CN110818440A - Near-net compression molding and moisture-proof treatment method for sandwich-structure quartz composite ceramic radome - Google Patents
Near-net compression molding and moisture-proof treatment method for sandwich-structure quartz composite ceramic radome Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 41
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 239000010453 quartz Substances 0.000 title claims abstract description 28
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 239000000919 ceramic Substances 0.000 title claims abstract description 22
- 238000000748 compression moulding Methods 0.000 title claims abstract description 16
- 239000000835 fiber Substances 0.000 claims description 26
- 239000002245 particle Substances 0.000 claims description 22
- 239000002002 slurry Substances 0.000 claims description 22
- 229920000642 polymer Polymers 0.000 claims description 19
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 18
- 239000010702 perfluoropolyether Substances 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 15
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 12
- 238000005507 spraying Methods 0.000 claims description 11
- 238000004513 sizing Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 238000007664 blowing Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 238000010009 beating Methods 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000013461 design Methods 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 3
- 229910021645 metal ion Inorganic materials 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229920002401 polyacrylamide Polymers 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 abstract description 12
- 238000000465 moulding Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 3
- 230000032683 aging Effects 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 229910010293 ceramic material Inorganic materials 0.000 description 5
- 239000002250 absorbent Substances 0.000 description 4
- 238000007723 die pressing method Methods 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011799 hole material Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910001867 inorganic solvent Inorganic materials 0.000 description 2
- 239000003049 inorganic solvent Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000003075 superhydrophobic effect Effects 0.000 description 2
- 238000007669 thermal treatment Methods 0.000 description 2
- 239000011800 void material Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229920000247 superabsorbent polymer Polymers 0.000 description 1
Classifications
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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
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0045—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by a process involving the formation of a sol or a gel, e.g. sol-gel or precipitation processes
-
- 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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
-
- 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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- 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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/82—Asbestos; Glass; Fused 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
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/46—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 organic materials
- C04B41/49—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes
- C04B41/4905—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes containing silicon
- C04B41/495—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes containing silicon applied to the substrate as oligomers or polymers
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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
- C04B41/82—Coating or impregnation with organic materials
- C04B41/84—Compounds having one or more carbon-to-metal of carbon-to-silicon linkages
-
- 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
- H01Q1/422—Housings not intimately mechanically associated with radiating elements, e.g. radome comprising two or more layers of dielectric material
Abstract
The near-net compression molding and moisture-proof treatment method for the sandwich-structure quartz composite ceramic radome, which is designed by the invention, can realize near-net size integrated molding, and has high molding efficiency and low cost. The density of each layer of the radome is adjustable, the radome is suitable for a method for molding more layers of radomes, the process is high in designability, meets various requirements for broadband wave-transmitting functions, and has heat-proof and heat-insulating properties. The invention has the advantages of excellent moisture-proof effect, low carbon residue rate, simple process and low cost, and can not lose the moisture-proof effect due to microcrack generated by long-time aging.
Description
Technical Field
The invention belongs to the technical field of aerospace composite materials, and particularly relates to a near-net compression molding and moisture-proof treatment method for a sandwich-structure quartz composite ceramic radome.
Background
The missile radome is positioned at the most front end of the missile, is an important component of a radar guidance system, is a product integrating the structure and the function, and is an important guarantee for realizing accurate guidance of the missile under the high-speed flight condition. The quartz composite ceramic is the most mature material applied to the antenna housing at home and abroad at present, and has excellent performance, high temperature resistance and high wave transmission. With the development of aerospace technology and the improvement of missile weapon precision guidance technology, the missile radome presents the development trend of a multi-medium interlayer structure, and the integration functions of broadband wave transmission and heat insulation are realized.
The quartz composite ceramic material is a brittle high-hardness material, the structural molding and the precision processing of the material are technical short plates, the multilayer structure integrated molding cannot be realized, the cost is high, the period is long, a novel molding method is urgently needed to be developed, and the functional development requirement is met.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a preparation method of a multi-medium sandwich structure quartz composite ceramic radome, which can realize the integrated molding of a multilayer structure quartz composite ceramic material, has high process designability and low cost and efficiency, and provides a super-hydrophobic moisture-proof treatment process method which is adaptively matched with a porous ceramic material.
