CN117926469A - High-temperature-resistant wave-absorbing silicon carbide nanofiber and preparation method thereof - Google Patents
High-temperature-resistant wave-absorbing silicon carbide nanofiber and preparation method thereof Download PDFInfo
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- CN117926469A CN117926469A CN202410125175.9A CN202410125175A CN117926469A CN 117926469 A CN117926469 A CN 117926469A CN 202410125175 A CN202410125175 A CN 202410125175A CN 117926469 A CN117926469 A CN 117926469A
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- 239000002121 nanofiber Substances 0.000 title claims abstract description 56
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 28
- 229920003257 polycarbosilane Polymers 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- 229920000642 polymer Polymers 0.000 claims abstract description 13
- 239000002135 nanosheet Substances 0.000 claims abstract description 12
- 230000003647 oxidation Effects 0.000 claims abstract description 9
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 9
- 230000008569 process Effects 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 27
- 239000002243 precursor Substances 0.000 claims description 16
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 14
- 238000009987 spinning Methods 0.000 claims description 14
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000004132 cross linking Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000000138 intercalating agent Substances 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000005530 etching Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 230000007613 environmental effect Effects 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 2
- 238000003486 chemical etching Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052799 carbon Inorganic materials 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- 239000010936 titanium Substances 0.000 description 13
- 239000000835 fiber Substances 0.000 description 7
- 239000011358 absorbing material Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000001419 dependent effect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000005291 magnetic effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- DXZIFGZIQQRESB-UHFFFAOYSA-N [C].[Ti].[Si] Chemical compound [C].[Ti].[Si] DXZIFGZIQQRESB-UHFFFAOYSA-N 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000005298 paramagnetic effect Effects 0.000 description 1
- 238000002464 physical blending Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 description 1
- 230000035899 viability Effects 0.000 description 1
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Abstract
The invention discloses a high-temperature-resistant wave-absorbing silicon carbide nanofiber and a preparation method thereof, wherein a two-dimensional Ti 3C2Tx nano sheet is introduced into a polycarbosilane solution, and the high-temperature-resistant wave-absorbing silicon carbide nanofiber is prepared by utilizing electrostatic spinning and a polymer conversion process; the surface of the prepared nanofiber consists of an amorphous Si-O-C phase, the core consists of two-dimensional Ti 3C2Tx nano sheets, crystal SiC particles and free carbon which are distributed in a discrete mode, the purpose of adjusting and controlling the wave absorbing performance within a certain range can be achieved by adjusting the adding proportion and the technological parameters of raw materials, the minimum reflection loss can reach-48.58 dB, the corresponding radar wave frequency is 10.16GHz, the thickness is 2.5mm, the effective absorption bandwidth can reach 3.12GHz, and the high-temperature oxidation resistance temperature can reach 1400 ℃.
Description
Technical Field
The invention belongs to the field of high-temperature-resistant wave-absorbing materials, and particularly relates to a high-temperature-resistant wave-absorbing silicon carbide nanofiber and a preparation method thereof.
Background
The high-temperature-resistant wave-absorbing material has important significance and practical application value for improving the stealth and viability of hypersonic aircrafts. With the continuous breakthrough of the flying speed (> Mach 5), the strong pneumatic friction can lead to the rapid rise of the surface temperature (> 1000 ℃) of the aircraft, so that the wave-absorbing material commonly used in the market at present has serious failure problem. For example: the higher temperature can lead most of carbon-based and high-molecular wave-absorbing materials to be chemically decomposed, and the magnetic wave-absorbing materials are paramagnetic transformed when the Curie temperature is exceeded, so that the magnetic loss capacity is lost, and the stealth requirement of high-temperature parts of the hypersonic aircraft cannot be met.
