CN117832831A - High-strength negative pressure-resistant basalt fiber radome - Google Patents
High-strength negative pressure-resistant basalt fiber radome Download PDFInfo
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- CN117832831A CN117832831A CN202410187431.7A CN202410187431A CN117832831A CN 117832831 A CN117832831 A CN 117832831A CN 202410187431 A CN202410187431 A CN 202410187431A CN 117832831 A CN117832831 A CN 117832831A
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- 229920002748 Basalt fiber Polymers 0.000 title claims abstract description 99
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 96
- 239000002002 slurry Substances 0.000 claims abstract description 56
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 37
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 37
- 229910052582 BN Inorganic materials 0.000 claims abstract description 21
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000002791 soaking Methods 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- 238000004519 manufacturing process Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 76
- 239000000835 fiber Substances 0.000 claims description 43
- 239000004744 fabric Substances 0.000 claims description 42
- 238000010438 heat treatment Methods 0.000 claims description 40
- 238000009987 spinning Methods 0.000 claims description 34
- 238000001816 cooling Methods 0.000 claims description 31
- 239000007789 gas Substances 0.000 claims description 26
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 24
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 24
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 21
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 16
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 16
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims description 14
- 239000005049 silicon tetrachloride Substances 0.000 claims description 14
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 12
- 239000002202 Polyethylene glycol Substances 0.000 claims description 12
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 229920000058 polyacrylate Polymers 0.000 claims description 12
- 229920001223 polyethylene glycol Polymers 0.000 claims description 12
- 239000002243 precursor Substances 0.000 claims description 12
- 239000004576 sand Substances 0.000 claims description 12
- 238000007711 solidification Methods 0.000 claims description 12
- 230000008023 solidification Effects 0.000 claims description 12
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 12
- WRECIMRULFAWHA-UHFFFAOYSA-N trimethyl borate Chemical compound COB(OC)OC WRECIMRULFAWHA-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000006004 Quartz sand Substances 0.000 claims description 10
- 239000004113 Sepiolite Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 229910052903 pyrophyllite Inorganic materials 0.000 claims description 10
- 229910052624 sepiolite Inorganic materials 0.000 claims description 10
- 235000019355 sepiolite Nutrition 0.000 claims description 10
- 239000000454 talc Substances 0.000 claims description 10
- 229910052623 talc Inorganic materials 0.000 claims description 10
- 235000012222 talc Nutrition 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 239000001257 hydrogen Substances 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 238000009941 weaving Methods 0.000 claims description 2
- 230000005540 biological transmission Effects 0.000 abstract description 3
- 238000005452 bending Methods 0.000 abstract description 2
- 238000009954 braiding Methods 0.000 abstract description 2
- 238000009826 distribution Methods 0.000 abstract description 2
- 238000005245 sintering Methods 0.000 abstract description 2
- 238000002844 melting Methods 0.000 description 18
- 230000008018 melting Effects 0.000 description 18
- 239000000203 mixture Substances 0.000 description 12
- 230000008595 infiltration Effects 0.000 description 10
- 238000001764 infiltration Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 238000000151 deposition Methods 0.000 description 4
- 230000004888 barrier function Effects 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
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Abstract
The invention provides a high-strength negative pressure resistant basalt fiber radome and a preparation method thereof, the method comprises the steps of preparing basalt fibers, forming a coated nano silicon dioxide layer on the surfaces of the basalt fibers, forming a boron nitride layer, preparing a braiding body, soaking in slurry, co-curing and sintering to obtain the radome, wherein the radome has a wave transmission rate of more than 90% within 0.1MHz-20GHz, a tensile strength of more than 350MPa and a bending strength of more than 100MPa, has good negative pressure resistant performance, and has controllable process, strong operability, high forming efficiency and more uniform product density distribution, and realizes low-cost and mass stable production of the high-performance radome.
Description
Technical Field
The invention relates to a high-strength negative pressure resistant basalt fiber radome.
Background
The radome is positioned at the nose of the cabin of the aircraft and is used for protecting the normal and effective work of the internal radar antenna, and is not only a structural member of the aircraft, but also an important component of a guidance system. The radome is a structure/functional component integrating high performance requirements such as heat resistance, wave transmission, bearing, weather resistance and the like, and correspondingly, the material for the radome also meets the multifunctional integrated requirements. The wave-transmitting performance of the radome is closely related to the wall structure of the radome, the wave-transmitting performance of the radome with the thin-wall structure is excellent, but the thickness of the radome is thinner, so that the cooperation of broadband wave-transmitting and mechanical properties is difficult to realize, and how to obtain the radome with high wave-transmitting performance and high-strength negative pressure resistance is an important research and development direction of the technicians in the field to meet the requirements of the radome.
