CN116283237A - Low-thermal-conductivity silicon nitride wave-transparent ceramic material and preparation method thereof - Google Patents
Low-thermal-conductivity silicon nitride wave-transparent ceramic material and preparation method thereof Download PDFInfo
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- CN116283237A CN116283237A CN202310020466.7A CN202310020466A CN116283237A CN 116283237 A CN116283237 A CN 116283237A CN 202310020466 A CN202310020466 A CN 202310020466A CN 116283237 A CN116283237 A CN 116283237A
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 74
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000835 fiber Substances 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 23
- 239000002904 solvent Substances 0.000 claims abstract description 23
- 238000000498 ball milling Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000000748 compression moulding Methods 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 21
- 238000005245 sintering Methods 0.000 claims abstract description 20
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000005011 phenolic resin Substances 0.000 claims abstract description 19
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000003605 opacifier Substances 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000007873 sieving Methods 0.000 claims abstract description 10
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 5
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims description 5
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 4
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 229910021426 porous silicon Inorganic materials 0.000 abstract description 3
- 239000012780 transparent material Substances 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- VWQVUPCCIRVNHF-OUBTZVSYSA-N Yttrium-90 Chemical group [90Y] VWQVUPCCIRVNHF-OUBTZVSYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical group O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 230000008054 signal transmission Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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Abstract
The invention relates to the technical field of silicon nitride functional ceramic materials, and provides a low-heat-conductivity silicon nitride wave-transparent ceramic material and a preparation method thereof. The method comprises the steps of mixing raw materials of silicon nitride chopped fibers, a light shielding agent, aluminum oxide, yttrium oxide, phenolic resin and a solvent, and then performing ball milling to obtain a wet mixed material; and then sequentially drying, sieving and compression molding to obtain a blank, and finally performing gradient sintering to obtain the low-heat-conductivity silicon nitride wave-transparent ceramic material. According to the invention, the silicon nitride chopped fiber and the opacifier are matched for use, so that the thermal conductivity of the silicon nitride wave-transparent ceramic material is reduced, and the strength of the silicon nitride wave-transparent ceramic material is improved by adding the phenolic resin; by using a specific gradient sintering process, the porous silicon nitride wave-transparent ceramic material is obtained, so that the heat conductivity is further reduced, the dielectric constant is reduced, and the problem of strength reduction caused by a pore-forming agent is avoided.
Description
Technical Field
The invention relates to the technical field of silicon nitride functional ceramic materials, in particular to a low-heat-conductivity silicon nitride wave-transparent ceramic material and a preparation method thereof.
Background
The radome is an important component for protecting the normal work of the aircraft radar antenna in the service environment, and adopts wave-transparent materials to realize electromagnetic signal transmission. With the development of high-speed aircrafts, the ever-increasing flying speed and the severe service environment put strict requirements on the thermal protection performance, mechanical performance and environmental performance of wave-transparent materials. The development of high-temperature wave-transparent materials with excellent comprehensive properties has become a difficult point and an important point of research.
Among the numerous high temperature wave-transparent material systems, silicon nitride-based ceramics have gained extensive attention from researchers due to their excellent mechanical properties, resistance to rain erosion and sand erosion, and good thermal stability, and are considered to be one of the most potential high temperature wave-transparent materials.
Silicon nitride ceramics applied to radomes in special fields are required to meet the comprehensive characteristics of high strength, low thermal conductivity and low dielectric constant. In the prior art, in order to pursue low thermal conductivity and low dielectric constant, a large amount of pore-forming agents are added in the preparation process of the silicon nitride ceramic material, and the mechanical strength of the material is often seriously reduced by the method. Therefore, it is needed to provide a preparation method of a silicon nitride wave-transparent ceramic material which simultaneously satisfies the comprehensive characteristics of high strength, low thermal conductivity and low dielectric constant.
