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Preparation and Applications of Silicon Carbide Monolithic Aerogels

Zhen Zhang , Shuang Zhao , Guobing Chen , Kunfeng Li , Zhifang Fei , Zichun Yang

Progress in Chemistry ›› 2021, Vol. 33 ›› Issue (9) : 1511 -1524.

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Progress in Chemistry ›› 2021, Vol. 33 ›› Issue (9) : 1511-1524 DOI: 10.7536/PC210203
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Preparation and Applications of Silicon Carbide Monolithic Aerogels
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Abstract

Silicon carbide aerogels have excellent properties such as high temperature stability, low thermal expansion coefficient, good thermal shock resistance, oxidation resistance and corrosion resistance, etc. They have great application potential in the fields of high temperature thermal insulation, electromagnetic wave adsorbing, filtration and adsorption under high temperature and high corrosive environment. However, the controllable preparation of bulk silicon carbide aerogels has always been a major challenge. As a new kind of aerogels, the preparation process of bulk SiC aerogels is more complicated than that of traditional oxide and carbon aerogels. In recent years, the research on preparation and application of SiC aerogels has entered a new stage. Many new strategies for preparing SiC aerogels have been developed, and many important progress has been made in the research of SiC aerogels in the fields of heat insulation and electromagnetic wave adsorbing. In this paper, the research progress on preparation and application of monolithic silicon carbide aerogels is reviewed. Firstly, the advantages and disadvantages of various preparation technologies are analyzed and summarized, including carbon thermal reduction method with organic/SiO2 composite aerogels, cracking method with pre-ceramic polymer, chemical vapor deposition method, high-temperature vapor-phase silicon cementation method and self-assembly method of SiC nanowire. Then the application research progress of SiC aerogel in high temperature insulation and electromagnetic wave adsorbing are introduced in detail. Finally, the development trend of SiC aerogel in the future is prospected.

Contents

1 Introduction

2 Preparation of SiC aerogels

2.1 Carbon thermal reduction of organic/SiO2composite aerogels

2.2 Cracking of pre-ceramic polymer

2.3 Chemical vapor deposition

2.4 High-temperature vapor-phase silicon cementation

2.5 Assembly of SiC nanowire

3 Applications of SiC aerogels

3.1 High-temperature thermal insulation

3.2 Electromagnetic wave adsorbing

3.3 Other applications

4 Conclusion and outlook

Graphical abstract

Keywords

silicon carbide aerogel / preparation process / high-temperature thermal insulation / electromagnetic wave adsorbing

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Zhen Zhang, Shuang Zhao, Guobing Chen, Kunfeng Li, Zhifang Fei, Zichun Yang. Preparation and Applications of Silicon Carbide Monolithic Aerogels. Progress in Chemistry, 2021, 33(9): 1511-1524 DOI:10.7536/PC210203

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1 Introduction

Aerogels, known as solidified smoke, are the lowest density solid materials known in the world. It has a three-dimensional hierarchical porous network structure, which endows it with high specific surface area (>200 m2/g), high porosity (> 90%), low density (<0.3 g/cm3) and extremely low thermal conductivity (< 0.02 W/ (m · K)), and makes it have a wide range of applications in adsorption, thermal insulation, sound insulation, noise reduction and catalysis[1⇓⇓~4]. Since Kistler first used sodium silicate as precursor and ethanol supercritical drying technology to invent SiO2 aerogel in 1931, various new aerogels have emerged and the family of aerogels has been expanding.At present, it can be divided into oxide-based aerogel, organic aerogel, carbon/carbide aerogel, other new aerogels (including metal aerogels, chalcogenide aerogels, perovskite aerogells, etc.) And Composite Aerogels[5⇓⇓~8]. In addition to some of the conventional properties of aerogels, important properties of different aerogels depend on their solid constituents. For example, TiO2 is an n-type semiconductor material with strong oxidation-reduction, chemical stability, corrosion resistance and other characteristics, so TiO2 aerogel can be used as an excellent semiconductor photocatalyst[9]; Due to the high conductivity of carbon materials, carbon aerogel is a kind of conductive aerogel with great potential applications in the fields of energy and electrocatalysis[10,11]. Silicon carbide (SiC) has excellent properties such as wide band gap, high temperature stability, low thermal expansion coefficient, high mechanical strength, good thermal shock resistance, oxidation resistance and corrosion resistance, so SiC aerogels are particularly suitable for a variety of applications in high temperature and/or highly corrosive environments, such as high temperature thermal insulation, electromagnetic wave absorption, filtration and catalyst support[12,13][14][15,16][17,18][19].
Because the temperature resistance of oxide aerogels is generally below 800 C, carbon aerogels are easy to be oxidized and ineffective when used in air atmosphere above 400 C, and organic aerogels are generally used for thermal insulation of buildings and pipelines at lower temperatures.In contrast, only ceramic aerogels have excellent high temperature resistance, oxidation resistance and thermal shock resistance, which can be used for high temperature insulation above 1000 ℃[20,21][22,23][2,24]. Silicon carbide (SiC) aerogel, as a typical ceramic aerogel, also has the advantages of high strength, corrosion resistance, low thermal expansion coefficient and infrared shielding effect, which is especially suitable for many applications in high temperature and high corrosive environments, and is a very potential high temperature thermal insulation material[25][26]. Moreover, SiC aerogels can further improve the microwave absorbing properties through the multiple microwave loss mechanism of the nanostructure, which makes SiC aerogels become a potential electromagnetic wave absorbing material applied in special environments[27]. Traditionally, carbon thermal reduction method, direct foaming method, hydrothermal method and foam gel casting method are used to prepare porous SiC materials, but these methods are not conducive to the rapid and low-cost preparation of SiC aerogels, and it is difficult to accurately control the macro and micro morphology of SiC aerogels, which greatly limits the wide application of SiC aerogel[28⇓~30][31][32⇓⇓~35]. In recent years, the research on the preparation and application of SiC aerogels has entered a new stage, many new processes for the preparation of SiC aerogels have been developed, and many important advances have been made in the fields of high temperature thermal insulation and electromagnetic wave absorption. In this paper, the research progress of SiC aerogels in recent years is reviewed from the perspectives of preparation process and application research.