Silicon carbide is used as a typical semiconductor ceramic material, and has great application potential in the field of high-temperature wave absorption by virtue of the advantages of high temperature resistance, high strength, low density, stable chemical property, adjustable dielectric property and the like. Among the numerous preparation methods, the polymer conversion method is beneficial to the design of the appearance of a complex structure and the mass industrialized production, and the obtained polymer conversion silicon carbide consists of crystal SiC particles, amorphous Si-O-C phase and free carbon. The method is influenced by factors such as phase distribution, size, conversion rate and the like, so that the resistivity is higher, the dielectric loss capacity is limited, the overall wave-absorbing performance is not ideal (the minimum reflection loss is in the vicinity of-20 dB), and a large modification and improvement space is still reserved.
The second phase component is introduced into the silicon carbide fiber by a physical blending or chemical doping method to remarkably improve the wave absorbing performance of the silicon carbide fiber, for example, patent CN 115538155B discloses a preparation method for producing a titanium silicon carbon layer and a carbon nano tube layer on the surface of the silicon carbide fiber in situ, and patent CN 115802730A discloses a preparation method for loading tungsten disulfide on the surface of the silicon carbide fiber. Although the wave absorbing performance is significantly improved, specific performance indexes of service in a high-temperature environment are not involved.
In view of this, there is a need to develop high performance radar wave absorbing materials that are resistant to high temperatures in combination with strong absorption to meet the stringent demands of hypersonic aircraft manufacturing.
The invention comprises the following steps:
The invention mainly aims to provide a high-temperature-resistant wave-absorbing silicon carbide nanofiber material and a preparation method thereof, so as to solve the problems of higher resistivity, weak dielectric loss capacity, low minimum reflection loss and narrow effective wave-absorbing bandwidth of the traditional polymer converted silicon carbide fiber, and simultaneously meet the high-temperature-resistant use requirement of more than 1400 ℃.
In order to achieve the purpose, the two-dimensional Ti 3C2Tx nano-sheets are introduced into a polycarbosilane solution, and the high-temperature-resistant wave-absorbing silicon carbide nano-fibers are prepared by utilizing electrostatic spinning and a polymer conversion process, and the specific technical scheme is as follows:
the preparation method of the high-temperature-resistant wave-absorbing silicon carbide nanofiber comprises the following steps of:
Step 1, ti 3AlC2 powder is selected as a raw material, a mixed aqueous solution of HF, HCl and deionized water is used as an etchant, a LiCl aqueous solution is used as an intercalating agent, and a two-dimensional Ti 3C2Tx nano-sheet is prepared by a chemical etching method;
Step 2, preparing a polycarbosilane solution, adding the two-dimensional Ti 3C2Tx nano-sheets obtained in the step 1 into the polycarbosilane solution, and then performing strong ultrasonic and stirring treatment to obtain a uniformly dispersed electrostatic spinning solution;
step 3, transferring the electrostatic spinning solution obtained in the step 2 into an injector for electrostatic spinning, and obtaining a nanofiber precursor by controlling electrostatic spinning voltage, receiving distance, spinning temperature, environmental humidity and spinning advancing speed;
And 4, transferring the nanofiber precursor obtained in the step 3 to a drying oven for thermal oxidation crosslinking, and then transferring to a vacuum furnace for polymer conversion to obtain the high-temperature-resistant wave-absorbing silicon carbide nanofiber.
Further, the specific practice of the step 1 is as follows: slowly adding 2g of Ti 3AlC2 powder into 50mL of etching agent, stirring at 35 ℃ for 12h, repeatedly centrifuging, and cleaning until the pH value is neutral; collecting precipitate, adding into 40mL of intercalating agent, stirring at room temperature for 12h, cleaning, centrifuging, collecting supernatant, suction filtering, and drying at room temperature for 12h; wherein, the composition ratio of the etchant is 20mL50wt% HF, 20mL 37wt% HCl and 10mL deionized water, and the intercalating agent is 40mL2gLiCl aqueous solution.
Further, the polycarbosilane solution in the step 2 consists of 0.5g of polycarbosilane, 0.9-1.1 g of polyvinylpyrrolidone, 4-6 mL of absolute ethyl alcohol and 6mL of tetrahydrofuran.
Further, in the step 2, the average molecular weight of the polycarbosilane is between 1000 and 2000, the softening point temperature is between 180 and 200 ℃, and the residual weight rate at 1000 ℃ under the protection of N 2 is more than 57 percent.