Disclosure of Invention
In view of the above, the present invention aims to provide a low thermal conductivity silicon nitride wave-transparent ceramic material and a preparation method thereof. The silicon nitride wave-transparent ceramic material obtained by the preparation method provided by the invention has the characteristics of high strength, low thermal conductivity and low dielectric constant.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a low-thermal-conductivity silicon nitride wave-transparent ceramic material, which comprises the following steps:
(1) Mixing raw materials of silicon nitride chopped fibers, a light shielding agent, aluminum oxide, yttrium oxide, phenolic resin and a solvent, and performing ball milling to obtain a wet mixed material;
(2) Sequentially drying, sieving and compression molding the wet mixed material obtained in the step (1) to obtain a blank;
(3) Performing gradient sintering on the blank obtained in the step (2) to obtain a low-heat-conductivity silicon nitride wave-transparent ceramic material;
wherein, the gradient sintering process is as follows: raising the temperature to 500-600 ℃ at a heating rate of 1 ℃/min, and preserving the temperature for 1-1.5 h, wherein the atmosphere is vacuum; then the temperature is raised to 1300-1800 ℃ at the heating rate of 10 ℃/min, and the temperature is kept for 0.5-3 h, and the atmosphere is nitrogen.
Preferably, the raw materials in the step (1) are used in parts by weight: 60-90 parts of silicon nitride chopped fiber, 3-5 parts of opacifier, 5-10 parts of alumina, 5-10 parts of yttrium oxide, 10-20 parts of phenolic resin and 80-100 parts of solvent.
Preferably, the opacifier in the step (1) comprises at least one of zirconium silicate, zirconium oxide, titanium oxide and potassium hexatitanate.
Preferably, the length of the silicon nitride chopped fiber in the step (1) is 0.1 to 80mm.
Preferably, the solvent in the step (1) is ethanol and/or methanol.
Preferably, the ball milling time in the step (1) is 10-20 h, and the ball milling rotating speed is 200-350 r/min.
Preferably, the temperature of the drying in the step (2) is 40-80 ℃, and the drying time is 60-120 min.
Preferably, the mesh number of the sieving in the step (2) is more than or equal to 40 meshes.
Preferably, the pressure of the compression molding in the step (2) is 150-200 MPa, and the compression molding time is 0.5-3 min.
The invention also provides the low-thermal-conductivity silicon nitride wave-transparent ceramic material prepared by the preparation method.
The invention provides a preparation method of a low-thermal-conductivity silicon nitride wave-transparent ceramic material, which comprises the following steps: (1) Mixing raw materials of silicon nitride chopped fibers, a light shielding agent, aluminum oxide, yttrium oxide, phenolic resin and a solvent, and performing ball milling to obtain a wet mixed material; (2) Sequentially drying, sieving and compression molding the wet mixed material obtained in the step (1) to obtain a blank; (3) Performing gradient sintering on the blank obtained in the step (1) to obtain a low-heat-conductivity silicon nitride wave-transparent ceramic material; wherein, the gradient sintering process is as follows: raising the temperature to 500-600 ℃ at a heating rate of 1 ℃/min, and preserving the temperature for 1-1.5 h, wherein the atmosphere is vacuum; then the temperature is raised to 1300-1800 ℃ at the heating rate of 10 ℃/min, and the temperature is kept for 0.5-3 h, and the atmosphere is nitrogen. According to the invention, the silicon nitride chopped fiber and the opacifier are matched for use, so that the thermal conductivity of the silicon nitride wave-transparent ceramic material is reduced, and the strength of the silicon nitride wave-transparent ceramic material is improved by adding the phenolic resin; by using a specific gradient sintering process, the porous silicon nitride wave-transparent ceramic material is obtained, so that the heat conductivity is further reduced, the dielectric constant is reduced, and the problem of strength reduction caused by a pore-forming agent is avoided. Experimental results show that the low-thermal-conductivity silicon nitride wave-transparent ceramic material obtained by the preparation method provided by the invention has a normal-temperature dielectric constant of 1.5-1.8, a normal-temperature thermal conductivity of 0.02-0.04 w/m.k and a bending strength of 480-500 MPa.
Detailed Description
The invention provides a preparation method of a low-thermal-conductivity silicon nitride wave-transparent ceramic material, which comprises the following steps:
(1) Mixing raw materials of silicon nitride chopped fibers, a light shielding agent, aluminum oxide, yttrium oxide, phenolic resin and a solvent, and performing ball milling to obtain a wet mixed material;
(2) Sequentially drying, sieving and compression molding the wet mixed material obtained in the step (1) to obtain a blank;
(3) And (3) carrying out gradient sintering on the blank obtained in the step (2) to obtain the low-heat-conductivity silicon nitride wave-transparent ceramic material.
The invention mixes the raw materials of silicon nitride chopped fiber, opacifier, alumina, yttrium oxide, phenolic resin and solvent and then carries out ball milling to obtain wet mixed materials.
