CN112607740A - Preparation method of silicon carbide nanofiber aerogel - Google Patents
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Abstract
The invention discloses a preparation method of silicon carbide nanofiber aerogel. The method comprises the following steps: 1) coating SiO on the surface of carbon fiber by a sol-gel method2Gelling; 2) coating the surface with SiO2Dispersing the gelled carbon fiber aggregate to obtain a fluffy carbon fiber felt; 3) preparation of SiO by sol-gel method2C gel powder; 4) mixing SiO2Laying the gel powder at the bottom of the crucible, and putting the fluffy carbon fiber felt prepared in the step 2) to SiO2Covering a crucible cover above the gel powder; 5) and (3) placing the crucible in the step 4) into a high-temperature atmosphere furnace, and preparing the silicon carbide nanofiber aerogel under the high-temperature condition. The aerogel prepared by the invention is formed by interweaving the silicon carbide nano-fiber in three-dimensional space, the pore structure is controllable, the preparation process is simple, the reaction is sufficient, the subsequent calcination treatment is not needed,the macroscopic morphology of the product is controllable, and the large-size and large-scale production and preparation of the aerogel are easy to realize.
Description
Technical Field
The invention relates to a preparation method of aerogel, in particular to a preparation method of silicon carbide nanofiber aerogel.
Background
The aerogel is a nano-scale porous material, has excellent properties such as low thermal conductivity, low density, high porosity and super-large specific surface area, and has wide application prospects in the fields of aerospace, fire prevention, heat insulation, biomedicine, filtration, catalytic adsorption and the like.
Most studied at present is SiO2Aerogel, Al2O3Aerogel and carbon aerogel, the preparation process of traditional aerogel can be divided into two steps on the whole: sol-gel process and drying process. The sol-gel process generally refers to a process in which a precursor forms a sol after undergoing hydrolysis and polycondensation reactions under the action of a catalyst, and then forms a gel after aging. In the process of drying the gel, the key technology is to maintain the integrity of the gel structure as much as possible and avoid the damage of the network structure of the gel by the capillary tension generated on the surface of the gas and the liquid. Generally, the drying process of the aerogel is mainly divided into three types, namely supercritical drying, freeze drying and atmospheric drying.
The silicon carbide aerogel has excellent high temperature resistance and oxidation resistance, and is concerned by more and more researchers. The silicon carbide aerogel preparation technology in the prior art has the following problems that (1) the silicon carbide aerogel is prepared by a ceramic preparation method through conversion of a polycarbosilane polymer precursor, the raw material cost is high, and the whole structure of the aerogel is easy to collapse due to loose skeleton structure and low mechanical property of the aerogel material; (2) the freeze drying preparation technology of the silicon carbide aerogel material, particularly the supercritical drying technology, causes high preparation cost and long preparation period; (3) harsh drying technical conditions put great demands on the temperature or pressure performance of equipment, so that the reaction process can be performed in a smaller cavity, and the preparation of large-size aerogel is difficult to realize. These problems severely limit the practical industrial application of aerogel materials.
Disclosure of Invention
In order to solve the problems in the background art, the invention provides a preparation method of silicon carbide nanofiber aerogel. The main reaction mechanism is as follows: under the condition of high temperature, the sol-gel powder containing expandable graphite generates gases such as SiO, Si, CO and the like, and reacts with carbon fibers to generate silicon carbide crystal nuclei. The silicon carbide crystal nucleus grows mainly according to two steps: after silicon source gases such as SiO, Si and the like are contacted with carbon fibers, gas-solid reaction is carried out on the surfaces and the interfaces of the fibers to form SiC crystal nuclei; and (3) performing gas phase reaction on carbon source gases such as CO and the like and silicon source gases such as SiO and Si after contacting the surface of the carbon fiber, and enabling SiC crystal nuclei to grow in one dimension along a specific lattice direction according to the preferred orientation of a crystal face to form the silicon carbide nanofiber. In addition, the invention coats SiO2The carbon fiber aggregate is separated into single fiber state after passing through huge drawing force between a licker-in of the cotton fluffer and a roller, and forms fluffy carbon fiber felt through a cotton conveying channel under the action of air flow, thereby providing a favorable space for the growth of silicon carbide nano fibers in a subsequent high-temperature atmosphere furnace; the carbon fibers fully react, subsequent calcination for carbon removal is not needed, and oxidation of the silicon carbide nanofibers in the calcination process is avoided; carbon fiber surface coated with SiO2Is beneficial to the growth of SiC crystal nucleus. The method has the advantages of simple process, low requirement on equipment, low preparation cost, high production efficiency and easy realization of large-scale industrial production.