2 Preparation of SiC Aerogel

The applications of SiC aerogels in high temperature insulation, electromagnetic wave absorption, filtration and other fields generally require that SiC aerogels have good blocky macromorphology and abundant three-dimensional network nanostructure. The preparation process can directly determine the morphology and structure of the material, and the material is prepared by the traditional powder sintering method, foaming method, freeze-casting method, organic foam impregnation method, hydrothermal method, foam gel casting method and silicon powder carbothermal reduction method.The prepared porous SiC mainly has large pores with the diameter of more than tens of microns, the specific surface area is small, and the products are mostly particles or whiskers, so it is difficult to prepare blocky SiC aerogels with desired macroscopic and microscopic morphologies[36,37][38⇓⇓~41]. It is still a great challenge to find a simple and environmentally friendly process to prepare SiC aerogel bulk with controllable porous nanostructure. In recent years, researchers have developed new methods to prepare high-performance bulk SiC aerogels, such as carbothermal reduction of organic /SiO2 composite aerogels, preceramic polymer pyrolysis, chemical vapor deposition, high temperature vapor infiltration and self-assembly of SiC nanowires.

2.1 Organic /SiO2 composite aerogel carbon thermal reduction method

Carbothermal reduction method has been a common method to synthesize porous SiC materials because of its advantages of simple process and high product quality. However, SiC prepared by carbothermal reduction of binary precursors of silicon oxide and carbon at high temperature generally coexists in a variety of microstructures.Comprises fibers, whiskers and the like, and the pores are formed by carbothermal reduction of the silicon oxide nanosphere core and the carbonized polymer coating to form a new ceramic skeleton and CO escape, so that the blocky SiC aerogel is difficult to obtain[41⇓~43]. In 2010, Leventis et al. Synthesized bulk SiC aerogel for the first time by using polyacrylonitrile (PAN) crosslinked SiO2 aerogel as precursor, although the synthesis process was complex, and the prepared SiC aerogel also had problems such as high apparent density (~0.5 g/cm3) and low specific surface area (~20 m2/g).However, this method can use organic polymer cross-linked silica aerogel as a template, can retain the porous structure and morphology of the original aerogel, and can prepare high-porosity bulk SiC aerogel, which brings a new idea for the synthesis of SiC aerogel[44].
The basic technical route for preparing the bulk SiC aerogel by using the organic /SiO2 composite aerogel as a precursor through a carbothermal reduction method comprises the following steps of: firstly preparing an organic /SiO2 aerogel precursor through a sol-gel method,Then the C/SiO2 composite aerogel is obtained by carbonization, and the C/SiO2 composite aerogel is subjected to high-temperature carbon (magnesium) thermal reduction (and calcination to remove free carbon) to obtain the SiC aerogel (as shown in fig. 1)[14,45⇓⇓⇓ ~49]. It was found that the structure and properties of the final SiC aerogel were directly determined by the structure of the precursor and the carbothermal reduction process in the carbothermal reduction method of organic /SiO2 composite aerogel.