Disclosure of Invention
The invention provides a high-strength negative pressure resistant basalt fiber radome and a preparation method thereof, the method comprises the steps of preparing basalt fibers, forming a coated nano silicon dioxide layer on the surfaces of the basalt fibers, forming a boron nitride layer, preparing a braiding body, soaking in slurry, co-curing and sintering to obtain the radome, wherein the radome has a wave transmission rate of more than 90% within 0.1MHz-20GHz, a tensile strength of more than 350MPa and a bending strength of more than 100MPa, has good negative pressure resistant performance, and has controllable process, strong operability, high forming efficiency and more uniform product density distribution, and realizes low-cost and mass stable production of the high-performance radome.
A method for preparing a high-strength negative pressure resistant basalt fiber radome, which comprises the following steps:
1) Crushing basalt ore, mutually fusing the basalt ore, high-purity quartz sand, pyrophyllite, talcum and sepiolite according to a certain proportion, then pouring the basalt ore, rapidly cooling the basalt ore in deionized water, and then crushing and fusing the basalt ore again to form spinning solution; drawing the spinning solution to obtain basalt fiber precursor with low dielectric coefficient;
2) Placing the activated basalt fiber in a tube furnace, introducing silicon tetrachloride, mixed gas of oxygen and hydrogen, heating and preserving heat to obtain basalt fiber coated with nano silicon dioxide;
3) Placing the basalt fiber obtained in the step 2) into mixed gas of trimethyl borate and ammonia gas, heating and preserving heat to obtain nano silicon dioxide coated basalt fiber with the surface coated with boron nitride;
4) Stranding the fibers obtained in the step 3), weaving the fibers into fiber cloth, and then soaking the fiber cloth in an ethanol solution of vinyltriethoxysilane; taking out and drying;
5) Placing the fiber cloth obtained in the step 4) into a mold, then adopting vacuum introduction to inject slurry into the mold, and preserving heat to complete solidification of the slurry;
6) And placing the slurry in a constant temperature chamber, presintering at a low temperature, heating, introducing mixed gas of silicon tetrachloride and ammonia, preserving heat, and cooling to room temperature to obtain the high-strength negative pressure resistant basalt fiber radome.
Further, wherein in step 1): the mass ratio of basalt ore to high-purity quartz sand to pyrophyllite to talcum to sepiolite is 100:10-15:5-8:2-5:2-5.
Further, in the step 2), heating is carried out at 350-400 ℃, the temperature is kept for 3-5 hours, and cooling is carried out to room temperature, so that the basalt fiber coated with nano silicon dioxide is obtained.
Further, wherein in step 3): the molar ratio is 1:1, heating to 200-350 ℃ in the mixed gas of trimethyl borate and ammonia gas, and preserving heat for 3-5h.
Further wherein in step 4), the concentration of vinyltriethoxysilane in the ethanol solution is 5-10wt%.
Further, in the step 4), twisting a plurality of basalt fibers obtained in the step 3) into one strand by using a strand making machine, wherein the linear density of coarse sand is 1500-2400tex, and the gram weight of the fiber cloth is 200-800 g.m < -2 >.
Further, in the step 5), the slurry comprises 20-25 parts by mass of ethanol, 15-20 parts by mass of acetone, 2-4 parts by mass of triethyl phosphate, 0.5-1 part by mass of ammonium polyacrylate, 4-5 parts by mass of acrylamide, 1-2 parts by mass of polyethylene glycol, 40-50 parts by mass of silicon nitride whisker, 15-20 parts by mass of nano silicon dioxide and 0.3-0.5 part by mass of ammonium persulfate.
Further, in the step 6), the temperature is raised to 100-150 ℃, the temperature is kept for 3-5 hours, then the temperature is raised to 300-350 ℃, and the molar ratio is 3:4, preserving the temperature of the mixed gas of silicon tetrachloride and ammonia for 10-15h.
A high-strength negative pressure resistant basalt fiber radome is obtained by the preparation method.