In the present invention, the raw materials used are all conventional commercial products in the art unless otherwise specified.
In the present invention, the light-shielding agent preferably includes at least one of zirconium silicate, zirconium oxide, titanium oxide, and potassium hexatitanate, more preferably at least one of zirconium silicate, zirconium oxide, and titanium oxide. In the invention, the opacifier has the effect of preventing heat transfer, thereby reducing the thermal conductivity of the silicon nitride wave-transparent ceramic material.
In the present invention, the length of the silicon nitride chopped fiber is preferably 0.1 to 80mm, more preferably 1 to 50mm. The invention utilizes the characteristics of low heat conductivity and good dielectric property of the silicon nitride chopped fiber to reduce the dielectric constant of the silicon nitride wave-transparent ceramic material, and simultaneously, the heat conductivity of the material is further reduced by matching with the use of a light shielding agent.
In the present invention, the solvent is preferably ethanol and/or methanol, more preferably ethanol. According to the invention, ethanol is added into the raw materials, so that the subsequent ball milling operation is facilitated.
In the invention, the aluminum oxide can improve the wear resistance, corrosion resistance and high temperature resistance of the silicon nitride wave-transparent ceramic material. In the invention, the yttrium oxide can improve the wave-transmitting performance of the silicon nitride wave-transmitting ceramic material. In the invention, the phenolic resin can bond the raw materials together, which is beneficial to the material molding, and can improve the strength of the silicon nitride wave-transparent ceramic material.
In the present invention, the raw materials preferably include, by weight, 60 to 90 parts of a silicon nitride chopped fiber, 3 to 5 parts of a light-shielding agent, 5 to 10 parts of alumina, 5 to 10 parts of yttria, 10 to 20 parts of a phenolic resin, and 80 to 100 parts of a solvent, more preferably 80 to 85 parts of a silicon nitride chopped fiber, 3.5 to 4.5 parts of a light-shielding agent, 6 to 8 parts of alumina, 6 to 8 parts of yttria, 15 to 18 parts of a phenolic resin, and 85 to 90 parts of a solvent. The invention controls the dosage of the raw materials in the range, and the obtained low-heat conductivity silicon nitride wave-transparent ceramic material has better comprehensive performance.
In the present invention, the time of the ball milling is preferably 10 to 20 hours, more preferably 15 to 18 hours; the rotation speed of the ball mill is preferably 200-350 r/min, more preferably 250-300 r/min. The invention can further realize the full mixing of materials by ball milling, and is beneficial to crushing the raw materials to the required granularity, thereby improving the compactness of the prepared low-heat-conductivity silicon nitride wave-transparent ceramic material.
The mixing mode is not particularly limited in the invention, and the raw materials are fully and uniformly mixed by adopting a mixing mode well known to a person skilled in the art.
After the wet mixed material is obtained, the wet mixed material is dried, sieved and compression molded in sequence to obtain a blank.
In the present invention, the temperature of the drying is preferably 40 to 80 ℃, more preferably 50 to 70 ℃; the drying time is preferably 60 to 120 minutes, more preferably 80 to 110 minutes. The invention limits the temperature and time of the drying to the above range, which is beneficial to fully removing the solvent in the wet mixed material.
In the present invention, the number of the sieved mesh is preferably not less than 40 mesh, more preferably not less than 60 mesh. The invention limits the mesh number of the sieving to the above range, which is beneficial to obtaining silicon nitride ceramic material with compact structure.
In the present invention, the pressure of the compression molding is preferably 150 to 200MPa, more preferably 160 to 180MPa; the time for the compression molding is preferably 0.5 to 3 minutes, more preferably 1 to 2 minutes. The pressure and the time of the compression molding are limited in the range, so that the method is favorable for fully compressing and molding the raw materials and the later sintering process, and the silicon nitride ceramic material with better comprehensive performance is obtained.
After the blank is obtained, the blank is subjected to gradient sintering, so that the low-heat-conductivity silicon nitride wave-transparent ceramic material is obtained.