Further, the electrostatic spinning process parameters in the step 3 are as follows: the spinning voltage is 16-20 kV, the receiving distance is 18-22 cm, the spinning temperature is 20-30 ℃, the ambient humidity is 10-30%, and the advancing speed of the spinning solution is 0.0010mm/s.
Further, the specific implementation of the step 4 is as follows: transferring the nanofiber precursor obtained in the step 3 to a drying oven for thermal oxidation crosslinking, wherein the thermal oxidation crosslinking temperature is 180-200 ℃, the heat preservation time is 2h, the atmosphere requirement is air, then transferring the nanofiber precursor into a vacuum furnace for polymer conversion, the polymer conversion temperature is 1300-1500 ℃, the heating rate is 3-5 ℃/min, the heat preservation time is 2h, and the atmosphere requirement is argon or vacuum.
Compared with the prior art, the invention has the beneficial effects that:
the high-temperature-resistant wave-absorbing silicon carbide nanofiber surface is composed of amorphous Si-O-C phases, so that impedance matching between the fiber and a free space can be remarkably improved, and introduction and subsequent absorption of radar waves are promoted.
The high-temperature-resistant wave-absorbing silicon carbide nanofiber core consists of two-dimensional Ti 3C2Tx nano sheets, crystal SiC particles and free carbon which are distributed in a discrete mode, an intercommunicating conductive network is built among the three, and the conductivity loss capacity is remarkably improved and the polarization loss capacity is promoted.
The high-temperature-resistant wave-absorbing silicon carbide nanofiber can change the size, shape and distribution of each component by adjusting the addition proportion and the technological parameters of raw materials, and achieve the purpose of adjusting and controlling the wave-absorbing performance within a certain range as required.
The minimum reflection loss of the high-temperature-resistant wave-absorbing silicon carbide nanofiber can reach-48.58 dB, the corresponding radar wave frequency is 10.16GHz, the thickness is 2.5mm, and the effective absorption bandwidth can reach 3.12GHz.
The high-temperature oxidation resistance temperature of the high-temperature resistant wave-absorbing silicon carbide nanofiber can reach 1400 ℃, and the high-temperature resistant wave-absorbing silicon carbide nanofiber has the best high-temperature resistance in the radar wave-absorbing silicon carbide nanofiber.
Drawings
FIG. 1 is a scanning electron microscope image of a high temperature resistant wave-absorbing silicon carbide nanofiber prepared in example 1 of the present invention.
Fig. 2 is a graph of real and imaginary parts of frequency-dependent dielectric constants of the high temperature resistant wave-absorbing silicon carbide nanofibers prepared in example 1 of the present invention.
Fig. 3 is a graph showing the minimum reflection loss of the high temperature resistant wave-absorbing silicon carbide nanofiber prepared in example 1 of the present invention at different thicknesses.
Detailed Description
The invention will be described in detail below with reference to the drawings and the detailed description.
The invention provides a preparation method of high-temperature-resistant wave-absorbing silicon carbide nanofiber, which comprises the following steps:
Step 1, slowly adding 2g of Ti 3AlC2 powder into 50mL of etching agent (the composition ratio of the etching agent is 20mL of 50wt% HF, 20mL of 37wt% HCl and 10mL of deionized water), stirring for 12h at 35 ℃, repeatedly centrifuging, and cleaning until the pH value is neutral; the precipitate was collected and added to 40mL of an aqueous LiCl (2 g) solution, stirred at room temperature for 12h, centrifuged to collect the supernatant, and filtered with suction and dried at room temperature for 12h.
And 2, uniformly mixing 0.5g of polycarbosilane, 0.9-1.1 g of polyvinylpyrrolidone, 4-6 mL of absolute ethyl alcohol and 6mL of tetrahydrofuran to obtain a polycarbosilane solution, wherein the average molecular weight of the polycarbosilane is 1000-2000, the softening point temperature is 180-200 ℃, and the residual weight rate of the polycarbosilane at 1000 ℃ under the protection of N 2 is more than 57%. And (3) adding the two-dimensional Ti 3C2Tx nano-sheets obtained in the step (1) into the polycarbosilane solution, performing ultrasonic treatment for 15min, and then stirring at room temperature for 6-10 h to obtain the electrostatic spinning solution.