The beneficial technical effects of the invention
1) In order to improve the combination property of basalt fiber cloth and silicon nitride, a boron nitride interface is deposited on the surface of basalt fiber in advance, the surface of boron nitride has good interface affinity with slurry of silicon nitride, meanwhile, the inventor finds that boron nitride can permeate into basalt fiber to damage the internal crystal structure of basalt fiber and lead the strength of basalt fiber to be reduced, therefore, a nano silicon dioxide barrier layer is arranged before depositing boron nitride to avoid the permeation of boron nitride, and in order to uniformly deposit the nano silicon dioxide barrier layer, after adjusting the composition of components in the process of preparing basalt fiber, the basalt fiber is quenched by cold water to lead the basalt fiber to have partial magnetism, thereby improving the deposition uniformity;
2) The basalt fiber cloth is soaked in the ethanol solution of the vinyl triethoxysilane, so that the wettability and the bonding performance between the basalt fiber cloth and the sizing agent can be improved, and the mechanical strength of the product is improved;
3) Aiming at the slurry, the fiber cloth has good infiltration performance and bonding performance, and simultaneously has lower dielectric constant and higher wave-transmitting rate;
4) After the slurry is sintered and solidified, the silicon nitride fills the gap of the radome by secondary heating of the mixed gas of silicon tetrachloride and ammonia gas, so that the porosity of the radome is reduced and the strength is improved.
Detailed Description
The present invention will be described more specifically with reference to examples and comparative examples, but the present invention is not limited to these examples within the scope of the present invention.
Example 1
1) Crushing basalt ore, mixing the basalt ore with high-purity quartz sand, pyrophyllite, talcum and sepiolite according to a certain proportion, wherein the mass ratio of the basalt ore to the high-purity quartz sand to the pyrophyllite to the talcum to the sepiolite is 100:12:6:4:3, a step of; melting at 1400 ℃, then pouring into deionized water for rapid cooling, then crushing again, and melting at 1300 ℃ to form spinning solution; drawing the spinning solution to obtain basalt fiber precursor with the diameter of 13 microns;
2) Placing the activated basalt fiber in a tube furnace, introducing silicon tetrachloride, mixed gas of oxygen and hydrogen, heating at 350 ℃, preserving heat for 5 hours, and cooling to room temperature to obtain basalt fiber coated with nano silicon dioxide;
3) Placing basalt fiber obtained in the step 2) in a mole ratio of 1:1, heating to 350 ℃ in mixed gas of trimethyl borate and ammonia gas, and preserving heat for 5 hours to obtain nano silicon dioxide coated basalt fiber with surface coated with boron nitride;
4) Twisting a plurality of basalt fibers obtained in the step 3) into one strand by using a strand making machine, wherein the linear density of coarse sand is 2000tex, and then spinning into fiber cloth, and the gram weight of the fiber cloth is 500 g.m -2 Then placing the mixture in an ethanol solution of vinyl triethoxysilane for infiltration, wherein the concentration of the vinyl triethoxysilane in the ethanol solution is 5wt%; taking out and drying;
5) Placing the fiber cloth obtained in the step 4) into a mold, and then injecting slurry into the mold, wherein the slurry comprises 20 parts by mass of ethanol, 15 parts by mass of acetone, 2 parts by mass of triethyl phosphate, 0.5 part by mass of ammonium polyacrylate, 4 parts by mass of acrylamide, 1 part by mass of polyethylene glycol, 40 parts by mass of silicon nitride whisker, 15 parts by mass of nano silicon dioxide and 0.3 part by mass of ammonium persulfate; preserving the temperature at 70 ℃ for 4 hours to finish solidification of the slurry;
6) Placing the slurry in a high-temperature furnace, heating to 150 ℃, preserving heat for 5 hours, heating to 350 ℃, and introducing the slurry with the molar ratio of 3:4, preserving heat for 15h, and cooling to room temperature to obtain the high-strength negative pressure resistant basalt fiber radome.
