CN116084161A - Biomass-based silicon carbide composite fiber, preparation method thereof and electromagnetic absorption material - Google Patents
Biomass-based silicon carbide composite fiber, preparation method thereof and electromagnetic absorption material Download PDFInfo
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
Abstract
The invention relates to the technical field of preparation of carbon fiber materials and composite materials thereof, in particular to a biomass-based silicon carbide composite fiber, a preparation method thereof and an electromagnetic absorption material. The invention provides a biomass-based silicon carbide composite fiber, which comprises a hollow carbon fiber and silicon carbide compounded on the hollow carbon fiber; the hollow carbon fiber is carbide of tree cotton fiber. According to the composite fiber provided by the invention, the hollow carbon fiber obtained by carbonizing the tree cotton fiber with high hollowness and large specific surface area with hollow morphology is used as a carbon source to carry out carbothermic reduction reaction, and the silicon carbide phase is introduced to realize the carbon/silicon carbide composite fiber. The silicon carbide component can shuttle inside the hollow carbon tube under the action of the catalyst, so that the interface of the composite material is increased, the dielectric constant of the composite material is regulated, and the optimization of electromagnetic absorption performance can be realized; the electrochemical application can be realized, the economic added value of the tree cotton fiber is improved, and the multifunctional application is shown.
Description
Technical Field
The invention relates to the technical field of preparation of carbon fiber materials and composite materials thereof, in particular to a biomass-based silicon carbide composite fiber, a preparation method thereof and an electromagnetic absorption material.
Background
The carbon fiber is used as a novel multifunctional fiber material, has excellent mechanical and electrical properties and other excellent properties, and has a huge application prospect in the fields of high-performance composite materials and novel functional materials. The carbon fiber material is a typical conductive loss material and has wide application in the field of electromagnetic wave absorption, and in order to improve the wave absorption performance, the carbon/silicon carbide composite material is a potential composite wave absorption material and has the advantages of good chemical stability and the like, the SiC component is introduced into the composite fiber, the interface between SiC and C is increased, the interface polarization loss capacity is enhanced, and the wave absorption performance of the composite material is obviously improved. However, the electromagnetic wave reflection is caused by the fact that the conductivity of the carbon fiber raw material is high, so that the impedance mismatch phenomenon is easy to generate, and the electromagnetic absorption performance is affected.
Disclosure of Invention
In view of the above, the technical problem to be solved by the invention is to provide a biomass-based silicon carbide composite fiber, a preparation method thereof and an electromagnetic absorption material.
The invention provides a biomass-based silicon carbide composite fiber, which comprises a hollow carbon fiber and silicon carbide compounded on the hollow carbon fiber; the hollow carbon fiber is carbide of tree cotton fiber.
The composite fiber of the present invention comprises a hollow carbon fiber. Specifically, the hollow carbon fiber is carbide of tree cotton fiber; the hollowness of the hollow carbon fiber is 85% -90%; the fiber diameter of the hollow carbon fiber is 10-15 mu m; the thickness of the carbon wall of the hollow carbon fiber is 500 nm-1000 nm.
The tree cotton is crown wool fiber produced by accidentally finding fruits of wild plant shrub fiber species Calotropis gigantea at the edge of the original forest in Yunnan, and is a second plant fiber produced once after only one plant fiber of cotton is used for thousands of years worldwide. The tree cotton has the self excellent characteristics far exceeding that of cotton, and has high hollowness; the specific gravity is one fourth of that of cotton fiber, and can float and float in the air. The tree cotton fiber is used as a biomass template to be subjected to subsequent carbonization treatment to obtain the hollow carbon tube fiber, and in the carbonization process, the tree cotton fiber comprises cellulose, hemicellulose, lignin, wax and a small amount of ash, and the components are decomposed to generate a simple substance carbon material in the high-temperature carbonization treatment process. In certain embodiments of the invention, the hollowness of the cotton fiber is 85% -90%; the fiber length of the tree cotton fiber is 31 mm-35 mm; the fineness of the cotton fiber, namely the fiber diameter or the cross-sectional area, is 16-28 mu m.