In order to achieve the purpose, the near-net compression molding and moisture-proof treatment method for the sandwich-structure quartz composite ceramic radome is characterized by comprising the following steps of:
s1, soaking quartz fiber yarns prepared by drawing without the impregnating compound in high-purity silica sol with 25% -40% of silicon oxide solid content for 1-1.5 h, taking out and airing at room temperature, then blowing and drying, and beating the fibers into fluffy shapes by adopting a high-speed mixer, wherein the fibers are required not to be adhered, thus preparing sizing fibers;
s2, mixing the high-solid-content high-purity silica sol, the sizing fiber and the super water-absorbing polymer particles according to the ratio of 100: 50: a and 100: 50: b, preparing materials according to the mass ratio, respectively stirring and mixing uniformly at a high speed, and standing to form a component A slurry and a component B slurry; the values of a and b are determined according to the design of the porosity of the sandwich structure material of the antenna housing, wherein a is more than or equal to 0.5 and less than or equal to 1.5; b is more than or equal to 8 and less than or equal to 12;
s3, pouring the X-mass component A slurry into a concave die cavity of a radome die, closing a convex die, pressurizing to 0.8-1 MPa by a press machine, and standing at room temperature for more than 24 hours to form an outer radome layer;
s4, opening the male die, continuously pouring the slurry of the component B with the mass Y into a concave die cavity of a radome die, closing the male die, pressurizing to 0.3-0.4 MPa by using a press machine, and standing at room temperature for more than 24 hours to form a radome middle layer;
s5, opening the male die, pouring the slurry of the component A in the mass Z into a concave die cavity of a radome die, closing the male die, pressurizing to 0.8-1 MPa by a press machine, standing at room temperature for more than 24 hours to form a radome inner layer, and taking out a radome blank;
s6, blowing and drying the radome blank for 24 hours at the temperature of 40-60 ℃, and heating according to the following curve for heat treatment: gradually increasing to 100 ℃ within 1h, preserving heat for 2h at 100 ℃, gradually increasing to 300 ℃ within 3h, preserving heat for 3h at 300 ℃, gradually increasing to 500 ℃ within 2h, preserving heat for 3h at 500 ℃, gradually increasing to 900 ℃ within 4h, preserving heat for 3h at 900 ℃, and cooling along with the furnace after finishing;
s7, spraying a layer of KH550 silane coupling agent solution on the inner and outer surfaces of the sintered and molded antenna housing, airing at room temperature for 2h, spraying a layer of amino-terminated modified perfluoropolyether siloxane solution on the inner and outer surfaces, airing at room temperature for no glue flowing on the surfaces, and drying at 100-120 ℃ for 2-3 h to form the moisture-proof coating.
Preferably, in S1, the quartz fiber yarn is selected from short fibers with a length of 10mm to 30 mm. The quartz fiber yarn prepared by drawing without the impregnating compound has good bonding performance with a silicon oxide matrix, does not need to remove the impregnating compound again, and has simple process and low cost.
Preferably, in S1, the room temperature airing time is 24-48 h, and the blowing temperature is 100 ℃.
Preferably, in S2, the high-purity silica sol has a solid content of more than 60%, a metal ion content of not more than 1000ppm, and a pH of 8-10.
Preferably, in S2, the super absorbent polymer particles can be polyacrylamide or polyvinyl alcohol, and the diameter of the particles is not more than 300 μm. The super water-absorbing polymer particles have the following functions: (a) the antenna housing is in a closed environment during mould pressing, the moisture volatilization difficulty is high, the shaping is difficult, and the super-absorbent polymer particles are added to quickly absorb water so as to shape the blank. (b) The super-absorbent polymer particles are organic matters, and can be oxidized and volatilized during high-temperature heat treatment to form gaps in the ceramic, so that the density of the polymer material is adjusted.
Preferably, in S2, the standing time is not less than 30 min.
Preferably, in S3 to S5, the mass X, Y, Z of the slurry added for preparing the outer layer, the middle layer and the inner layer of the radome is determined according to the volume and the designed predetermined density of each layer of the radome, the mass of the solid silica required by each layer is determined, and then the value X, Y, Z is determined according to the solid content of the silica sol and the ratio of each component.
Preferably, in S6, oxygen supply is started when the temperature is required to rise to 300 ℃. The radome blank needs to slowly volatilize water absorbed by the super water-absorbing polymer particles at a low temperature, then the temperature is slowly increased in a stepped manner, and the super water-absorbing polymer particle material is gradually oxidized and volatilized, so that the structural strength and the microscopic void structure are prevented from being damaged due to too fast temperature increase. So, can fully get rid of super polymer particles that absorb water, form sandwich structure antenna house to because fibre reinforced composite ceramic material is porous, through-hole material, do benefit to super polymer particles that absorb water high temperature thermal treatment more and get rid of.