Example 2
1) Crushing basalt ore, mixing the basalt ore with high-purity quartz sand, pyrophyllite, talcum and sepiolite according to a certain proportion, wherein the mass ratio of the basalt ore to the high-purity quartz sand to the pyrophyllite to the talcum to the sepiolite is 100:12:6:4:3, a step of; melting at 1500 ℃, then pouring into deionized water for rapid cooling, then crushing again, and melting at 1350 ℃ to form spinning solution; drawing the spinning solution to obtain basalt fiber precursor with the diameter of 13 microns;
2) Placing the activated basalt fiber in a tube furnace, introducing silicon tetrachloride, mixed gas of oxygen and hydrogen, heating at 300 ℃, preserving heat for 3 hours, and cooling to room temperature to obtain basalt fiber coated with nano silicon dioxide;
3) Placing basalt fiber obtained in the step 2) in a mole ratio of 1:1, heating to 300 ℃ in mixed gas of trimethyl borate and ammonia gas, and preserving heat for 3 hours to obtain nano silicon dioxide coated basalt fiber with surface coated with boron nitride;
4) Twisting a plurality of basalt fibers obtained in the step 3) into one strand by using a strand making machine, wherein the linear density of coarse sand is 2000tex, and then spinning into fiber cloth, and the gram weight of the fiber cloth is 500 g.m -2 Then placing the mixture in an ethanol solution of vinyltriethoxysilane for infiltration, wherein the concentration of vinyltriethoxysilane in the ethanol solution is 10wt%; taking out and drying;
5) Placing the fiber cloth obtained in the step 4) into a mold, and then injecting slurry into the mold, wherein the slurry comprises 25 parts by mass of ethanol, 20 parts by mass of acetone, 4 parts by mass of triethyl phosphate, 1 part by mass of ammonium polyacrylate, 5 parts by mass of acrylamide, 2 parts by mass of polyethylene glycol, 50 parts by mass of silicon nitride whisker, 20 parts by mass of nano silicon dioxide and 0.5 part by mass of ammonium persulfate; preserving the temperature at 70 ℃ for 4 hours to finish solidification of the slurry;
6) Placing the slurry in a high-temperature furnace, heating to 100 ℃, preserving heat for 3 hours, heating to 350 ℃, and introducing the mixture with the molar ratio of 3:4, preserving heat for 10 hours, and cooling to room temperature to obtain the high-strength negative pressure resistant basalt fiber radome.
Example 3
1) Crushing basalt ore, mixing the basalt ore with high-purity quartz sand, pyrophyllite, talcum and sepiolite according to a certain proportion, wherein the mass ratio of the basalt ore to the high-purity quartz sand to the pyrophyllite to the talcum to the sepiolite is 100:12:6:4:3, a step of; melting at 1400 ℃, then pouring into deionized water for rapid cooling, then crushing again, and melting at 1350 ℃ to form spinning solution; drawing the spinning solution to obtain basalt fiber precursor with the diameter of 13 microns;
2) Placing the activated basalt fiber in a tube furnace, introducing silicon tetrachloride, mixed gas of oxygen and hydrogen, heating at 350 ℃, preserving heat for 4 hours, and cooling to room temperature to obtain basalt fiber coated with nano silicon dioxide;
3) Placing basalt fiber obtained in the step 2) in a mole ratio of 1:1, heating to 300 ℃ in mixed gas of trimethyl borate and ammonia gas, and preserving heat for 4 hours to obtain nano silicon dioxide coated basalt fiber with surface coated with boron nitride;
4) Twisting a plurality of basalt fibers obtained in the step 3) into one strand by using a strand making machine, wherein the linear density of coarse sand is 2000tex, and then spinning into fiber cloth, and the gram weight of the fiber cloth is 500 g.m -2 Then placing the mixture in an ethanol solution of vinyl triethoxysilane for infiltration, wherein the concentration of the vinyl triethoxysilane in the ethanol solution is 8wt%; taking out and drying;
5) Placing the fiber cloth obtained in the step 4) into a mold, and then injecting slurry into the mold, wherein the slurry comprises 22 parts by mass of ethanol, 18 parts by mass of acetone, 3 parts by mass of triethyl phosphate, 0.8 part by mass of ammonium polyacrylate, 4 parts by mass of acrylamide, 2 parts by mass of polyethylene glycol, 45 parts by mass of silicon nitride whisker, 18 parts by mass of nano silicon dioxide and 0.4 part by mass of ammonium persulfate; preserving the temperature at 70 ℃ for 4 hours to finish solidification of the slurry;
6) Placing the slurry in a high-temperature furnace, heating to 150 ℃, preserving heat for 4 hours, heating to 300 ℃, and introducing the slurry with the molar ratio of 3:4, preserving heat for 12 hours, and cooling to room temperature to obtain the high-strength negative pressure resistant basalt fiber radome.