2.1.1 Effect of Precursor on the Properties of SiC Aerogel

The commonly used organic precursors are mainly phenolic monomers (RF) such as resorcinol and formaldehyde, cheap and high carbon yield carbon source phenolic resin, polyurea and polyacrylonitrile[50,51][52][42][45]. The commonly used silicon sources are mainly methyl orthosilicate, ethyl orthosilicate and polysilsesquioxane[53]. However, when these raw materials are used for the preparation of the precursor, there are problems that the sol-gel process is complicated and time-consuming, a large amount of acid and base catalysts are required (even pH adjustment is required), and the silicon source and the carbon source are prepared separately and then mixed. In order to simplify the process, Kong et al. used 3-aminopropyltriethoxysilane (APTES) as silicon source to synthesize amino-hybrid RF/SiO2 aerogels by a simple one-pot method and supercritical CO2 drying, and then synthesized bulk crack-free mesoporous SiC aerogels by carbothermal reduction, with BET specific surface area of 251 m2/g, pore volume of 0.965 cm3/g and bulk density of 0.288 g/cm3[54]. Because APTES contains basic amino groups, it not only acts as a silicon source, but also acts as an internal catalyst, which greatly accelerates the hydrolysis polymerization reaction, and the Si-C bond in APTES accelerates the carbothermal reduction. The C/Si atomic ratio in the organic /SiO2 composite aerogels also has a great influence on the formation of SiC nanostructures. It is found that the mole ratio of C∶SiO2 is higher than 3 to realize the complete conversion of SiO2 to SiC[45]. If the C∶SiO2 ratio is lower than 3, the obtained SiC aerogel still contains SiO2 components, and if the C∶SiO2 ratio is much higher than 3, the SiC aerogel contains more free carbon, and the free carbon needs to be removed by a calcination process[55,56]. In addition, the three-dimensional network nanoporous structure in the organic /SiO2 mixed aerogel can serve as a diffusion path of gaseous products in the carbothermal reduction process, which is beneficial to mass transfer and rapid formation of SiC in the carbothermal reduction process and improves the efficiency of carbothermal reduction[57].
In order to obtain a complete bulk SiC aerogel, the precursor must be a complete, crack-free, uniform and defect-free bulk organic and /SiO2 composite aerogel. Before that carbothermal reduction treatment, the organic component is subject to a carbonization and pyrolysis process, a large amount of gas is release and large volume shrinkage occurs, and the original appearance of the organic component is not easy to maintain, so in the prepared organic /SiO2 composite aerogel,The skeleton structure of SiO2 aerogel should be the basic support unit, and the organic component should be wrapped around the network structure of SiO2 aerogel, so that the three-dimensional network nano-porous structure of SiC aerogel can be well retained[58]. The density of the precursor of the organic /SiO2 composite aerogel also has an important influence on the structure of the SiC aerogel. If the density of the precursor is too small, the SiC skeleton obtained after carbothermal reduction is difficult to support the three-dimensional network nanoporous structure and is easy to crack and collapse; If the density of the precursor is too high, the density of the final SiC aerogel is also too high, and it is difficult to obtain SiC aerogel with high specific surface area and low density[59]. Kong et al. Synthesized RF/SiO2 composite aerogel by one-pot method and supercritical CO2 drying, and then prepared SiC aerogel by carbothermal reduction and calcination. The obtained SiC aerogel is composed of α-SiC nanocrystals.The microstructure has a monolithic mesoporous morphology (as shown in fig. 2), the BET specific surface area is 251 m2/g, the pore volume is 0.965 cm3/g, the packing density and framework density are 0.288 g/cm3 and 3.12 g/cm3, respectively, and the porosity is 90.8%, which remains stable at a temperature close to 650 ° C[59].
SiO2 aerogel is used as a support framework for the preparation of organic /SiO2 composite aerogel by carbothermal reduction method, and the prepared SiC aerogel inherits the microscopic morphology and structure of the SiO2 aerogel, and the specific surface area is generally below 500 m2/g. The specific surface area of porous carbon and carbon aerogels is generally higher than that of SiO2 aerogels, and it is expected to increase the specific surface area of SiC aerogels by using porous carbon or carbon aerogel as a supporting framework[60]. Lu et al. used the highly porous carbon fiber skeleton as the three-dimensional space for the growth and self-assembly of SiC nanowires, and used methyltrimethoxysilane and dimethyldiethoxysilane (4:1) as silicon sources to remove excess liquid by vacuum filtration after sol formation to obtain a viscous sol and fiber complex.The SiC nanowire aerogel (SiC NWAG, as shown in fig. 3) was prepared after drying and carbothermal reduction (high temperature treatment at 1550 ℃ and 0.2 MPa argon for 2 H). The aerogel has a highly porous structure, in which the SiC nanowires are intertwined and well connected with each other, the density is controllable between 0.003~0.035 g/cm3, the porosity is > 99%, and it shows good mechanical elasticity and thermal stability[61].