Preferably, in the S7, a KH550 solution diluted by ethanol is selected, wherein the mass fraction of the KH550 is 10-20%. Therefore, the perfluoropolyether siloxane can be well combined with the quartz composite ceramic to form an interface.
Preferably, in S7, the amino-terminated modified perfluoropolyether siloxane is a solution prepared by taking amino-terminated modified perfluoropolyether triethoxy siloxane as a solute and n-hexane as a solvent, wherein the mass fraction of the amino-terminated modified perfluoropolyether triethoxy siloxane is 50-60%, the spraying thickness is 30-50 μm, and the spraying can be carried out for multiple times. The amino-terminated modified perfluoropolyether siloxane has low surface energy superhydrophobicity, can form a superhydrophobic protective film on the surface of ceramic, has excellent moisture-proof effect, and can control the moisture absorption rate within 0.5 percent. The high toughness of the perfluoropolyether siloxane prevents microcracking; the perfluoropolyether siloxane is a polymer with a high molecular chain, has micro-permeation on the surface of the microporous ceramic, but has extremely small thickness after permeating into a base material, can be controlled within the range of 1mm, and has extremely low high-temperature carbon residue rate, so that carbonization influence can not be formed when the perfluoropolyether siloxane is used in a high-temperature environment flying at high speed.
The invention has the beneficial effects that: the invention can be integrally formed with near net size, and has high forming efficiency and low cost. The density of each layer of the radome is adjustable, the radome is suitable for a method for molding more layers of radomes, the process is high in designability, meets various requirements for broadband wave-transmitting functions, and has heat-proof and heat-insulating properties. The invention has excellent moisture-proof effect, low carbon residue rate, simple process and low cost, and can not lose the moisture-proof effect due to microcracks generated in a long-time mode. The slurry prepared from the high-solid-content high-purity silica sol, the sizing fiber and the super-absorbent polymer particles has better fluidity, is suitable for a die pressing process, solves the problem that inorganic dry materials have poor fluidity and are not uniformly molded, and simultaneously solves the problem that solvents cannot volatilize and are not suitable for the die pressing process of inorganic solvent type slurry.
The above-mentioned near net size means near net size, and is a common word.
Detailed Description
The technical solutions of the present invention (including the preferred ones) are described in further detail below by way of listing some alternative embodiments of the present invention. It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without any inventive step, are within the scope of the present invention.
The invention discloses a near-net compression molding and moisture-proof treatment method for a sandwich-structure quartz composite ceramic radome, which is characterized by comprising the following steps of:
s1, soaking the quartz fiber yarn of the short fiber with the length of 10 mm-30 mm, which is prepared by drawing without the impregnating compound, in high-purity silica sol with the solid content of 25% -40% of silicon oxide for 1-1.5 h at room temperature, taking out, airing at room temperature for 24-48 h, blowing and drying at 100 ℃, beating the fiber into fluffy shape by adopting a high-speed mixer, and preparing sizing fiber when the fiber is required not to be adhered; the quartz fiber yarn prepared by drawing without the sizing agent has good bonding performance with a silicon oxide matrix, does not need to remove the sizing agent again, and has simple process and low cost.
S2, mixing the high-solid-content high-purity silica sol, the sizing fiber and the super water-absorbing polymer particles according to the ratio of 100: 50: a and 100: 50: b, preparing materials according to the mass ratio, respectively stirring and mixing uniformly at a high speed, and standing for no less than 30min to form a component A slurry and a component B slurry; the values of a and b are determined according to the design of the porosity of the sandwich structure material of the antenna housing, wherein a is more than or equal to 0.5 and less than or equal to 1.5; b is more than or equal to 8 and less than or equal to 12;
wherein the solid content of the silica sol is more than 60%, the content of metal ions is not more than 1000ppm, and the PH value is 8-10; the super water-absorbing polymer particles can be made of materials such as polyacrylamide or polyvinyl alcohol, and the particle diameter is not more than 300 mu m;
the slurry prepared from the high-solid-content high-purity silica sol, the sizing fiber and the super-absorbent polymer particles has better fluidity, is suitable for a die pressing process, solves the problem that inorganic dry materials have poor fluidity and are not uniformly molded, and simultaneously solves the problem that solvents cannot volatilize and are not suitable for the die pressing process of inorganic solvent type slurry.