The invention adopts the following technical scheme that the method comprises the following steps:
1) SiO on carbon fiber surface2Coating: coating SiO on the surface of carbon fiber by a sol-gel method2Gelling;
2) preparing a fluffy carbon fiber felt: coating the surface with SiO2Dispersing the gelled carbon fiber aggregate to obtain a fluffy carbon fiber felt;
3)SiO2preparation of gel powder raw material: preparation of SiO by sol-gel method2C gel powder;
4) filling raw materials: mixing SiO2Laying the gel powder at the bottom of the crucible, and putting the fluffy carbon fiber felt prepared in the step 2) into SiO in a set shape2Covering a crucible cover above the gel powder;
5) preparing silicon carbide nanofiber aerogel by carbothermal reduction: placing the crucible in the step 4) in a high-temperature atmosphere furnace, and preparing the silicon carbide nanofiber aerogel under the high-temperature condition;
the step 1) is specifically as follows: hydrolyzing ethyl orthosilicate (TEOS), water and absolute ethyl alcohol as raw materials until the solution is clear to obtain silica sol, dipping the silica sol into the degummed short-cut carbon fibers, draining and drying to obtain the surface-coated SiO2The carbon fiber aggregate of (1).
The length of the short carbon fiber is 3-80 mm, the carbon fibers with different lengths influence the density of the fluffy carbon fiber felt, and further influence the density of the silicon carbide nano-fiber aerogel obtained through preparation.
In the step 2), the surface is coated with SiO by using a dispersing mode such as a cotton fluffer or airflow impact2The carbon fiber aggregates of the gel are dispersed.
The carbon fiber aggregate is separated into single fibers by huge drawing force between the licker-in of the cotton fluffer and the roller, and the fluffy carbon fiber felt is formed through a cotton conveying channel under the action of air flow.
In the step 2), the density degree of the silicon carbide nanofiber aerogel is regulated and controlled by changing the density degree of the fluffy carbon fiber felt.
The macroscopic morphology of the fluffy carbon fiber felt determines the macroscopic morphology of the silicon carbide nanofiber aerogel, and the macroscopic morphology of the silicon carbide nanofiber aerogel is directly or indirectly regulated and controlled in a mode of changing the appearance of the fluffy carbon fiber felt and the size and shape of the crucible.
The step 3) is specifically that tetraethoxysilane, water and absolute ethyl alcohol are hydrolyzed to be used as raw materials, the hydrolysis is carried out until the solution is clear, silica sol is obtained, expandable graphite is added into the silica sol, the mixture is continuously stirred to gel, and the gel is dried and crushed to obtain SiO2C gel powder.
The mass of the expandable graphite is 2-20% of that of ethyl orthosilicate.
The silica sol comprises the following raw materials in percentage by mass: 50-70% of ethyl orthosilicate, 10-20% of water and 10-40% of absolute ethyl alcohol.
The SiO2The mass of the/C gel powder is 150 to600g, and adjusting SiO according to the using amount of the fluffy carbon fiber felt and the size of a high-temperature atmosphere furnace hearth2The mass of the gel powder/C.
The step 5) is specifically as follows: circularly vacuumizing the high-temperature atmosphere furnace and filling nitrogen for three times to reduce the oxygen partial pressure; heating the high-temperature atmosphere furnace to 1450-1700 ℃ at a heating rate of 1-10 ℃/min, and carrying out heat preservation sintering for 3-6 h, wherein the reaction pressure is positive pressure; and after the reaction is finished, cooling to normal temperature along with the furnace to obtain the silicon carbide nanofiber aerogel.
The silicon carbide nanofiber aerogel in the step 5) is composed of 3C-SiC with the density of 1-8 mg/cm3The porosity is more than 98 percent.