Comparative example 1
1) Crushing basalt ore, and melting at 1300 ℃ to form spinning solution; drawing the spinning solution to obtain basalt fiber precursor with the diameter of 13 microns;
2) Placing basalt fiber obtained in the step 1) in a molar ratio of 1:1, heating to 300 ℃ in mixed gas of trimethyl borate and ammonia gas, and preserving heat for 5 hours to obtain basalt fiber with surface coated with boron nitride;
3) Twisting a plurality of basalt fibers obtained in the step 2) into one strand by using a strand making machine, wherein the linear density of coarse sand is 2000tex, and then spinning into fiber cloth, and the gram weight of the fiber cloth is 500 g.m -2 Then placing the mixture in an ethanol solution of vinyl triethoxysilane for infiltration, wherein the concentration of the vinyl triethoxysilane in the ethanol solution is 5wt%; taking out and drying;
4) Placing the fiber cloth obtained in the step 3) into a mold, and then injecting slurry into the mold, wherein the slurry comprises 20 parts by mass of ethanol, 15 parts by mass of acetone, 2 parts by mass of triethyl phosphate, 0.5 part by mass of ammonium polyacrylate, 4 parts by mass of acrylamide, 1 part by mass of polyethylene glycol, 40 parts by mass of silicon nitride whisker, 15 parts by mass of nano silicon dioxide and 0.3 part by mass of ammonium persulfate; preserving the temperature at 70 ℃ for 4 hours to finish solidification of the slurry;
5) And (3) placing the slurry in a high-temperature furnace, heating to 300 ℃, preserving heat for 5 hours, and cooling to room temperature to obtain the radome.
Comparative example 2
1) Crushing basalt ore, and melting at 1300 ℃ to form spinning solution; drawing the spinning solution to obtain basalt fiber precursor with the diameter of 13 microns;
2) Placing the activated basalt fiber in a tube furnace, introducing silicon tetrachloride, mixed gas of oxygen and hydrogen, heating at 350 ℃, preserving heat for 5 hours, and cooling to room temperature to obtain basalt fiber coated with nano silicon dioxide;
3) Placing basalt fiber obtained in the step 2) in a mole ratio of 1:1, heating to 300 ℃ in mixed gas of trimethyl borate and ammonia gas, and preserving heat for 5 hours to obtain nano silicon dioxide coated basalt fiber with surface coated with boron nitride;
4) Twisting a plurality of basalt fibers obtained in the step 3) into one strand by using a strand making machine, wherein the linear density of coarse sand is 2000tex, and then spinning into fiber cloth, and the gram weight of the fiber cloth is 500 g.m -2 Soaking in ethanol solution of vinyltriethoxysilane, and soaking in ethanol solution of ethyl acetateThe concentration of alkenyltriethoxysilane in the ethanol solution was 5wt%; taking out and drying;
5) Placing the fiber cloth obtained in the step 3) into a mold, and then injecting slurry into the mold, wherein the slurry comprises 20 parts by mass of ethanol, 15 parts by mass of acetone, 2 parts by mass of triethyl phosphate, 0.5 part by mass of ammonium polyacrylate, 4 parts by mass of acrylamide, 1 part by mass of polyethylene glycol, 40 parts by mass of silicon nitride whisker, 15 parts by mass of nano silicon dioxide and 0.3 part by mass of ammonium persulfate; preserving the temperature at 70 ℃ for 4 hours to finish solidification of the slurry;
6) And (3) placing the slurry in a high-temperature furnace, heating to 300 ℃, preserving heat for 5 hours, and cooling to room temperature to obtain the radome.