S3, pouring the X-mass component A slurry into a concave die cavity of a radome die, closing a convex die, pressurizing to 0.8-1 MPa by a press machine, and standing at room temperature for more than 24 hours to form an outer radome layer;
s4, opening the male die, continuously pouring the slurry of the component B with the mass Y into a concave die cavity of a radome die, closing the male die, pressurizing to 0.3-0.4 MPa by using a press machine, and standing at room temperature for more than 24 hours to form a radome middle layer;
s5, opening the male die, pouring the slurry of the component A in the mass Z into a concave die cavity of a radome die, closing the male die, pressurizing to 0.8-1 MPa by a press machine, standing at room temperature for more than 24 hours to form a radome inner layer, and taking out a radome blank;
the mass X, Y, Z of the slurry added for preparing the outer layer, the middle layer and the inner layer of the antenna housing is determined according to the volume of each layer of the antenna housing and the designed preset density, the mass of the solid silicon oxide required by each layer is determined, and then the value X, Y, Z is determined according to the solid content of the silica sol and the proportion of each component.
S6, blowing and drying the radome blank for 24 hours at the temperature of 40-60 ℃, and heating according to the following curve for heat treatment: gradually increasing to 100 ℃ within 1h, preserving heat for 2h at 100 ℃, gradually increasing to 300 ℃ within 3h, preserving heat for 3h at 300 ℃, gradually increasing to 500 ℃ within 2h, preserving heat for 3h at 500 ℃, gradually increasing to 900 ℃ within 4h, preserving heat for 3h at 900 ℃, and cooling along with the furnace after finishing; starting to introduce oxygen when the temperature rises to 300 ℃; the radome blank needs to slowly volatilize water absorbed by the super water-absorbing polymer particles at a low temperature, then the temperature is slowly increased in a stepped manner, and the super water-absorbing polymer particle material is gradually oxidized and volatilized, so that the structural strength and the microscopic void structure are prevented from being damaged due to too fast temperature increase; so, can fully get rid of super polymer particles that absorb water, form sandwich structure antenna house to because fibre reinforced composite ceramic material is porous, through-hole material, do benefit to super polymer particles that absorb water high temperature thermal treatment more and get rid of.
S7, spraying a layer of KH550 silane coupling agent solution diluted by ethanol on the inner and outer surfaces of the sintered and molded antenna housing, wherein the mass fraction of KH550 is 10% -20%, airing at room temperature for 2h, then spraying a layer of amino-terminated modified perfluoropolyether siloxane solution on the inner and outer surfaces, airing at room temperature for no glue flow on the surfaces, and then drying at 100-120 ℃ for 2 h-3 h to form a moisture-proof coating; the amino-terminated modified perfluoropolyether siloxane solution is prepared by taking amino-terminated modified perfluoropolyether triethoxy siloxane as a solute and n-hexane as a solvent, wherein the mass fraction of the amino-terminated modified perfluoropolyether triethoxy siloxane is 50-60%, the spraying thickness is 30-50 mu m, and the amino-terminated modified perfluoropolyether triethoxy siloxane can be sprayed for multiple times.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and any modification, combination, replacement, or improvement made within the spirit and principle of the present invention is included in the scope of the present invention.