In the invention, the gradient sintering process is as follows: raising the temperature to 500-600 ℃ at a heating rate of 1 ℃/min, and preserving the temperature for 1-1.5 h, wherein the atmosphere is vacuum; then raising the temperature to 1300-1800 ℃ at a heating rate of 10 ℃/min, and preserving the temperature for 0.5-3 h under the atmosphere of nitrogen; preferably, the temperature is raised to 550 ℃ at a heating rate of 1 ℃/min, the temperature is kept for 1.5 hours, and the atmosphere is vacuum; then the temperature is raised to 1400 ℃ at a heating rate of 10 ℃/min, and the temperature is kept for 3 hours under the atmosphere of nitrogen. The gradient sintering process is favorable for obtaining the porous silicon nitride wave-transparent ceramic material, thereby further reducing the heat conductivity, simultaneously reducing the dielectric constant and avoiding the problem of strength reduction caused by pore formers.
The invention also provides the low-thermal-conductivity silicon nitride wave-transparent ceramic material prepared by the preparation method. In the invention, the low-heat conductivity silicon nitride wave-transparent ceramic material has a normal temperature dielectric constant of 1.5-1.8, a normal temperature heat conductivity of 0.02-0.04 w/m.k and a bending strength of 480-500 MPa.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention. The described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The preparation method of the low-heat-conductivity silicon nitride wave-transparent ceramic material comprises the following steps:
(1) Mixing raw materials of silicon nitride chopped fibers, a light shielding agent, aluminum oxide, yttrium oxide, phenolic resin and a solvent, and performing ball milling to obtain a wet mixed material;
wherein the length of the silicon nitride chopped fiber is 1-30 mm, the opacifier is zirconium silicate, and the solvent is ethanol; 80 parts by weight of silicon nitride chopped fiber, 4 parts by weight of opacifier, 8 parts by weight of alumina, 15 parts by weight of yttrium oxide, and 90 parts by weight of phenolic resin and solvent; the ball milling time is 16 hours, and the ball milling rotating speed is 300r/min;
(2) Sequentially drying, sieving and compression molding the wet mixed material obtained in the step (1) to obtain a blank;
wherein the drying temperature is 80 ℃ and the drying time is 100min; the mesh number of the sieve is 65 meshes; the pressure of compression molding is 160MPa, and the time of compression molding is 2min;
(3) Performing gradient sintering on the blank obtained in the step (2) to obtain a low-heat-conductivity silicon nitride wave-transparent ceramic material;
wherein, the gradient sintering process is as follows: raising the temperature to 550 ℃ at a heating rate of 1 ℃/min, and preserving the temperature for 1.5 hours, wherein the atmosphere is vacuum; then the temperature is raised to 1400 ℃ at a heating rate of 10 ℃/min, and the temperature is kept for 3 hours under the atmosphere of nitrogen.
Example 2
The preparation method of the low-heat-conductivity silicon nitride wave-transparent ceramic material comprises the following steps:
(1) Mixing raw materials of silicon nitride chopped fibers, a light shielding agent, aluminum oxide, yttrium oxide, phenolic resin and a solvent, and performing ball milling to obtain a wet mixed material;
wherein the length of the silicon nitride chopped fiber is 1-30 mm, the opacifier is zirconia, and the solvent is ethanol; the weight parts of the silicon nitride chopped fiber, the opacifier, the alumina, the yttrium oxide, the phenolic resin and the solvent are respectively 90 parts, 5 parts, 9 parts, 18 parts and 95 parts; the ball milling time is 18 hours, and the ball milling rotating speed is 300r/min;
(2) Sequentially drying, sieving and compression molding the wet mixed material obtained in the step (1) to obtain a blank;
wherein the drying temperature is 80 ℃ and the drying time is 110min; the mesh number of the sieve is 65 meshes; the pressure of compression molding is 180MPa, and the time of compression molding is 1min;
(3) Performing gradient sintering on the blank obtained in the step (2) to obtain a low-heat-conductivity silicon nitride wave-transparent ceramic material;
wherein, the gradient sintering process is as follows: raising the temperature to 550 ℃ at a heating rate of 1 ℃/min, and preserving the temperature for 1.5 hours, wherein the atmosphere is vacuum; then the temperature is raised to 1400 ℃ at a heating rate of 10 ℃/min, and the temperature is kept for 3 hours under the atmosphere of nitrogen.