And 3, filling the electrostatic spinning solution obtained in the step 2 into a 10mL syringe for electrostatic spinning, selecting a stainless steel needle with the 20G number, setting the electrostatic spinning voltage to be 16-20 kV, the receiving distance to be 18-22 cm, the spinning temperature to be 20-30 ℃, the environmental humidity to be 10-30%, and the propulsion speed to be 0.0010mm/s, so as to obtain the nanofiber precursor.
Step 4, heating the nanofiber precursor obtained in the step 3 to 180-200 ℃ for thermal oxidation crosslinking, and keeping the temperature for 2 hours, wherein the atmosphere is air; transferring the mixture into a vacuum furnace after the reaction is finished, slowly heating the mixture to 1300-1500 ℃ to perform polymer conversion, heating the mixture at a speed of 3-5 ℃/min, maintaining the temperature for 2h, wherein the atmosphere is required to be argon or vacuum, and naturally cooling the mixture to room temperature to obtain the high-temperature-resistant wave-absorbing silicon carbide nanofiber.
Example 1
Slowly adding 2g of Ti 3AlC2 powder into 50mL of etchant (the composition ratio of the etchant is 20mL of 50wt% HF, 20mL of 37wt% HCl and 10mL of deionized water), stirring for 12h at 35 ℃, repeatedly centrifuging, and cleaning until the pH value is neutral; the precipitate was collected and added to 40mL of an aqueous LiCl (2 g) solution, stirred at room temperature for 12h, centrifuged to collect the supernatant, and filtered with suction and dried at room temperature for 12h.
0.5G of polycarbosilane (average molecular weight 1000, softening point temperature of 180-200 ℃ and residual weight ratio of 1000 ℃ under the protection of N 2 of more than 57%), 0.9g of polyvinylpyrrolidone, 4mL of absolute ethyl alcohol and 6mL of tetrahydrofuran are uniformly mixed and stirred for 0.5h, then 0.0736g of two-dimensional Ti 3C2Tx nano-sheet (total mass of 5%) is added, and uniformly stirred for 6h at room temperature, thus obtaining an electrostatic spinning solution.
Transferring the obtained electrostatic spinning solution into a 10mL injector for electrostatic spinning, selecting a stainless steel needle with the size of 20G, setting the electrostatic spinning voltage to be 16kV, and obtaining the nanofiber precursor, wherein the receiving distance is 18cm, the spinning temperature is 20 ℃, the ambient humidity is 10%, and the advancing speed is 0.0010 mm/s.
Heating the obtained nanofiber precursor to 180 ℃, preserving heat in air for 2 hours, transferring into a vacuum furnace after the reaction is finished, slowly heating to 1400 ℃ at the speed of 3 ℃/min, preserving heat in argon for 2 hours, and naturally cooling to room temperature to obtain the high-temperature-resistant wave-absorbing silicon carbide nanofiber.
FIG. 1 is a scanning electron microscope image of a high temperature resistant wave-absorbing silicon carbide nanofiber prepared in example 1 of the present invention, and it can be observed that the fiber is smooth and flat without obvious defects. FIG. 2 is a graph showing the frequency-dependent dielectric constants of the high temperature resistant wave-absorbing silicon carbide nanofibers prepared in example 1 of the present invention, wherein the real part is between 11.6 and 8.8 and the imaginary part is between 2.8 and 2.9 in the frequency range of 2 to 18 GHz. FIG. 3 is a graph showing the minimum reflection loss of the high-temperature-resistant wave-absorbing silicon carbide nanofiber prepared in the embodiment 1 of the invention under different thicknesses, wherein the minimum reflection loss can reach-48.58 dB, the corresponding radar wave frequency is 10.16GHz, the thickness is 2.5mm, and the effective absorption bandwidth can reach 3.12GHz. The highest service temperature of the high-temperature-resistant wave-absorbing silicon carbide nanofiber prepared in the embodiment 1 of the invention is 1400 ℃ limited by the conversion temperature of the polymer, and the high-temperature-resistant wave-absorbing silicon carbide nanofiber has the best high-temperature resistance in the radar wave-absorbing silicon carbide nanofiber reported at present.