2.1.2 Effect of carbothermal reduction process on the properties of SiC aerogel

Carbothermal reduction is a reaction between carbon and silica nanoparticles at T ≥ 1350 ℃, which is one of the most critical processes for the preparation of bulk SiC aerogels[38]. Reactions that may occur during carbothermal reduction include:
SiO2(s)+C(s)→SiO(g)+CO(g )
SiO2(s)+CO(g)→SiO(g)+CO2(g )
CO2(g)+C(s)→2CO(g )
SiO(g)+2C(s)→SiC(s)+CO(g)
SiO(g)+3CO(g)→SiC(s)+2CO2(g )
The general reaction formula is:
SiO2(s)+3C(s)→SiC(s)+2CO(g )
It can be seen that CO2, CO, SiO and other gases will be produced in the process of carbothermal reduction, and the organic /SiO2 composite aerogel will produce huge volume shrinkage in the process of high temperature carbonization and pyrolysis or C/SiO2 composite aerogel will produce huge volume shrinkage in the process o f carbothermal reduction.In order to make SiC aerogels keep the blocky structure and three-dimensional nano-porous network structure of organic /SiO2 mixed aerogel precursors as much as possible, the heating rate of carbothermal reduction process should be small (generally 1 ~ 2 ℃/min). The protective atmosphere is also very important in the process of carbothermal reduction. When the inert atmosphere is N2, the product usually contains a lot of Si3N4. When the inert atmosphere is Ar, SiC aerogel is obtained after carbothermal reduction[42,62]. As for the carbothermal reduction temperature, Kong et al found that SiC nanocrystals could not be obtained when the organic /SiO2 composite aerogel precursor was below 1500 ℃, but when the carbothermal reduction temperature was 1500 ℃, SiC nanocrystals appeared after heat treatment for 1 H, and the amorphous SiO2 was almost completely reduced to SiC after 5 H[49]. However, the carbothermal reduction temperature above 1500 ℃ not only greatly increases the energy consumption and equipment requirements, but also easily leads to the generation of a large number of gaseous SiO at a high temperature above 1100 ℃, resulting in a volume shrinkage of up to 40%, resulting in the destruction of the nano-porous network structure, and the prepared SiC aerogels mostly exist in the form of nano-powder or nanowires[49]. In order to reduce the carbothermal reduction temperature, Chen et al. used the C/SiO2 composite aerogel as a template, and converted it into massive mesoporous SiC aerogel (as shown in Figure 4) at a low temperature (700 ℃) through a template-limited magnesium-thermal reduction method, with a density of 0.13 g/cm3,BET and a specific surface area of 232 m2/g, which well retained the morphology and structure of the aerogel[47][47,63]. In addition, Xie et al. Synthesized a new type of carbonaceous SiC/mullite aerogel in situ from pyrocatechol-formaldehyde/silica/mullite mixed aerogel (CF/SiO2/AlOOH). Compared with the conventional method, the addition of mullite reduced the temperature of SiC phase formation[64]. The composite aerogel has an average pore size of 6.531 nm and a specific surface area of 69.61 m2/g. In addition, the structural effect of mullite phase is beneficial to improve the oxidation resistance of the composite aerogel due to its high melting temperature, good stability, low oxygen permeability and thermal expansion coefficient close to that of SiC.
Complete bulk SiC aerogels can be prepared by sol-gel method and carbothermal reduction method with organic and /SiO2 composite aerogels as precursors. However, this method is based on the premise of preparing RF/SiO2 aerogels with good morphology, which has the problems of complex process and long preparation cycle.The problem of high carbothermal reduction temperature needs to be further solved, and the huge volume contraction in the process of high temperature carbothermal reduction is easy to cause internal stress, which makes it difficult to prepare large size SiC aerogel components. Therefore, the new idea of using flexible carbon fibers as SiC support structure and growth template may be an important direction for future research of this technology.

2.2 Preceramic polymer pyrolysis method

The synthesis of aerogels from preceramic polymers is a new field of aerogel preparation. For example, SiC, SiOC, SiCN and SiBC/N aerogels can be synthesized from silicon-based preceramic polymers[65⇓⇓~68][69,70][71]. For SiC aerogels, this preceramic polymer pyrolysis strategy can avoid the carbothermal reduction of organic /SiO2 composite aerogels and get rid of the dependence on the preparation of RF/SiO2 aerogels first, and the Si and C elements in the preceramic polymer precursor are mixed at the atomic level, so the high temperature heat treatment temperature is significantly reduced[72]. According to the different molding methods of pre-ceramic polymer, it can be divided into direct cross-linking molding method of pre-ceramic polymer and nano-casting molding method.

