbonized and falls off after high temperature (800 ℃ resistance), so that the moisture-proof effect is influenced, and the ceramic radome cannot be reused. In the existing antenna housing using the inorganic moisture-proof layer, the inorganic coating is made of non-silicon dioxide materials such as phosphate and the like, cracks and the like can be generated due to the difference of thermal matching property with quartz ceramics, and the antenna housing using the quartz material needs high-temperature construction and is complex in operation and difficult to operate.
Disclosure of Invention
The invention aims to provide a preparation method of an inorganic moisture-proof layer of a quartz ceramic radome, so as to improve the high-temperature resistance of the moisture-proof layer of the quartz ceramic radome, and the moisture-proof layer can be repeatedly used under a high-temperature condition.
In order to achieve the purpose, the preparation method of the inorganic moisture-proof layer of the quartz ceramic radome provided by the invention comprises the following steps:
1) preparing vitrification glue: the organic silicon resin, the silicon oxide powder, the low-melting-point glass powder, the silane coupling agent and the solvent are weighed according to the proportion, mixed uniformly and vacuumized to remove bubbles.
2) Antenna housing surface treatment: polishing the surface of the quartz ceramic radome with sand paper, blowing off surface dust by using an inert gas source, brushing the surface once with a silane coupling agent (KH550, 560 or 570), washing with ethanol, volatilizing the ethanol, and drying by blowing in a blowing drying oven at the temperature of 60 ℃/2h → 150 ℃/2 h.
3) Spraying glue on the surface: spraying glue on the surface of the radome by adopting a high-pressure spraying mode, putting the prepared vitrified glue into a high-pressure spray gun, spraying the vitrified glue on the surface of the radome by using an inert gas source, wherein the pressure is more than 1-2MPa, the diameter phi 1mm of a nozzle is 45-75 degrees with the surface of the radome, the speed of reaching the surface of the product reaches more than 50m/s, and if the conditions allow, the pressure of 60-90kPa is applied on the back of the sprayed product, so that air holes can be reduced, and the compactness effect is better.
4) And (3) curing: putting the mixture into an atmosphere high-temperature furnace, vacuumizing and pre-curing, wherein the curing system is as follows: 60 ℃/3h → 120 ℃/2h → 150 ℃/2 h; then, continuously heating in the oxygen atmosphere, and carrying out medium-temperature curing, wherein the curing system is as follows: 350 ℃/1h → 500 ℃/2h → 700 ℃/1 h; and finally, continuously heating under the vacuum condition, and carrying out high-temperature curing: the curing system is as follows: 700 ℃/1h → 900 ℃/2h, and then cooling to room temperature along with the furnace.
5) Aging treatment: the method comprises the steps of heating the radome to 350 ℃ at a speed of 2-5 ℃/min in the air atmosphere, preserving heat for 2-5 h, cooling to room temperature along with a furnace, and removing stress.
Further, in the step 1), 100 parts of organic silicon resin, 30-40 parts of silicon oxide powder, 80-100 parts of low-melting-point glass powder, 2-3 parts of silane coupling agent and 30-50 parts of solvent. The organic silicon resin can adopt methyl silicon resin or phenyl silicon resin. The silica powder is prepared by evaporating water from silica sol, calcining at 900-1000 deg.C with oxygen, grinding, and sieving to 2000-25%A 00 mesh powder, which is in an amorphous state. The low-melting-point glass powder is PbO-B 2 O 3 -SiO 2 The glass powder of the system has the content of metal sodium ions lower than 500 ppm. The silane coupling agent can be selected according to the silicone resin, and a corresponding curing agent such as KH550 can be selected. The solvent is organic solvent such as xylene.
Further, in the step 4), pre-curing, medium-temperature curing and high-temperature curing in curing are required to be continuously carried out, and the heating rate is 2-5 ℃/min. The pre-curing is to cure the organic silicon resin, the medium-temperature curing is to remove organic matters in the vitrified layer in an aerobic environment, and the high-temperature curing is to melt the low-melting-point glass powder and fill gaps to form a continuous phase to form a vitrified film layer, so that the vitrified film layer has good moisture resistance.
Further, in the step 5), the aging treatment is to release stress of the vitrified layer, the heat preservation time is determined according to the thickness of the antenna housing product, and the time needs to be prolonged as the thickness of the antenna housing is larger.
Compared with the prior art, the invention has the following advantages:
according to the invention, due to the addition of the organic silicon resin, effective components of the moisture-proof layer can be promoted to be well adhered to the surface of the radome, and the bonding force between the moisture-proof layer and the interface of the quartz ceramic radome and the manufacturability of the vitrification layer are greatly improved. The added low-melting-point glass powder can effectively reduce the forming temperature of the ceramic vitrified layer. The organic silicon resin can be cured through pre-curing, and the organic matters in the vitrification layer can react to form a silicon-oxygen compound under an aerobic environment through medium-temperature curing, so that the organic silicon resin which is not resistant to high temperature is converted into the high-temperature resistant silicon-oxygen compound, and then the low-melting-point glass powder is melted through high-temperature curing to fill the gaps to form a continuous phase and form a vitrified film layer, so that the coating is resistant to high temperature and has better moisture resistance.