The silicon carbide nanofiber aerogel is formed by interweaving SiC nanofibers with high length-diameter ratio in a three-dimensional space, the diameter of the SiC fibers ranges from a nanometer level to a submicron level, the diameter range of the nanometer level is 30-100 nm, and the diameter range of the submicron level is 0.1-0.6 mu m.
The length-diameter ratio of the SiC nano-fiber can reach 1.5 multiplied by 105
The invention has the beneficial effects that:
1) the silicon carbide nanofiber aerogel prepared by the invention is formed by interweaving the ultra-long SiC nanofibers with high length-diameter ratio in a three-dimensional network space. Compared with the traditional preparation method of the silicon carbide aerogel, the silicon carbide nanofiber aerogel prepared by the method has high purity, controllable pore structure and simple preparation process, and does not need to adopt complex process means such as traditional aerogel supercritical drying and the like.
2) The invention has the advantages of full reaction without subsequent calcination treatment, controllable product macro-morphology, easy realization of large-size and large-scale production and preparation of aerogel, and wide application prospect in the fields of high-temperature heat insulation, catalyst carriers, wave-absorbing materials, high-temperature composite materials and the like.
3) The invention adopts the dispersing technology of the cotton fluffer and the like, can form a fluffy and controllable raw material carbon fiber structure, is favorable for conveying reaction gas, and is favorable for the growth of nano fibers, the control of gaps of aerogel and the like. The preparation method can obtain the large-size silicon carbide nanofiber aerogel, the original shape, size and density of the large-size silicon carbide nanofiber aerogel can be controlled in a multi-dimensional mode through parameters such as an external die, raw material quality, raw material size and a filling mode, and the large-scale industrial production of the silicon carbide aerogel is easy to realize.
Drawings
Fig. 1 is a flow chart of a preparation process of silicon carbide nanofiber aerogel.
Fig. 2 is a Scanning Electron Microscope (SEM) photograph of the microstructure of the silicon carbide nanofiber aerogel prepared in example 1.
Fig. 3 is an X-ray diffraction (XRD) spectrum of the silicon carbide nanofiber aerogel prepared in example 1.
Fig. 4 is a process diagram of the rebound resilience test of the silicon carbide nanofiber aerogel prepared in example 3, 4(a) is a state diagram of the aerogel before the test, 4(b) is a state diagram of the crucible placed on the aerogel, and 4(c) is a state diagram of the aerogel after the crucible is removed, respectively.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The invention is further illustrated with reference to the accompanying drawings and specific examples. These embodiments are merely illustrative of the present invention and are not intended to limit the scope of the present invention.
The preparation process flow of the silicon carbide nanofiber aerogel is shown in figure 1.
Example 1
a. Preparing silica sol by taking tetraethoxysilane (mass fraction of 67 wt.%) as a sol raw material, water as a cross-linking agent (mass fraction of 22 wt.%) and absolute ethyl alcohol as a solvent (mass fraction of 11 wt.%), fully soaking 50g of chopped carbon fibers with the length of about 8mm in the silica sol, draining and drying to obtain 86g of surface-coated SiO2The carbon fiber aggregate of (4);
b. coating the surface with SiO2The carbon fiber aggregate is occluded and dispersed by a cotton fluffer to obtain 83g of SiO coated on the surface2The fluffy carbon fiber felt of (1);
c. adding expandable graphite (5% of ethyl orthosilicate by mass) into the silica sol prepared by the scheme of the step a, continuously stirring until the silica sol is naturally gelled, drying and grinding the gel to obtain SiO2C gel powder;
d. taking 200g of SiO2the/C gel powder is flatly laid onCoating 32g of SiO on the surface of the bottom of the graphite crucible2The carbon fiber felt is uniformly dispersed above the sol-gel powder in a square preset shape, covered with a crucible cover and placed in a high-temperature atmosphere furnace;
e. controlling temperature in high temperature atmosphere furnace, heating to 1600 deg.C, maintaining for 6 hr to obtain product with dimensions of 34cm × 25cm × 8cm and density of 4.25mg/cm3The silicon carbide nanofiber aerogel prepared by the method consists of SiC nanofibers, and is high in purity and intact in tissue structure.
The SEM photo of the silicon carbide nanofiber aerogel is shown in fig. 2, and according to the SEM photo, the silicon carbide nanofiber aerogel prepared by the present invention is constructed by interweaving ultra-long silicon carbide nanofibers in a three-dimensional network space.