2.2.1 Crosslinking molding method

The process route for preparing the SiC aerogel by the cross-linking forming method comprises the following steps of: firstly, controlling the cross-linking of a pre-ceramic polymer in a highly diluted solution to generate a wet gel; then, drying by using a supercritical CO2 to remove the solvent to obtain a pre-ceramic polymer aerogel; and finally, converting the pre-ceramic polymer aerogel into the SiC aerogel through a pyrolysis process[73]. The structure and pyrolysis process of the preceramic polymer precursor directly determine the structure and properties of the final SiC aerogel. The composition, macro/micro morphology and nanostructure of SiC aerogels are derived from their preceramic polymer precursors[74,75]. The polymer precursor is mainly composed of Si, C, H and N and/or O atoms. In order to obtain SiC aerogel without other substances (Si3N4, SiO2), the polymer precursor with high Si and C content should be selected as far as possible[76⇓~78]. The porosity of preceramic polymer aerogels and SiC aerogels is mainly affected by the concentration of solution in the process of dilution and crosslinking. The crosslinking reaction needs to be carried out in a highly diluted solution, and the low concentration of reactants will reduce the reaction rate and prolong the crosslinking time. Therefore, it is generally necessary to add catalysts to accelerate the crosslinking reaction, and solvothermal methods are often used to promote the crosslinking of preceramic polymers. The high temperature and high pressure environment provided by solvothermal method can not only shorten the reaction time, but also prepare SiC aerogels with different shapes from 0 D to 3D by using a mold to shape the pre-ceramic polymer[79]. During the crosslinking process, the polymer forms spherical nanoparticles through nucleation and growth, and phase separation occurs with the solvent. These spherical nanoparticles continue to crosslink to form a three-dimensional nanoporous network structure, and then form a wet gel. The microstructure of the preceramic polymer aerogel can be controlled by adjusting the amounts of reactants, catalysts and solvents, the types of solvents and the process parameters, thereby affecting the structure of the SiC aerogel[80,81]. In the process of pyrolysis, the pyrolysis atmosphere has an important influence on the composition of the final products. The pyrolysis under N2 atmosphere is easy to cause the products to contain Si3N4. Pyrolysis is carried out in Ar atmosphere, and the obtained product generally contains a free carbon phase; Pure SiC aerogels without free carbon phase can be obtained by pyrolysis in H2 atmosphere. As for the heating rate, unlike many reactions in the carbothermal reduction process, only the pyrolysis rearrangement and the escape of small molecules occur in the pyrolysis process of the preceramic precursor, so the heating rate can be slightly faster[82]. In 2014, Zera et al., using polycarbosilane as a precursor, cross-linked divinylbenzene and commercial polycarbosilane to form a wet gel by Pt-catalyzed hydrosilylation in a highly diluted solution, and then replaced by cyclohexane and dried by supercritical CO2 to obtain an aerogel.Finally, highly porous carbon-rich SiC/C aerogels with density of 0.166 g/cm3, specific surface area of 444 m2/g, micropore volume of 0.79 cm3/g and compressive strength of 1.6 MPa were prepared by pyrolysis and heat treatment (Ar gas, above 1 500 ℃)[82].

2.2.2 Nano pouring forming method

The nano-casting method is to pour the pre-ceramic polymer precursor into the template by pressure-assisted or wet impregnation method.The advantage of nano-casting method is that it can make the SiC aerogel obtain more ideal micromorphology, but it also has the disadvantages of complex process and high cost caused by the use of template[79].
Using KIT-6 silica as a hard template and polycarbosilane as a preceramic polymer precursor, Wang et al. Designed and prepared ordered mesoporous SiC bulk with three-dimensional bicontinuous cubic phase structure by pressure-assisted preceramic polymer nano-casting method, which is amorphous below 1200 ℃.The specific surface area and pore volume of the ordered mesoporous SiC bulk are up to 942 m2/g and 0.864 cm3/g, respectively, and the pore size is about 3.6 nm. Although the SiC skeleton in the ordered mesoporous SiC bulk transforms from amorphous to nanocrystalline after heat treatment at 1400 ℃ in Ar atmosphere, it does not affect the maintenance of the overall macroscopic morphology, and the microstructure is also well maintained, showing a very good stability[83].
Wood is a kind of porous composite material with anisotropic structure, and the axial arrangement of its tracheids can make the precursor penetrate into its pore structure, which makes it possible to prepare new nano-porous materials using wood as a template. In order to solve the problems of high cost and complex removal process of traditional template preparation, Wang et al. Used balsa wood cellulose nanofiber aerogel as biological template and polycarbosilane as precursor to prepare biomorphic silicon carbide (BioSiC) ceramics with highly interconnected porous three-dimensional structure by precursor solution infiltration and pyrolysis[84]. The results show that the framework structure of cellulose can be perfectly replicated by polycarbosilane ceramicization.BioSiC has high porosity (61. 03%) and low density (0.86 g/cm3)[84,85].
SiC aerogels prepared by preceramic polymer strategy have the advantages of simple process and low pyrolysis temperature.However, the prepared SiC aerogels are generally composed of spherical nanoparticles with necklace-like ceramic nanoparticles, which leads to serious brittleness, no bending and poor elasticity. In addition, the pore structure of SiC aerogels was controlled by the crosslinking temperature and time, the amount and properties of the solvent. When the nano-casting method is used, the pore structure replicates the pore structure of the template. In general, the ability to control the pore structure is relatively poor, the synthesized pore structure is relatively large, and the specific surface area is small.