Claims (10)
1. A near-net compression molding and moisture-proof treatment method for a sandwich-structure quartz composite ceramic radome is characterized by comprising the following steps of:
s1, soaking the quartz fiber yarn prepared by drawing without the impregnating compound in high-purity silica sol with 25-40% of silicon oxide solid content for 1-1.5 h at room temperature, taking out and airing at room temperature, then blowing and drying, and beating the fiber into fluffy shape by using a high-speed mixer, wherein the fibers are required to be not adhered, thus preparing sizing fiber;
s2, mixing the high-solid-content high-purity silica sol, the sizing fiber and the super water-absorbing polymer particles according to the ratio of 100: 50: a and 100: 50: b, preparing materials according to the mass ratio, respectively stirring and mixing uniformly at a high speed, and standing to form a component A slurry and a component B slurry; the values of a and b are determined according to the design of the porosity of the sandwich structure material of the antenna housing, wherein a is more than or equal to 0.5 and less than or equal to 1.5; b is more than or equal to 8 and less than or equal to 12;
s3, pouring the X-mass component A slurry into a concave die cavity of a radome die, closing a convex die, pressurizing to 0.8-1 MPa by a press machine, and standing at room temperature for more than 24 hours to form an outer radome layer;
s4, opening the male die, continuously pouring the slurry of the component B with the mass Y into a concave die cavity of a radome die, closing the male die, pressurizing to 0.3-0.4 MPa by using a press machine, and standing at room temperature for more than 24 hours to form a radome middle layer;
s5, opening the male die, pouring the slurry of the component A in the mass Z into a concave die cavity of a radome die, closing the male die, pressurizing to 0.8-1 MPa by a press machine, standing at room temperature for more than 24 hours to form a radome inner layer, and taking out a radome blank;
s6, blowing and drying the radome blank for 24 hours at the temperature of 40-60 ℃, and heating according to the following curve for heat treatment: gradually increasing to 100 ℃ within 1h, preserving heat for 2h at 100 ℃, gradually increasing to 300 ℃ within 3h, preserving heat for 3h at 300 ℃, gradually increasing to 500 ℃ within 2h, preserving heat for 3h at 500 ℃, gradually increasing to 900 ℃ within 4h, preserving heat for 3h at 900 ℃, and cooling along with the furnace after finishing;
s7, spraying a layer of KH550 silane coupling agent solution on the inner and outer surfaces of the sintered and molded antenna housing, airing at room temperature for 2h, spraying a layer of amino-terminated modified perfluoropolyether siloxane solution on the inner and outer surfaces, airing at room temperature for no glue flowing on the surfaces, and drying at 100-120 ℃ for 2-3 h to form the moisture-proof coating.
2. The near-net compression molding and moisture-proof treatment method for the sandwich-structure quartz composite ceramic radome of claim 1, wherein the method comprises the following steps: in S1, a quartz fiber yarn of short fiber with a length of 10 mm-30 mm is selected.
3. The near-net compression molding and moisture-proof treatment method for the sandwich-structure quartz composite ceramic radome of claim 1, wherein the method comprises the following steps: and in S1, airing at room temperature for 24-48 h, wherein the blowing temperature is 100 ℃.
4. The near-net compression molding and moisture-proof treatment method for the sandwich-structure quartz composite ceramic radome of claim 1, wherein the method comprises the following steps: in S2, the high-purity silica sol has a solid content of more than 60%, a metal ion content of not more than 1000ppm, and a pH of 8-10.
5. The near-net compression molding and moisture-proof treatment method for the sandwich-structure quartz composite ceramic radome of claim 1, wherein the method comprises the following steps: in S2, the super water-absorbing polymer particles adopt polyacrylamide or polyvinyl alcohol, and the particle diameter is not more than 300 μm.
6. The near-net compression molding and moisture-proof treatment method for the sandwich-structure quartz composite ceramic radome of claim 1, wherein the method comprises the following steps: and in S2, the standing time is not less than 30 min.
7. The near-net compression molding and moisture-proof treatment method for the sandwich-structure quartz composite ceramic radome of claim 1, wherein the method comprises the following steps: and in S3-S5, the mass X, Y, Z of the slurry added for preparing the outer layer, the middle layer and the inner layer of the antenna cover is determined according to the volume of each layer of the antenna cover and the designed preset density, the mass of solid silicon oxide required by each layer is determined, and then the value X, Y, Z is determined according to the solid content of silica sol and the proportion of each component.
8. The near-net compression molding and moisture-proof treatment method for the sandwich-structure quartz composite ceramic radome of claim 1, wherein the method comprises the following steps: in S6, oxygen supply is started when the temperature is required to rise to 300 ℃.
9. The near-net compression molding and moisture-proof treatment method for the sandwich-structure quartz composite ceramic radome of claim 1, wherein the method comprises the following steps: in S7, KH550 solution diluted by ethanol is selected, wherein the mass fraction of KH550 is 10-20%.
10. The near-net compression molding and moisture-proof treatment method for the sandwich-structure quartz composite ceramic radome of claim 1, wherein the method comprises the following steps: in S7, the amino-terminated modified perfluoropolyether siloxane solution is prepared by taking amino-terminated modified perfluoropolyether triethoxy siloxane as a solute and n-hexane as a solvent, wherein the amino-terminated modified perfluoropolyether triethoxy siloxane accounts for 50-60% by mass, the spraying thickness is 30-50 μm, and the spraying can be carried out for multiple times.
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