The composite fiber also comprises silicon carbide compounded on the hollow carbon fiber. The silicon carbide is compounded in the hollow carbon fiber and the pipe wall of the hollow carbon fiber. In certain embodiments of the present invention, the composite fiber further comprises silicon carbide nanowires dispersed inside the hollow carbon fiber and silicon carbide particles in situ compounded on the tube wall of the hollow carbon fiber.
According to the biomass-based silicon carbide composite fiber provided by the invention, the carbide of the tree cotton fiber is used as the hollow carbon fiber, and the hollow light characteristic of the tree cotton fiber is utilized to compound silicon carbide on the hollow carbon fiber; the SiC component is introduced into the composite fiber, so that the interface between SiC and C is increased, the interface polarization loss capacity is enhanced, the wave absorbing performance of the composite material is obviously improved, the dielectric loss performance of the system is also enhanced due to the defect and the porous structure of the hollow light multi-wall carbon nano tube prepared by taking the hollow biomass fiber as a template, the regulation and control of the dielectric performance of the composite material can be realized by adjusting the content of the introduced silicon carbide component, and the wave absorbing performance of the composite material is further improved.
The invention also provides a preparation method of the biomass-based silicon carbide composite fiber, which comprises the following steps: carrying out solid phase reaction on the hollow carbon fiber and a silicon source to obtain a biomass-based silicon carbide composite fiber; the hollow carbon fiber is carbide of tree cotton fiber.
The hollow carbon fiber is carbide of tree cotton fiber. The invention selects the biomass fiber tree cotton fiber with unique hollow morphology as the raw material, has high hollow degree and hollow light characteristic, and can be used as a template to carry out carbonization treatment under the protection of inert gas so as to realize the preparation of the hollow carbon fiber. Specifically, the invention carries out carbonization treatment on the cotton fiber under the protection of inert gas to obtain the carbide of the cotton fiber, namely the hollow carbon fiber. In certain embodiments of the invention, the hollowness of the cotton fiber is 85% -90%; the fiber length of the tree cotton fiber is 31 mm-35 mm; the fiber diameter of the tree cotton fiber is 16-28 mu m. In certain embodiments of the invention, the inert gas is nitrogen, and the purity of the nitrogen is 99.99% or more. In certain embodiments of the invention, the carbonization treatment is performed at a temperature of 600 ℃ to 800 ℃ for a time of 1h to 6h; the heating rate of the carbonization treatment is 1-5 ℃ per minute, preferably 1 ℃ per minute. In one embodiment, the temperature of the carbonization treatment is 800 ℃, the time of the carbonization treatment is 2 hours, and the temperature rising rate of the carbonization treatment is 2 ℃/min.
After the hollow carbon fiber is prepared, carbon thermal reduction reaction is carried out by taking the hollow carbon fiber as a carbon source, and a silicon carbide phase is introduced, so that the preparation of the carbon/silicon carbide composite fiber can be realized. The hollow carbon fiber and a silicon source are subjected to solid phase reaction to obtain the biomass-based silicon carbide composite fiber. In some embodiments of the present invention, the hollow carbon fiber is mixed with a silicon source and then sintered at a high temperature under an inert protective gas atmosphere to perform a solid phase reaction, so as to obtain a biomass-based silicon carbide composite fiber; and naturally cooling to room temperature to obtain the hollow carbon/silicon carbide composite fiber. In some embodiments of the present invention, the hollow carbon fiber prepared as described above has a hollowness of 85% to 90%; the fiber diameter of the hollow carbon fiber is 10-15 mu m; the thickness of the carbon wall of the hollow carbon fiber is 500 nm-1000 nm. In certain embodiments of the invention, the mass ratio of the hollow carbon fiber to the silicon source is 4 to 10:1, preferably 6:1. in certain embodiments of the present invention, the silicon source is selected from at least one of silicon dioxide, silicon powder, sodium silicate, methyl orthosilicate (TMOS), and ethyl orthosilicate (TEOS). In one embodiment, the silicon source is selected from the group consisting of a molar ratio of 1:1, silica and silica fume.