2.3 Chemical Vapor Deposition

Preparing SiC aerogel by chemical vapor deposition method refers to preparing SiC nano structure units in a template with a three-dimensional nano porous network structure by applying polymer pyrolysis chemical vapor deposition (PPCVD),With the gradual increase of the building units, the SiC nanostructure units will self-assemble, and the SiC aerogel can be obtained after removing the template, and the prepared SiC aerogel can better maintain the shape and size of the template[86⇓~88]. Porous carbon materials are often used as templates and growth substrates for SiC aerogels due to their advantages such as uniform pores, stable skeleton structure, high porosity and low oxidation temperature. Li et al. Deposited SiC nanowires in the pores of carbon foam by PPCVD process using polycarbosilane as precursor, and then removed the carbon foam by high temperature oxidation.SiC nanowire aerogels with highly porous 3D structure composed of ultra-long SiC nanowires were synthesized, and a large number of SiC nanowires with diameters of 80-100 nm and lengths of hundreds of microns were interwoven to form a highly porous 3D nanowire structure of SiC aerogels.Its density is about 0.03 g/cm3, high temperature oxidation resistance temperature is 750 ℃, compressive strength is 0. 11 MPa, thermal conductivity is 0. 03 W/ (m · K) at room temperature in He atmosphere, and it is nonflammable, suitable for high temperature insulation, ceramic matrix composites, high temperature flue gas filters, fireproof materials and catalyst carriers[17]. Su et al. Prepared SiC nanowires by chemical vapor deposition, and used them as building units to make a large number of 3C-SiC nanowires overlap each other through electrostatic interaction and Van der Waals force to prepare highly porous three-dimensional SiC nanowire aerogel, whose density is as low as 5 mg/cm3, porosity is as high as 99.8%, and the maximum recoverable compressive strain is as high as 70%.And has excellent heat insulation (the thermal conductivity is 0.026 W/ (m · K) at normal temperature and 0.11 W/ (m · K) at 800 deg C), high temperature resistance (2 H at 1500 deg C in inert atmosphere) and oxidation resistance (2 H at 900 deg C in air), thereby having wide application prospect in the fields of heat insulation, adsorption and the like[18].
Yu et al. designed and prepared a three-dimensional cross-linked SiCw reinforced SiC foam SiCw-SiC by using melamine-based carbon foam as a flexible matrix template and a high-temperature ceramic material with excellent thermal stability and low thermal conductivity as a reinforcement through a two-step chemical vapor infiltration method and an oxidation process. Because the carbon skeleton is removed through the oxidation process, the SiC skeleton is a hollow structure with a density of 0.11~0.12 g/cm3.The porosity of the foam is more than 96%, and the average pore size of the foam is effectively reduced due to the fact that the SiC whiskers are uniformly dispersed in the pores of the hollow SiC skeleton foam, so that the thermal conductivity at room temperature is 0.040 to 0.075 W/ (m · K) and slowly increases with the increase of temperature; and in addition, the thermal conductivity is reduced by increasing the amount of SiC whiskers or reducing the size of the SiC whiskers, so that the foam has great application potential in the field of high-temperature thermal insulation[89]. Xu et al. First prepared graphene aerogel template by improved hydrothermal reduction and non-contact freeze-drying technology, and then prepared β-SiC aerogels (β-SiCAGs) by template-assisted chemical vapor deposition, with a porosity of 99.99% and a specific surface area of 1080 m2/g[90]. β-SiCAGs is composed of nano-layered double-wall pore structure, which presents a hyperbolic structure.This special superstructure design endows the material with negative Poisson's ratio and negative thermal expansion characteristics, so that it has good thermal stability and excellent deformability.At the same time, it shows the advantages of ultra-light, super-elastic, high thermal stability and excellent thermal insulation. With strains up to 95%, β-SiCAGs aerogels show attractive mechanical properties compared to ceramic aerogels with a one-dimensional fibrous structure.
SiC aerogels prepared by chemical vapor deposition are mostly composed of SiC nanowires, so they have good elasticity, bending and reversible compressibility. However, the preparation process of chemical vapor deposition requires harsh conditions and high cost, which is not conducive to large-scale industrial production.