The XRD spectrogram of the silicon carbide nanofiber aerogel is shown in figure 3, and the silicon carbide nanofiber aerogel prepared by the method disclosed by the invention is pure and single 3C-SiC without C component according to the XRD spectrogram, so that the carbon fiber felt is fully reacted in the preparation process disclosed by the invention.
Example 2
a. Preparing silica sol by taking tetraethoxysilane (mass fraction of 67 wt.%) as a sol raw material, water as a cross-linking agent (mass fraction of 22 wt.%) and absolute ethyl alcohol as a solvent (mass fraction of 11 wt.%), fully soaking 60g of chopped carbon fibers with the length of about 12mm in the silica sol, draining and drying to obtain 103g of surface-coated SiO2The carbon fiber aggregate of (4);
b. coating the surface with SiO2The carbon fiber aggregate is occluded and dispersed by a cotton fluffer to obtain 99g of SiO coated on the surface2The carbon fiber felt of (1);
c. adding a certain amount of expandable graphite (8 percent of the weight of the tetraethoxysilane) into the silica sol prepared by the scheme of the step a, continuously stirring the mixture until the mixture is naturally gelled, drying and grinding the gel to obtain SiO2C gel powder;
d. taking 200g of SiO2Paving the gel powder/C at the bottom of a graphite crucible, and coating 26g of the surface with SiO2The carbon fiber felt is uniformly dispersed above the sol-gel powder in a square preset shape, covered with a crucible cover and placed in a high-temperature atmosphere furnace；
e. Controlling temperature in high temperature atmosphere furnace, heating to 1600 deg.C, maintaining for 5 hr to obtain product with dimensions of 34cm × 25cm × 5cm and density of 1.41mg/cm3The silicon carbide nanofiber aerogel of (1).
The silicon carbide nanofiber aerogel with the size of about 10cm multiplied by 8cm multiplied by 7cm is cut and placed on the growing leaves due to the ultrahigh porosity (99.96%) and the extremely low density (1.41 mg/cm)3) So that the aerogel has excellent light weight property, and the silicon carbide nanofiber aerogel can be easily lifted by leaves.
Example 3
a. Preparing silica sol by taking tetraethoxysilane (mass fraction of 67 wt.%) as a sol raw material, water as a cross-linking agent (mass fraction of 22 wt.%) and absolute ethyl alcohol as a solvent (mass fraction of 11 wt.%), fully soaking 60g of chopped carbon fibers with the length of about 20mm in the silica sol, draining and drying to obtain 112g of silica sol coated on the surface of which the surface is coated with SiO2The carbon fiber aggregate of (4);
b. coating the surface with SiO2The carbon fiber aggregate is occluded and dispersed by a cotton fluffer to obtain 105g of SiO coated on the surface2The carbon fiber felt of (1);
c. adding a certain amount of expandable graphite (the mass of the expandable graphite is 10 percent of that of the ethyl orthosilicate) into the silica sol prepared by the scheme of the step a, continuously stirring the mixture until the mixture is naturally gelled, drying and grinding the gel to obtain SiO2C gel powder;
d. taking 200g of SiO2Paving the gel powder/C at the bottom of a graphite crucible, and coating 24g of the surface with SiO2The carbon fiber felt is uniformly dispersed in SiO in a square preset shape2Covering a crucible cover above the gel powder, and placing the crucible cover in a high-temperature atmosphere furnace;
e. and controlling the temperature in a high-temperature atmosphere furnace by program, heating to 1600 ℃, and preserving the heat for 5 hours to obtain the silicon carbide nano-fiber aerogel with the size of 32cm multiplied by 25cm multiplied by 7 cm.
Cutting two silicon carbide nano fiber aerogels with the size of 4.8cm multiplied by 1.5cm, and laminating up and down, wherein the whole thickness is 3cm, as shown in figure 4 (a); placing a 160g corundum crucible on two laminated aerogels, wherein the overall thickness of the two laminated aerogels is compressed from 3cm to 2cm, as shown in FIG. 4 (b); after the corundum crucible was removed, the aerogel began to rebound, after 30 seconds to the original thickness, as shown in FIG. 4 (c). The resilience experiment fully proves that the silicon carbide nanofiber aerogel prepared by the invention has excellent resilience.