In some embodiments, the temperature of the solid phase reaction is 1000 ℃ to 1300 ℃, preferably 1100 ℃; the time of the solid phase reaction is 30 min-180 min, preferably 2h; the heating rate of the solid phase reaction is 1-3 ℃/min, preferably 2.5 ℃/min. In some embodiments, the inert shielding gas is selected from at least one of helium or argon, and the flow rate of the inert shielding gas is 10mL/min to 20mL/min. In one embodiment, the inert shielding gas is argon and the flow rate of the inert shielding gas is 10mL/min.
The invention further comprises the step of carrying out catalytic treatment on the hollow carbon fiber before carrying out solid phase reaction on the hollow carbon fiber and a silicon source. Specifically, the hollow carbon fiber is immersed in a catalyst solution for catalytic treatment; the catalytic treatment can facilitate subsequent silicon carbide formation. In certain embodiments of the invention, the temperature of the catalytic treatment is from 30 ℃ to 80 ℃; the time of the catalytic treatment is 0.5 h-10 h. In certain embodiments of the present invention, the catalytic treatment is carried out on disodium edetate, sodium chloride, sodium fluoride, feCl 3 ·6H 2 In one or more solutions of O and Co (NO 3) 2. In one embodiment, the catalytic treatment is carried out on disodium ethylenediamine tetraacetate at a concentration of 0.02mol/L and FeCl at a concentration of 0.2mol/L 3 ·6H 2 And O in a mixed solution.
The present invention further comprises pretreating the hollow carbon fiber before the catalytic treatment of the hollow carbon fiber with the silicon source. According to the preparation method, the hollow carbon fiber is subjected to pretreatment, the roughness and the functional groups of the surface of the carbon fiber are increased, and the subsequent loading of the catalyst and the reaction of generating silicon carbide with a silicon source can be facilitated. In certain embodiments of the invention, the temperature of the pretreatment is from 30 ℃ to 65 ℃; the pretreatment time is 0.5-2 h. In certain embodiments of the invention, the pretreatment is performed in one or more of hydrofluoric acid, dilute hydrochloric acid, dilute sulfuric acid, hypochlorous acid, hydrogen peroxide, and aqueous ammonia. In some embodiments, the hollow carbon fiber is immersed in one or more of hydrofluoric acid, dilute hydrochloric acid, dilute sulfuric acid, hypochlorous acid, hydrogen peroxide and ammonia water to perform pretreatment. In one embodiment, the present invention impregnates the hollow carbon fibers described above in 40wt% hydrofluoric acid for 4 hours.
The invention also provides an electromagnetic absorption material, which comprises a fiber material and an insulating material; the fiber material is the composite fiber or the composite fiber prepared by the method.
The invention provides a biomass-based silicon carbide composite fiber, which comprises a hollow carbon fiber and silicon carbide compounded on the hollow carbon fiber; the hollow carbon fiber is carbide of tree cotton fiber. According to the biomass-based silicon carbide composite fiber provided by the invention, the biomass fiber tree cotton fiber with unique hollow morphology and high hollowness and large specific surface area is selected as a raw material, and the hollow carbon fiber obtained after carbonization treatment is used as a carbon source to perform carbothermic reduction reaction and introduce silicon carbide phase to prepare the carbon/silicon carbide composite fiber, namely the biomass-based silicon carbide composite fiber. The silicon carbide component can shuttle in the hollow carbon tube under the action of the catalyst, the interface of the composite material is increased, the dielectric constant of the composite material is regulated, the optimization of electromagnetic absorption performance can be realized, the application in the electrochemical direction can be realized, the economic additional value of the tree cotton biomass fiber is improved, and meanwhile, the multifunctional application is shown.