Comparative example 3
1) Crushing basalt ore, melting at 1400 ℃, then pouring into deionized water for rapid cooling, crushing again, and melting at 1300 ℃ to form spinning solution; drawing the spinning solution to obtain basalt fiber precursor with the diameter of 13 microns;
2) Placing the activated basalt fiber in a tube furnace, introducing silicon tetrachloride, mixed gas of oxygen and hydrogen, heating at 350 ℃, preserving heat for 5 hours, and cooling to room temperature to obtain basalt fiber coated with nano silicon dioxide;
3) Twisting a plurality of basalt fibers obtained in the step 2 into one strand by using a strand making machine, wherein the linear density of coarse sand is 2000tex, and then spinning into fiber cloth, and the gram weight of the fiber cloth is 500 g.m -2 Then placing the mixture in an ethanol solution of vinyl triethoxysilane for infiltration, wherein the concentration of the vinyl triethoxysilane in the ethanol solution is 5wt%; taking out and drying;
4) Placing the fiber cloth obtained in the step 3) into a mold, and then injecting slurry into the mold, wherein the slurry comprises 20 parts by mass of ethanol, 15 parts by mass of acetone, 2 parts by mass of triethyl phosphate, 0.5 part by mass of ammonium polyacrylate, 4 parts by mass of acrylamide, 1 part by mass of polyethylene glycol, 40 parts by mass of silicon nitride whisker, 15 parts by mass of nano silicon dioxide and 0.3 part by mass of ammonium persulfate; preserving the temperature at 70 ℃ for 4 hours to finish solidification of the slurry;
5) And (3) placing the slurry in a high-temperature furnace, heating to 300 ℃, preserving heat for 5 hours, and cooling to room temperature to obtain the radome.
Comparative example 4
1) Crushing basalt ore, melting at 1400 ℃, then pouring into deionized water for rapid cooling, crushing again, and melting at 1300 ℃ to form spinning solution; drawing the spinning solution to obtain basalt fiber precursor with the diameter of 13 microns;
2) Placing basalt fiber obtained in the step 1) in a molar ratio of 1:1, heating to 300 ℃ in mixed gas of trimethyl borate and ammonia gas, and preserving heat for 5 hours to obtain basalt fiber with surface coated with boron nitride;
3) Twisting a plurality of basalt fibers obtained in the step 2) into one strand by using a strand making machine, wherein the linear density of coarse sand is 2000tex, and then spinning into fiber cloth, and the gram weight of the fiber cloth is 500 g.m -2 Then placing the mixture in an ethanol solution of vinyl triethoxysilane for infiltration, wherein the concentration of the vinyl triethoxysilane in the ethanol solution is 5wt%; taking out and drying;
4) Placing the fiber cloth obtained in the step 3) into a mold, and then injecting slurry into the mold, wherein the slurry comprises 20 parts by mass of ethanol, 15 parts by mass of acetone, 2 parts by mass of triethyl phosphate, 0.5 part by mass of ammonium polyacrylate, 4 parts by mass of acrylamide, 1 part by mass of polyethylene glycol, 40 parts by mass of silicon nitride whisker, 15 parts by mass of nano silicon dioxide and 0.3 part by mass of ammonium persulfate; preserving the temperature at 70 ℃ for 4 hours to finish solidification of the slurry;
5) And (3) placing the slurry in a high-temperature furnace, heating to 300 ℃, preserving heat for 5 hours, and cooling to room temperature to obtain the radome.
Comparative example 5
1) Crushing basalt ore, melting at 1400 ℃, then pouring into deionized water for rapid cooling, crushing again, and melting at 1300 ℃ to form spinning solution; drawing the spinning solution to obtain basalt fiber precursor with the diameter of 13 microns;
2) Twisting a plurality of basalt fibers obtained in the step 1) into one strand by using a strand making machine, wherein the linear density of coarse sand is 2000tex, and then spinning into fiber cloth, and the gram weight of the fiber cloth is 500g DEG Cm -2 Then placing the mixture in an ethanol solution of vinyl triethoxysilane for infiltration, wherein the concentration of the vinyl triethoxysilane in the ethanol solution is 5wt%; taking out and drying;
3) Placing the fiber cloth obtained in the step 2) into a mold, and then injecting slurry into the mold, wherein the slurry comprises 20 parts by mass of ethanol, 15 parts by mass of acetone, 2 parts by mass of triethyl phosphate, 0.5 part by mass of ammonium polyacrylate, 4 parts by mass of acrylamide, 1 part by mass of polyethylene glycol, 40 parts by mass of silicon nitride whisker, 15 parts by mass of nano silicon dioxide and 0.3 part by mass of ammonium persulfate; preserving the temperature at 70 ℃ for 4 hours to finish solidification of the slurry;
4) And (3) placing the slurry in a high-temperature furnace, heating to 300 ℃, preserving heat for 5 hours, and cooling to room temperature to obtain the basalt fiber radome.