2.4 High temperature gas phase siliconizing

The preparation of SiC aerogel by high temperature vapor infiltration method refers to the high temperature vapor infiltration of porous carbon materials with gaseous silicon (Si vapor and gaseous SiO) in a high temperature vacuum environment, so that the gaseous silicon enters the porous structure and reacts with carbon components to form SiC, and then SiC aerogel is obtained[91]. Using graphene foam (synthesized by CVD method) as a template, Chabi et al. Prepared three-dimensional SiC aerogel with low density and high strength by carbothermal reduction of SiO. The skeleton of the aerogel with a density of 0.009~0.017 g/cm3,SiC is composed of ultra-thin SiC sheets (thickness of 2 ~ 3 nm) and highly flexible 1D SiC nanowires, which is a mixture of α and β phase SiC, showing excellent compressive and thermal insulation properties[92].
Compared with traditional porous carbon materials, porous carbon synthesized from biomass as carbon precursor has the advantages of low cost and simple process, and the preparation and synthesis of materials using biomass as raw materials has become an important research direction. Liang et al. used cheap and widely available biomass materials such as dough and eggplant as raw materials to prepare new lightweight, high-strength and hierarchical porous SiC aerogels with density of 0.076 g/cm3 by freeze-drying, carbonization and high temperature gas phase siliconizing process (1500 ℃).The porosity is 97. 6%, the thermal conductivity is as low as 0. 02 W/ (m · K), and the compressive strength is as high as 9. 8 MPa, which indicates that the prepared SiC aerogel has great application potential in the fields of high-performance electromagnetic absorption materials and thermal insulation materials in the aerospace field[93,94][93⇓~95]. Although the biomass-derived strategy for the synthesis of SiC aerogels has the advantage of environmental protection, it should be noted that the biomass generally contains nitrogen, phosphorus, sulfur and other heteroatoms, which will be introduced into the prepared SiC aerogels in situ, and will have a great impact on the properties of the materials.
The preparation of SiC aerogels by high temperature vapor infiltration method is relatively simple, which has the advantages of short preparation cycle, adjustable composition and easy post-processing, but also has the problems of high heat treatment temperature and long reaction time. The preparation of SiC aerogels by high temperature vapor infiltration has high requirements for the initial porous carbon material, because the microstructure and morphology of porous carbon directly determine the microstructure of the prepared SiC aerogels. In addition, SiC aerogels prepared by high temperature vapor infiltration generally inherit the brittleness of porous carbon materials, and the preparation of SiC aerogels with good flexibility and bendability may be an important research direction in the future.

2.5 SiC nanowire assembly method

Compared with oxide ceramic aerogels, SiC aerogels have excellent high temperature chemical stability and high temperature resistance under harsh service conditions, but the problem of intrinsic brittleness still needs to be further solved. In recent years, it has been proved to be an effective way to overcome the brittleness of ceramic aerogels and achieve elastic compressibility by using one-dimensional or two-dimensional nanostructure units to construct structures with good interconnectivity and high porosity, such as carbon nanotube aerogels, carbon nanofiber aerogels, graphene aerogels and α-Si3N4 nanoribbon elastic aerogells[96,97][96,98]. SiC nanowires not only have the excellent properties of SiC ceramics, but also show excellent flexibility, elasticity, high bending strength and Young's modulus, so the preparation of three-dimensional SiC nanowire aerogels is an important idea to improve the brittleness of SiC aerogels[19,99,100]. Recently, through various bottom-up methods, researchers have prepared some novel SiC aerogels composed of one-dimensional SiC nanostructures (nanotubes, nanowires, etc.)[101][102]. An et al. Synthesized a new type of flexible and recyclable SiC nanofiber aerogel (SiCnf aerogel) by electrospinning and freeze-drying. The prepared SiCnf aerogel has low density (0.039~0.041 g/cm3), excellent thermal insulation (0.025 ~ 0.031 W/ (m · K)) and recoverable strain mechanical energy (~ 40%)[15].
Su et al. Prepared SiC@SiO2 nanowire aerogels with anisotropic and hierarchical microstructure of nanowire assembly by directional solidification casting and subsequent heat treatment, which have low thermal conductivity of 0.014 W/ (m · K) and high stiffness.With a specific modulus of about 24.7 kN · m/kg, it has excellent thermal and chemical stability even under butane burner heating at 1200 ° C (as shown in Figure 5), making it an ideal insulation material for extreme conditions[103].
The SiC aerogel prepared by the SiC nanowire self-assembly method has excellent flexibility, elasticity and high bendability, and is simple in process and easy to prepare on a large scale. However, the cost of high-quality SiC nanowire building blocks is high, and the prepared SiC nanowire aerogels are composed of physical bonds such as van der Waals forces and electrostatic forces between nanowires, which have low strength and poor tensile properties, and are vulnerable to structural degradation under rapid thermal shock or high temperature[101,102]. In addition, the inhibition effect of the micro nanowire assembly structure on the gaseous heat conduction is limited, and the thermal insulation performance of the SiC nanowire aerogel still needs to be further reduced.