Example 2
Slowly adding 2g of Ti 3AlC2 powder into 50mL of etchant (the composition ratio of the etchant is 20mL of 50wt% HF, 20mL of 37wt% HCl and 10mL of deionized water), stirring for 12h at 35 ℃, repeatedly centrifuging, and cleaning until the pH value is neutral; the precipitate was collected and added to 40mL of an aqueous LiCl (2 g) solution, stirred at room temperature for 12h, centrifuged to collect the supernatant, and filtered with suction and dried at room temperature for 12h.
0.5G of polycarbosilane (average molecular weight 1500, softening point temperature of 180-200 ℃ and residual weight ratio of 1000 ℃ under the protection of N 2 of more than 57%), 1.0g of polyvinylpyrrolidone, 5mL of absolute ethyl alcohol and 6mL of tetrahydrofuran are uniformly mixed and stirred for 0.5h, then 0.1054g of two-dimensional Ti 3C2Tx nano-sheet (total mass of 7%) is added, and uniformly stirred for 8h at room temperature, thus obtaining an electrostatic spinning solution.
Transferring the obtained electrostatic spinning solution into a 10mL injector for electrostatic spinning, selecting a stainless steel needle with the size of 20G, setting the electrostatic spinning voltage to 18kV, and obtaining the nanofiber precursor, wherein the receiving distance is 20cm, the spinning temperature is 25 ℃, the ambient humidity is 20%, and the advancing speed is 0.0010 mm/s.
Heating the obtained nanofiber precursor to 190 ℃, preserving heat in air for 2 hours, transferring into a vacuum furnace after the reaction is finished, slowly heating to 1300 ℃ at the speed of 4 ℃/min, preserving heat in vacuum for 2 hours, and then naturally cooling to room temperature to obtain the high-temperature-resistant wave-absorbing silicon carbide nanofiber.
Example 3
Slowly adding 2g of Ti 3AlC2 powder into 50mL of etchant (the composition ratio of the etchant is 20mL of 50wt% HF, 20mL of 37wt% HCl and 10mL of deionized water), stirring for 12h at 35 ℃, repeatedly centrifuging, and cleaning until the pH value is neutral; the precipitate was collected and added to 40mL of an aqueous LiCl (2 g) solution, stirred at room temperature for 12h, centrifuged to collect the supernatant, and filtered with suction and dried at room temperature for 12h.
0.5G of polycarbosilane (average molecular weight 2000, softening point temperature of 180-200 ℃ and residual weight ratio of 1000 ℃ under the protection of N 2 of more than 57%), 1.1g of polyvinylpyrrolidone, 6mL of absolute ethyl alcohol and 6mL of tetrahydrofuran are uniformly mixed and stirred for 0.5h, then 0.1385g of two-dimensional Ti 3C2Tx nano-sheet (total mass of 9%) is added, and uniformly stirred for 10h at room temperature, thus obtaining an electrostatic spinning solution.
Transferring the obtained electrostatic spinning solution into a 10mL injector for electrostatic spinning, selecting a stainless steel needle with the size of 20G, setting the electrostatic spinning voltage to be 20kV, and obtaining the nanofiber precursor, wherein the receiving distance is 22cm, the spinning temperature is 30 ℃, the ambient humidity is 30%, and the advancing speed is 0.0010 mm/s.
Heating the obtained nanofiber precursor to 200 ℃, preserving heat in air for 2 hours, transferring into a vacuum furnace after the reaction is finished, slowly heating to 1500 ℃ at a speed of 5 ℃/min, preserving heat in argon for 2 hours, and naturally cooling to room temperature to obtain the high-temperature-resistant wave-absorbing silicon carbide nanofiber.