Comparative example 6
1) Crushing basalt ore, melting at 1400 ℃, then pouring into deionized water for rapid cooling, crushing again, and melting at 1300 ℃ to form spinning solution; drawing the spinning solution to obtain basalt fiber precursor with the diameter of 13 microns;
2) Placing the activated basalt fiber in a tube furnace, introducing silicon tetrachloride, mixed gas of oxygen and hydrogen, heating at 350 ℃, preserving heat for 5 hours, and cooling to room temperature to obtain basalt fiber coated with nano silicon dioxide;
3) Placing basalt fiber obtained in the step 2) in a mole ratio of 1:1, heating to 300 ℃ in mixed gas of trimethyl borate and ammonia gas, and preserving heat for 5 hours to obtain nano silicon dioxide coated basalt fiber with surface coated with boron nitride;
4) Twisting a plurality of basalt fibers obtained in the step 3) into one strand by using a strand making machine, wherein the linear density of coarse sand is 2000tex, and then spinning into fiber cloth, and the gram weight of the fiber cloth is 500 g.m -2 Then placing the mixture in an ethanol solution of vinyl triethoxysilane for infiltration, wherein the concentration of the vinyl triethoxysilane in the ethanol solution is 5wt%; taking out and drying;
5) Placing the fiber cloth obtained in the step 3) into a mold, and then injecting slurry into the mold, wherein the slurry comprises 20 parts by mass of ethanol, 15 parts by mass of acetone, 2 parts by mass of triethyl phosphate, 0.5 part by mass of ammonium polyacrylate, 4 parts by mass of acrylamide, 1 part by mass of polyethylene glycol, 40 parts by mass of silicon nitride whisker, 15 parts by mass of nano silicon dioxide and 0.3 part by mass of ammonium persulfate; preserving the temperature at 70 ℃ for 4 hours to finish solidification of the slurry;
6) And (3) placing the slurry in a high-temperature furnace, heating to 300 ℃, preserving heat for 5 hours, and cooling to room temperature to obtain the basalt fiber radome.
Comparative example 7
1) Crushing basalt ores; melting at 1400 ℃, then pouring into deionized water for rapid cooling, then crushing again, and melting at 1350 ℃ to form spinning solution; drawing the spinning solution to obtain basalt fiber precursor with the diameter of 13 microns;
2) Placing the activated basalt fiber in a tube furnace, introducing silicon tetrachloride, mixed gas of oxygen and hydrogen, heating at 350 ℃, preserving heat for 4 hours, and cooling to room temperature to obtain basalt fiber coated with nano silicon dioxide;
3) Placing basalt fiber obtained in the step 2) in a mole ratio of 1:1, heating to 300 ℃ in mixed gas of trimethyl borate and ammonia gas, and preserving heat for 4 hours to obtain nano silicon dioxide coated basalt fiber with surface coated with boron nitride;
4) Twisting a plurality of basalt fibers obtained in the step 3) into one strand by using a strand making machine, wherein the linear density of coarse sand is 2000tex, and then spinning into fiber cloth, and the gram weight of the fiber cloth is 500 g.m -2 Then placing the mixture in an ethanol solution of vinyl triethoxysilane for infiltration, wherein the concentration of the vinyl triethoxysilane in the ethanol solution is 8wt%; taking out and drying;
5) Placing the fiber cloth obtained in the step 4) into a mold, and then injecting slurry into the mold, wherein the slurry comprises 22 parts by mass of ethanol, 18 parts by mass of acetone, 3 parts by mass of triethyl phosphate, 0.8 part by mass of ammonium polyacrylate, 4 parts by mass of acrylamide, 2 parts by mass of polyethylene glycol, 45 parts by mass of silicon nitride whisker, 18 parts by mass of nano silicon dioxide and 0.4 part by mass of ammonium persulfate; preserving the temperature at 70 ℃ for 4 hours to finish solidification of the slurry;
6) Placing the slurry in a high-temperature furnace, heating to 150 ℃, preserving heat for 4 hours, heating to 300 ℃, and introducing the slurry with the molar ratio of 3:4, preserving heat for 12 hours, and cooling to room temperature to obtain the high-strength negative pressure resistant basalt fiber radome.
Experimental effect
The tensile and flexural strength, dielectric constant and wave transmittance of the samples obtained by the present invention are shown in Table 1.