Drawings
FIG. 1 is an XRD pattern of the hollow carbon fiber material obtained in example 1;
FIG. 2 is an SEM image of a hollow carbon fiber material obtained in example 1;
FIG. 3 is an SEM image of a hollow carbon/silicon carbide composite fiber obtained in example 1;
FIG. 4 is a graph showing the dielectric constant of the hollow carbon fiber material obtained in example 1;
FIG. 5 is a graph showing the magnetic permeability of the hollow carbon fiber material obtained in example 1;
FIG. 6 is a graph showing the dielectric constant of the hollow carbon/silicon carbide composite fiber obtained in example 1;
fig. 7 is a graph showing the magnetic permeability of the hollow carbon/silicon carbide composite fiber obtained in example 1.
Detailed Description
The invention discloses a biomass-based silicon carbide composite fiber, a preparation method thereof and an electromagnetic absorption material. Those skilled in the art can, with the benefit of this disclosure, suitably modify the process parameters to achieve this. It is expressly noted that all such similar substitutions and modifications will be apparent to those skilled in the art, and are deemed to be included in the present invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those skilled in the relevant art that the invention can be practiced and practiced with modification and alteration and combination of the methods and applications herein without departing from the spirit and scope of the invention.
The invention is further illustrated by the following examples:
example 1
The biomass-based FeS particle composite fiber disclosed by the invention is prepared by the following steps:
step 1: preparing hollow carbon tube fibers, selecting biomass fiber material tree cotton fibers as raw materials, and carbonizing to obtain hollow carbon fiber materials; the carbonization treatment is to heat up to 800 ℃ under the protection of inert gas nitrogen with the gas purity of more than or equal to 99.99 percent for high-temperature treatment, and keep the slow heating rate of 2 ℃/min and keep the temperature for 2 hours.
Step 2: pretreatment of carbon fibers, namely pretreating the hollow carbon material obtained in the step 1, and increasing the roughness and functional groups on the surface of the carbon fibers, so that the subsequent loading of a catalyst and the reaction of generating silicon carbide with a silicon source are facilitated; the pretreatment is that deionized water is used for washing for many times after 40wt% hydrofluoric acid is adopted for soaking treatment for 4 hours.
Step 3: impregnating catalyst, and impregnating pretreated carbon fiber material in catalyst solutionIn order to generate 40 ℃ for 2 hours, specifically: the catalyst solution is EDTA disodium ethylenediamine tetraacetate with the concentration of 0.02mol/L and FeCl with the concentration of 0.2mol/L 3 ·6H 2 Mixed solution of O.
Step 4: carrying out solid-phase reaction on the carbon fiber obtained in the step 3 and a silicon source to generate silicon carbide, namely obtaining the hollow carbon/silicon carbide composite fiber; the silicon source is a silicon source with a mole ratio of 1:1 and silicon powder. The specific operation is as follows: and (3) mechanically and uniformly mixing the carbon fiber obtained in the step (3) with the silicon source according to the mass ratio of 6:1, placing the mixture into a crucible, placing the crucible into a sintering furnace, taking argon with the gas flow rate of 10mL/min as inert shielding gas, heating to 1100 ℃ at the heating rate of 2.5 ℃/min, carrying out high-temperature sintering reaction for 2 hours, and naturally cooling to room temperature after the reaction is completed, thus obtaining the hollow carbon/silicon carbide composite fiber.
XRD detection and SEM detection are carried out on the hollow carbon fiber material obtained in the step 1 of the embodiment, and SEM detection is carried out on the hollow carbon/silicon carbide composite fiber obtained in the step 4, and the detection results are shown in figures 1-3. FIG. 1 is an XRD pattern of the hollow carbon fiber material obtained in example 1, and it is understood from FIG. 1 that the carbonized cotton fiber protected by an inert gas at 800℃is completely converted into amorphous elemental carbon. FIG. 2 is an SEM image of the hollow carbon fiber material obtained in example 1, and as can be seen from FIG. 2, the carbon fiber morphology prepared after carbonization is a hollow morphology of the carbon fiber replication tree cotton; the surface of the fiber is shrunk to generate folds, the fiber diameter is 10-15 mu m, and the carbon wall thickness is about 500-1000 nm. Fig. 3 is an SEM image of the hollow carbon/silicon carbide composite fiber obtained in example 1, and as can be seen from fig. 3, the silicon carbide component is successfully introduced after the solid phase carbothermic reduction reaction of the silicon source, and the silicon carbide is two typical morphologies, namely SiC generated in situ by the carbon wall and nanowires dispersed inside the hollow carbon tube.