The vitrified moisture-proof layer prepared by the method is used for moisture prevention of the quartz ceramic radome, can control the moisture absorption rate of the quartz ceramic to be below 0.5% under the humidity of 95%, and can be repeatedly used under the high-temperature condition of 800 ℃. In addition, the method has good manufacturability and simple operation, is suitable for various radome products with special-shaped sizes, and can be applied to pure quartz ceramics and fiber reinforced quartz composite ceramic materials.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1:
1) preparing vitrification glue: weighing 100 parts of methyl silicone resin, 30 parts of silicon oxide powder and PbO-B 2 O 3 -SiO 2 85 parts of system glass powder (the content of metal sodium ions is lower than 500ppm), 2 parts of silane coupling agent (KH550) and 40 parts of dimethylbenzene, uniformly mixing, and vacuumizing to remove bubbles. Wherein, the silica powder is prepared by evaporating water of silica sol, roasting at 900 deg.C with oxygen, grinding, and sieving to 2000 mesh powder, which is amorphous.
2) Antenna housing surface treatment: polishing the surface of the quartz ceramic radome smoothly by using sand paper, blowing off surface dust by using high-pressure nitrogen, brushing the surface once by using a silane coupling agent (KH550), cleaning by using ethanol, volatilizing the ethanol, and drying by blowing in a forced air drying oven at the temperature of 60 ℃/2h → 150 ℃/2 h.
3) Spraying glue on the surface: spraying glue on the surface of the antenna housing by adopting a high-pressure spraying mode, applying 70kPa pressure on the back of the antenna housing, putting the prepared vitrified glue into a high-pressure spray gun, spraying the vitrified glue to the surface of a product at an angle of 60 degrees with the surface of the antenna housing by taking nitrogen as an inert gas source under the pressure of 1.2MPa and the diameter phi of a nozzle of 1mm, wherein the speed of reaching the surface of the product reaches 55 m/s.
4) And (3) curing: putting the mixture into an atmosphere high-temperature furnace, vacuumizing and pre-curing, wherein the curing system is as follows: 60 ℃/3h → 120 ℃/2h → 150 ℃/2 h; then, continuously heating in the oxygen atmosphere, and carrying out medium-temperature curing, wherein the curing system is as follows: 350 ℃/1h → 500 ℃/2h → 700 ℃/1 h; and finally, continuously heating under the vacuum condition, and carrying out high-temperature curing: the curing system is as follows: 700 ℃/1h → 900 ℃/2h, and then cooling to room temperature along with the furnace, wherein the heating rates of the three curing systems are all 3 ℃/min.
5) Aging treatment: the antenna housing is heated to 350 ℃ at the speed of 3 ℃/min in the air atmosphere, the temperature is kept for 3h, and then the temperature is reduced to room temperature along with the furnace, and the stress is removed.
Example 2:
1) preparing vitrification glue: 100 parts of glass, 40 parts of silicon oxide powder and PbO-B are weighed 2 O 3 -SiO 2 95 parts of system glass powder (the content of metal sodium ions is lower than 500ppm), 3 parts of silane coupling agent (KH570) and 45 parts of dimethylbenzene, uniformly mixing, and vacuumizing to remove bubbles. Wherein, the silica powder is obtained by evaporating water from silica sol, calcining at 1000 deg.C with oxygen, grinding, and sieving to 2500 mesh powder, which is amorphous.
2) Antenna housing surface treatment: polishing the surface of the quartz ceramic radome smoothly by using sand paper, blowing off surface dust by using high-pressure nitrogen, brushing the surface once by using a silane coupling agent (KH550), cleaning by using ethanol, volatilizing the ethanol, and drying by blowing in a forced air drying oven at the temperature of 60 ℃/2h → 150 ℃/2 h.
3) Spraying glue on the surface: spraying glue on the surface of the antenna housing by adopting a high-pressure spraying mode, putting the prepared vitrified glue into a high-pressure spray gun, spraying the vitrified glue to the surface of a product at an angle of 60 degrees with the surface of the antenna housing by taking nitrogen as an inert gas source, wherein the pressure is more than 1.5MPa, and the diameter phi of a nozzle is 1mm, and the speed of reaching the surface of the product reaches more than 60 m/s.
4) And (3) curing: putting the mixture into an atmosphere high-temperature furnace, vacuumizing and pre-curing, wherein the curing system is as follows: 60 ℃/3h → 120 ℃/2h → 150 ℃/2 h; then, continuously heating in the oxygen atmosphere, and carrying out medium-temperature curing, wherein the curing system is as follows: 350 ℃/1h → 500 ℃/2h → 700 ℃/1 h; and finally, continuously heating under the vacuum condition, and carrying out high-temperature curing: the curing system is as follows: 700 ℃/1h → 900 ℃/2h, and then cooling to room temperature along with the furnace, wherein the heating rates of the three curing systems are all 3 ℃/min.