The above examples merely illustrate specific embodiments of the invention, which are described in more detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (7)
1. The preparation method of the high-temperature-resistant wave-absorbing silicon carbide nanofiber is characterized by comprising the following steps of:
Step 1, ti 3AlC2 powder is selected as a raw material, a mixed aqueous solution of HF, HCl and deionized water is used as an etchant, a LiCl aqueous solution is used as an intercalating agent, and a two-dimensional Ti 3C2Tx nano-sheet is prepared by a chemical etching method;
Step 2, preparing a polycarbosilane solution, adding the two-dimensional Ti 3C2Tx nano-sheets obtained in the step 1 into the polycarbosilane solution, and then performing strong ultrasonic and stirring treatment to obtain a uniformly dispersed electrostatic spinning solution;
step 3, transferring the electrostatic spinning solution obtained in the step 2 into an injector for electrostatic spinning, and obtaining a nanofiber precursor by controlling electrostatic spinning voltage, receiving distance, spinning temperature, environmental humidity and spinning advancing speed;
And 4, transferring the nanofiber precursor obtained in the step 3 to a drying oven for thermal oxidation crosslinking, and then transferring to a vacuum furnace for polymer conversion to obtain the high-temperature-resistant wave-absorbing silicon carbide nanofiber.
2. The method for preparing the high-temperature-resistant wave-absorbing silicon carbide nanofiber according to claim 1, wherein the specific method of step 1 is as follows: slowly adding 2g of Ti 3AlC2 powder into 50mL of etching agent, stirring at 35 ℃ for 12h, repeatedly centrifuging, and cleaning until the pH value is neutral; collecting precipitate, adding into 40mL of intercalating agent, stirring at room temperature for 12h, cleaning, centrifuging, collecting supernatant, suction filtering, and drying at room temperature for 12h; wherein, the composition ratio of the etchant is 20mL 50wt% HF, 20mL 37wt% HCl and 10mL deionized water, and the intercalating agent is 40mL 2g LiCl aqueous solution.
3. The method for preparing the high-temperature-resistant wave-absorbing silicon carbide nanofiber according to claim 1, wherein the polycarbosilane solution in the step 2 consists of 0.5g of polycarbosilane, 0.9-1.1 g of polyvinylpyrrolidone, 4-6 mL of absolute ethyl alcohol and 6mL of tetrahydrofuran.
4. The method for preparing the high-temperature-resistant wave-absorbing silicon carbide nanofiber according to claim 3, wherein the average molecular weight of polycarbosilane in the step 2 is 1000-2000, the softening point temperature is 180-200 ℃, and the residual weight rate of the polycarbosilane at 1000 ℃ under the protection of N 2 is more than 57%.
5. The method for preparing the high-temperature-resistant wave-absorbing silicon carbide nanofiber according to claim 1, wherein the electrostatic spinning process parameters in the step 3 are as follows: the spinning voltage is 16-20 kV, the receiving distance is 18-22 cm, the spinning temperature is 20-30 ℃, the ambient humidity is 10-30%, and the advancing speed of the spinning solution is 0.0010mm/s.
6. The method for preparing the high-temperature-resistant wave-absorbing silicon carbide nanofiber according to claim 1, wherein the specific practice of the step 4 is as follows: transferring the nanofiber precursor obtained in the step 3 to a drying oven for thermal oxidation crosslinking, wherein the thermal oxidation crosslinking temperature is 180-200 ℃, the heat preservation time is 2h, the atmosphere requirement is air, then transferring the nanofiber precursor into a vacuum furnace for polymer conversion, the polymer conversion temperature is 1300-1500 ℃, the heating rate is 3-5 ℃/min, the heat preservation time is 2h, and the atmosphere requirement is argon or vacuum.
7. The high temperature resistant wave-absorbing silicon carbide nanofiber prepared by the method for preparing the high temperature resistant wave-absorbing silicon carbide nanofiber according to any one of claims 1 to 6.
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