The hollow carbon fiber material obtained in step 1 was subjected to electromagnetic parameter and wave-absorbing performance tests, and the results are shown in fig. 4 to 5, wherein fig. 4 is a graph of dielectric constant of the hollow carbon fiber material obtained in example 1, and fig. 5 is a graph of magnetic permeability of the hollow carbon fiber material obtained in example 1. As can be seen from fig. 4 to 5, the real part and the imaginary part of the magnetic permeability of the hollow carbon fiber material obtained in step 1 of example 1 are concentrated near 1 and 0, respectively, and belong to the magnetic permeability data characteristics of the composite dielectric loss type wave-absorbing material; the dielectric constant of the composite material is high in deficiency, and the dielectric constant of the composite material is higher than that of the real component, so that mismatch of impedance matching can be caused, and the wave absorbing performance of the composite material is seriously affected.
The hollow carbon/silicon carbide composite fiber obtained in the step 4 was subjected to electromagnetic parameter and wave absorption performance tests, and the results are shown in fig. 6 to 7, wherein fig. 6 is a graph of dielectric constant of the hollow carbon/silicon carbide composite fiber obtained in the example 1, and fig. 7 is a graph of magnetic permeability of the hollow carbon/silicon carbide composite fiber obtained in the example 1. As can be seen from fig. 6 to 7, the hollow carbon/silicon carbide composite fiber obtained in step 4 of example 1 has a significantly reduced dielectric constant compared to the hollow carbon fiber material obtained in step 1; and the real part of the dielectric constant is larger than the imaginary part, which proves that the introduction of the silicon carbide component has positive effect on the adjustment of dielectric properties. The subsequent adjustment process can realize excellent wave absorbing performance.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (10)
1. The biomass-based silicon carbide composite fiber is characterized by comprising hollow carbon fibers and silicon carbide compounded on the hollow carbon fibers;
the hollow carbon fiber is carbide of tree cotton fiber.
2. The composite fiber according to claim 1, wherein the hollow carbon fiber has a hollowness of 85 to 90%;
the fiber diameter of the hollow carbon fiber is 10-15 mu m;
the thickness of the carbon wall of the hollow carbon fiber is 500 nm-1000 nm.
3. The preparation method of the biomass-based silicon carbide composite fiber is characterized by comprising the following steps of:
carrying out solid phase reaction on the hollow carbon fiber and a silicon source to obtain a biomass-based silicon carbide composite fiber;
the hollow carbon fiber is carbide of tree cotton fiber.
4. A method according to claim 3, wherein the hollowness of the cotton fiber is 85-90%;
the fiber diameter of the tree cotton fiber is 16-28 mu m.
5. A method according to claim 3, wherein the silicon source is selected from at least one of silicon dioxide, silicon powder, sodium silicate, methyl orthosilicate and ethyl orthosilicate.
6. A method according to claim 3, wherein the mass ratio of the hollow carbon fiber to the silicon source is 4 to 10:1.
7. a method according to claim 3, wherein the temperature of the solid phase reaction is 1000 ℃ to 1300 ℃; the time of the solid phase reaction is 30-180 min.
8. A method according to claim 3, wherein the hollow carbon fiber further comprises subjecting it to a catalytic treatment prior to the solid phase reaction;
the temperature of the catalytic treatment is 30-80 ℃; the time of the catalytic treatment is 0.5 h-10 h.
9. The method according to claim 8, wherein the catalytic treatment is carried out on disodium ethylenediamine tetraacetate, sodium chloride, sodium fluoride, feCl 3 ·6H 2 In one or more solutions of O and Co (NO 3) 2.
10. An electromagnetic absorbing material, comprising a fibrous material and an insulating material; the fiber material is the composite fiber of any one of claims 1-2 or the composite fiber prepared by the method of any one of claims 3-9.
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