5) And (3) aging treatment: the antenna housing is heated to 350 ℃ at the speed of 3 ℃/min in the air atmosphere, the temperature is kept for 3h, and then the temperature is reduced to room temperature along with the furnace, and the stress is removed.
The vitrified moisture-proof layer prepared by the method is used for moisture prevention of the quartz ceramic radome, can control the moisture absorption rate of the quartz ceramic to be below 0.5% under the humidity of 95%, can be repeatedly used under the high-temperature condition of 800 ℃, and can also meet the wave transmission requirement of the radome.
Claims (8)
1. A preparation method of an inorganic moisture-proof layer of a quartz ceramic radome is characterized by comprising the following steps: the method comprises the following steps:
1) preparing vitrification glue: weighing organic silicon resin, silicon oxide powder, low-melting-point glass powder, a silane coupling agent and a solvent according to a ratio, uniformly mixing, and vacuumizing to remove bubbles; the low-melting-point glass powder is PbO-B 2 O 3 -SiO 2 The glass powder of the system has the metal sodium ion content lower than 500 ppm;
2) antenna housing surface treatment: polishing the surface of the quartz ceramic radome smoothly by using abrasive paper, blowing off surface dust by using an inert gas source, brushing the surface once by using a silane coupling agent, cleaning by using ethanol, volatilizing the ethanol, and carrying out forced air drying in a forced air drying oven;
3) spraying glue on the surface: spraying glue on the surface of the antenna housing by adopting a high-pressure spraying mode, putting the prepared vitrified glue into a high-pressure spray gun, spraying the vitrified glue to the surface of a product at an angle of 45-75 degrees with the surface of the antenna housing by using an inert gas source under the pressure of 1-2MPa and the diameter phi of a nozzle of 1mm, and ensuring that the speed of reaching the surface of the product reaches more than 50 m/s;
4) and (3) curing: putting the mixture into an atmosphere high-temperature furnace, vacuumizing and pre-curing, wherein the curing system is as follows: 60 ℃/3h → 120 ℃/2h → 150 ℃/2 h; then, continuously heating in the oxygen atmosphere, and carrying out medium-temperature curing, wherein the curing system is as follows: 350 ℃/1h → 500 ℃/2h → 700 ℃/1 h; and finally, continuously heating under the vacuum condition, and carrying out high-temperature curing: the curing system is as follows: 700 ℃/1h → 900 ℃/2h, and then cooling to room temperature along with the furnace;
5) aging treatment: the antenna housing is heated to 350 ℃ at the speed of 2-5 ℃/min in the air atmosphere, the temperature is kept for 2-5 h, then the temperature is reduced to the room temperature along with the furnace, and the stress is removed.
2. The method for preparing the inorganic moisture-proof layer of the quartz ceramic radome of claim 1, wherein the method comprises the following steps: in the step 1), 100 parts of organic silicon resin, 30-40 parts of silicon oxide powder, 80-100 parts of low-melting-point glass powder, 2-3 parts of silane coupling agent and 30-50 parts of solvent.
3. The preparation method of the inorganic moisture-proof layer of the quartz ceramic radome of claim 1 or 2, wherein the preparation method comprises the following steps: in the step 1), the organic silicon resin is methyl silicon resin or phenyl silicon resin.
4. The preparation method of the inorganic moisture-proof layer of the quartz ceramic radome of claim 1 or 2, wherein the preparation method comprises the following steps: in the step 1), the silicon oxide powder is amorphous powder which is obtained by evaporating water in silica sol, then roasting at 900-1000 ℃ by introducing oxygen, grinding and sieving to 2000-2500 meshes.
5. The preparation method of the inorganic moisture-proof layer of the quartz ceramic radome of claim 1 or 2, wherein the preparation method comprises the following steps: in the steps 1) and 2), the silane coupling agent is KH550, 560 or 570, and in the step 1), the solvent is xylene.
6. The preparation method of the inorganic moisture-proof layer of the quartz ceramic radome of claim 1 or 2, wherein the preparation method comprises the following steps: in the step 2), the forced air drying is carried out at 60 ℃ for two hours, and then at 150 ℃ for two hours.
7. The preparation method of the inorganic moisture-proof layer of the quartz ceramic radome of claim 1 or 2, wherein the preparation method comprises the following steps: in the step 3), when glue is sprayed on the surface of the antenna housing, 60-90kPa pressure is applied to the back surface of the antenna housing.
8. The preparation method of the inorganic moisture-proof layer of the quartz ceramic radome of claim 1 or 2, wherein the preparation method comprises the following steps: in the step 3), pre-curing, medium-temperature curing and high-temperature curing in curing are continuously carried out, and the heating rate is 2-5 ℃/min.
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