Example 3
The preparation method of the low-heat-conductivity silicon nitride wave-transparent ceramic material comprises the following steps:
(1) Mixing raw materials of silicon nitride chopped fibers, a light shielding agent, aluminum oxide, yttrium oxide, phenolic resin and a solvent, and performing ball milling to obtain a wet mixed material;
wherein the length of the silicon nitride chopped fiber is 1-30 mm, the opacifier is titanium oxide, and the solvent is ethanol; 80 parts by weight of silicon nitride chopped fiber, 4 parts by weight of opacifier, 6 parts by weight of alumina, 13 parts by weight of yttrium oxide, and 90 parts by weight of phenolic resin and solvent; the ball milling time is 18 hours, and the ball milling rotating speed is 300r/min;
(2) Sequentially drying, sieving and compression molding the wet mixed material obtained in the step (1) to obtain a blank;
wherein the drying temperature is 80 ℃ and the drying time is 110min; the mesh number of the sieve is 65 meshes; the pressure of compression molding is 180MPa, and the time of compression molding is 1min;
(3) Performing gradient sintering on the blank obtained in the step (2) to obtain a low-heat-conductivity silicon nitride wave-transparent ceramic material;
wherein, the gradient sintering process is as follows: raising the temperature to 550 ℃ at a heating rate of 1 ℃/min, and preserving the temperature for 1.5 hours, wherein the atmosphere is vacuum; then the temperature is raised to 1400 ℃ at a heating rate of 10 ℃/min, and the temperature is kept for 3 hours under the atmosphere of nitrogen.
The low thermal conductivity silicon nitride wave-transparent ceramic materials prepared in examples 1 to 3 were tested for dielectric constant by a resonant cavity method; testing the thermal conductivity by using an ASTM E1461 laser scattering method; the flexural strength was tested using GBT 4741-1999. The test results are shown in Table 1.
Table 1 results of performance test of low thermal conductivity silicon nitride wave-transparent ceramic materials prepared in examples 1 to 3
As can be seen from the data provided in Table 1, the low thermal conductivity silicon nitride wave-transparent ceramic material obtained by the preparation method provided by the invention has a dielectric constant of 1.5-1.8 at normal temperature, a thermal conductivity of 0.02-0.04 w/m.k at normal temperature and a flexural strength of 480-500 MPa.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. A preparation method of a low-thermal-conductivity silicon nitride wave-transparent ceramic material comprises the following steps:
(1) Mixing raw materials of silicon nitride chopped fibers, a light shielding agent, aluminum oxide, yttrium oxide, phenolic resin and a solvent, and performing ball milling to obtain a wet mixed material;
(2) Sequentially drying, sieving and compression molding the wet mixed material obtained in the step (1) to obtain a blank;
(3) Performing gradient sintering on the blank obtained in the step (2) to obtain a low-heat-conductivity silicon nitride wave-transparent ceramic material;
wherein, the gradient sintering process is as follows: raising the temperature to 500-600 ℃ at a heating rate of 1 ℃/min, and preserving the temperature for 1-1.5 h, wherein the atmosphere is vacuum; then the temperature is raised to 1300-1800 ℃ at the heating rate of 10 ℃/min, and the temperature is kept for 0.5-3 h, and the atmosphere is nitrogen.
2. The preparation method according to claim 1, wherein the raw materials in the step (1) are used in the following amounts in parts by weight: 60-90 parts of silicon nitride chopped fiber, 3-5 parts of opacifier, 5-10 parts of alumina, 5-10 parts of yttrium oxide, 10-20 parts of phenolic resin and 80-100 parts of solvent.
3. The method according to claim 1 or 2, wherein the light-shielding agent in the step (1) comprises at least one of zirconium silicate, zirconium oxide, titanium oxide and potassium hexatitanate.
4. The method according to claim 1 or 2, wherein the length of the silicon nitride chopped fiber in the step (1) is 0.1 to 80mm.
5. The process according to claim 1 or 2, wherein the solvent in step (1) is ethanol and/or methanol.
6. The method according to claim 1, wherein the ball milling time in the step (1) is 10 to 20 hours, and the rotational speed of the ball milling is 200 to 350r/min.
7. The method according to claim 1, wherein the temperature of the drying in the step (2) is 40 to 80 ℃ and the drying time is 60 to 120min.
8. The method according to claim 1, wherein the mesh number of the screen in the step (2) is not less than 40 mesh.
9. The method according to claim 1, wherein the pressure of the compression molding in the step (2) is 150 to 200MPa, and the time of the compression molding is 0.5 to 3min.
10. A low thermal conductivity silicon nitride wave-transparent ceramic material prepared by the preparation method of any one of claims 1 to 9.
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