TABLE 1
The data of the examples and the comparative examples show that other components are added to change the composition in the process of preparing basalt fibers, and the basalt fibers are quenched by cold water to enable the basalt fibers to have partial magnetism, so that the uniformity of nano silicon dioxide deposition is improved, a nano silicon dioxide barrier layer is arranged before boron nitride deposition, the penetration of boron nitride is avoided, the mechanical strength is improved, a boron nitride interface is deposited on the surface of the basalt fibers in advance, the surface of the boron nitride has good interface affinity with the sizing agent of silicon nitride, and the means of the invention plays a positive role in improving the mechanical strength and the negative pressure resistance of the radome, and simultaneously, the effects of low dielectric constant and high wave transmittance are maintained.
While the present invention has been described in detail through the foregoing description of the preferred embodiment, it should be understood that the foregoing description is not to be considered as limiting the invention.
Claims (9)
1. The preparation method of the high-strength negative pressure resistant basalt fiber radome is characterized by comprising the following steps of:
1) Crushing basalt ore, mutually fusing the basalt ore, high-purity quartz sand, pyrophyllite, talcum and sepiolite according to a certain proportion, then pouring the basalt ore, rapidly cooling the basalt ore in deionized water, and then crushing and fusing the basalt ore again to form spinning solution; drawing the spinning solution to obtain basalt fiber precursor with low dielectric coefficient;
2) Placing the activated basalt fiber in a tube furnace, introducing silicon tetrachloride, mixed gas of oxygen and hydrogen, heating and preserving heat to obtain basalt fiber coated with nano silicon dioxide;
3) Placing the basalt fiber obtained in the step 2) into mixed gas of trimethyl borate and ammonia gas, heating and preserving heat to obtain nano silicon dioxide coated basalt fiber with the surface coated with boron nitride;
4) Stranding the fibers obtained in the step 3), weaving the fibers into fiber cloth, and then soaking the fiber cloth in an ethanol solution of vinyltriethoxysilane; taking out and drying;
5) Placing the fiber cloth obtained in the step 4) into a mold, then adopting vacuum introduction to inject slurry into the mold, and preserving heat to complete solidification of the slurry;
6) And placing the slurry in a constant temperature chamber, presintering at a low temperature, heating, introducing mixed gas of silicon tetrachloride and ammonia, preserving heat, and cooling to room temperature to obtain the high-strength negative pressure resistant basalt fiber radome.
2. The method of claim 1, wherein in step 1): the mass ratio of basalt ore to high-purity quartz sand to pyrophyllite to talcum to sepiolite is 100:10-15:5-8:2-5:2-5.
3. The preparation method of claim 1, wherein in the step 2), the basalt fiber coated with nano silicon dioxide is obtained by heating at 350-400 ℃, preserving heat for 3-5 hours, and cooling to room temperature.
4. The method of claim 1, wherein in step 3): the molar ratio is 1:1, heating to 200-350 ℃ in the mixed gas of trimethyl borate and ammonia gas, and preserving heat for 3-5h.
5. The process according to claim 1, wherein in step 4), the concentration of vinyltriethoxysilane in the ethanol solution is from 5 to 10% by weight.
6. The method of claim 1, wherein in step 4), a plurality of basalt fibers obtained in step 3) are twisted into one strand by a strand machine, wherein the linear density of the coarse sand is 1500-2400tex, and the gram weight of the fiber cloth is 200-800 g.m -2 。
7. The method according to claim 1, wherein in step 5), the slurry comprises 20 to 25 parts by mass of ethanol, 15 to 20 parts by mass of acetone, 2 to 4 parts by mass of triethyl phosphate, 0.5 to 1 part by mass of ammonium polyacrylate, 4 to 5 parts by mass of acrylamide, 1 to 2 parts by mass of polyethylene glycol, 40 to 50 parts by mass of silicon nitride whisker, 15 to 20 parts by mass of nano silicon dioxide, and 0.3 to 0.5 part by mass of ammonium persulfate.
8. The method according to claim 1, wherein in step 6), the temperature is raised to 100-150 ℃, the temperature is kept for 3-5 hours, then the temperature is raised to 300-350 ℃, and the molar ratio is 3:4, preserving the temperature of the mixed gas of silicon tetrachloride and ammonia for 10-15h.
9. A high strength negative pressure resistant basalt fiber radome, characterized in that the radome is obtained by the manufacturing method of any one of claims 1 to 8.
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