Claims (10)
1. The preparation method of the silicon carbide nanofiber aerogel is characterized by comprising the following steps of:
1) SiO on carbon fiber surface2Coating: coating SiO on the surface of carbon fiber by a sol-gel method2Gelling;
2) preparing a fluffy carbon fiber felt: coating the surface with SiO2Dispersing the gelled carbon fiber aggregate to obtain a fluffy carbon fiber felt;
3)SiO2preparation of gel powder raw material: preparation of SiO by sol-gel method2C gel powder;
4) filling raw materials: mixing SiO2Laying the gel powder at the bottom of the crucible, and putting the fluffy carbon fiber felt prepared in the step 2) to SiO2Covering a crucible cover above the gel powder;
5) preparing silicon carbide nanofiber aerogel by carbothermal reduction: and (3) placing the crucible in the step 4) into a high-temperature atmosphere furnace, and preparing the silicon carbide nanofiber aerogel under the high-temperature condition.
2. The method for preparing the silicon carbide nanofiber aerogel according to claim 1, wherein the step 1) is specifically as follows: hydrolyzing ethyl orthosilicate, water and absolute ethyl alcohol as raw materials to obtain silica sol, soaking the silica sol in the degummed short-cut carbon fibers, draining and drying to obtain the surface-coated SiO2The carbon fiber aggregate of (1).
3. The preparation method of the silicon carbide nanofiber aerogel according to claim 2, wherein the length of the chopped carbon fibers is 3-80 mm.
4. The silicon carbide nanofiber as claimed in claim 1The preparation method of the aerogel is characterized in that in the step 2), the surface is coated with SiO by using a cotton fluffer or air flow impact2The carbon fiber aggregates of the gel are dispersed.
5. The method for preparing the silicon carbide nanofiber aerogel as claimed in claim 1, wherein in the step 2), the density degree of the silicon carbide nanofiber aerogel is adjusted by changing the density degree of the fluffy carbon fiber felt.
6. The method for preparing silicon carbide nanofiber aerogel according to claim 1, wherein the step 3) is specifically that tetraethoxysilane, water and absolute ethyl alcohol are hydrolyzed to obtain silica sol, expandable graphite is added into the silica sol, the mixture is continuously stirred to obtain gel, and the gel is dried and crushed to obtain SiO2C gel powder.
7. The preparation method of the silicon carbide nanofiber aerogel according to claim 2 or 6, wherein the raw materials of the silica sol comprise, by mass: 50-70% of ethyl orthosilicate, 10-20% of water and 10-40% of absolute ethyl alcohol.
8. The method for preparing the silicon carbide nanofiber aerogel according to claim 1, wherein the step 5) is specifically as follows: circularly vacuumizing the high-temperature atmosphere furnace and filling nitrogen for three times to reduce the oxygen partial pressure; heating the high-temperature atmosphere furnace to 1450-1700 ℃ at a heating rate of 1-10 ℃/min, and carrying out heat preservation sintering for 3-6 h, wherein the reaction pressure is positive pressure; and after the reaction is finished, cooling to normal temperature along with the furnace to obtain the silicon carbide nanofiber aerogel.
9. The method for preparing the silicon carbide nanofiber aerogel according to claim 1, wherein the silicon carbide nanofiber aerogel in the step 5) is composed of 3C-SiC with a density of 1-8 mg/cm3The porosity is more than 98 percent.
10. The preparation method of the silicon carbide nanofiber aerogel according to claim 1, wherein the silicon carbide nanofiber aerogel is formed by interweaving SiC nanofibers in a three-dimensional space, the diameter of the SiC fibers ranges from nanometer to submicron, the diameter of the nanometer ranges from 30 nm to 100nm, and the diameter of the submicron ranges from 0.1 μm to 0.6 μm.
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| CN115262079B (en) * | 2022-07-18 | 2024-03-22 | 浙江艾伦新材料有限公司 | Preparation method of aerogel heat-preservation Q elastic cotton |
| CN115259161A (en) * | 2022-08-10 | 2022-11-01 | 航天特种材料及工艺技术研究所 | Ring-shaped silicon carbide nanofiber aerogel material and preparation method thereof |
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