3 Application of SiC Aerogel

Compared with porous SiC ceramics, SiC aerogels have the advantages of abundant mesoporous structure, high specific surface area and low density, and show great potential applications in the fields of high temperature thermal insulation, electromagnetic wave absorption and adsorption.

3.1 High temperature insulation

Thermal insulation under extreme conditions, such as long-term high temperature service environments in aerospace and thermal power, requires the design and preparation of high temperature thermal insulation materials with excellent stability and reliability. Ceramic aerogel is a kind of high performance material in the field of high temperature thermal insulation because of its low density, low thermal conductivity, high fire resistance and high corrosion resistance. However, traditional oxide ceramic aerogels have the problem of insufficient temperature resistance, and are prone to structural fragmentation and volume shrinkage under long-term high temperature exposure[104]. Compared with SiO2 aerogels, carbon aerogels or other polymer aerogels, SiC aerogel shows better physical, chemical, mechanical and thermal stability under severe service conditions. Rewatkar et al. prepared high-strength bulk SiC aerogel with porosity > 85%, compressive strength of (37 ± 7) MPa and thermal conductivity of (0.16 ± 0.010) W/ (m · K) measured by laser scintillation method by carbothermal reduction of polyurea crosslinked silica xerogel powder formed by cold isostatic pressing[42]. It can be seen that SiC aerogels prepared by traditional carbothermal reduction method have high density and strength, but poor thermal insulation performance, which is attributed to their low porosity and poor pore structure. Therefore, the researchers improved the carbothermal reduction method, using organic and /SiO2 composite aerogels as the supporting framework and precursor, and endowed SiC aerogels with rich three-dimensional nanoporous network structure[49,52]. An et al. selected An alkaline silica sol as a supplementary silicon source, and through carbothermal reduction and calcination, converted the organic /SiO2 composite aerogel into a monolithic silicon carbide SiC aerogel with a mesoporous structure, a low thermal conductivity of 0.049 W/ (m · K), a relatively high compressive strength of 1.32 MPa, and a specific surface area of 162 m2/g[14,50].
SiC aerogels synthesized by carbothermal reduction method and preceramic polymer pyrolysis method have made great progress in thermal insulation and mechanical strength, but they have the shortcomings of brittleness and no bending. The mechanical properties of aerogels depend on their microstructure and framework characteristics. Aerogels based on one-dimensional and two-dimensional nanostructure units show high compression and recovery properties under large strain. Therefore, researchers have designed and prepared SiC nanowire aerogels with good flexibility and bending properties by chemical vapor deposition or self-assembly of SiC nano-units[17,89][18]. An et al. Synthesized a new type of SiCnf aerogel by electrospinning and freeze-drying method. The density of the aerogel can be adjusted between 0.039~0.041 g/cm3, showing excellent thermal insulation performance, thermal conductivity of 0.025 ~ 0.031 W/ (m · K), and recoverable compressive strain up to ~ 40%, which can be used as high temperature thermal insulation materials in vibration environment[15]. Using graphene aerogel as a template, Xu et al. prepared β silicon carbide aerogel by template-free catalyst-free chemical vapor deposition method, which showed superelasticity (strain up to 95%), thermal superinsulation and thermal stability at high temperature, and could withstand severe thermal shock at ~ 275 ℃/s and long-term exposure to air at 900 ℃[90].
In order to reduce the cost and simplify the process, Lu et al. Proposed a growth space-assisted method to prepare elastic SiC nanowire aerogels with controllable density and ideal shape (as shown in Figure 6).Wherein the SiC nanowires are mutually entangled and well connected, and show good mechanical elasticity and excellent high-temperature stability (the highest use temperature in argon and air can reach 1400 deg C and 1000 deg C respectively),The SiC nanowire aerogels with a thickness of 2 cm were exposed to butane torch flame (~ 1300 ℃), and the back surface temperature was kept below 170 ℃ for 5 min. The macro and micro morphologies of the ablation surface did not change significantly after 1000 s, which indicated that the SiC nanowire aerogels had excellent high temperature thermal insulation properties[61].
Researchers have also prepared high-performance SiC aerogels using biomass materials[94]. As mentioned above, Liang et al. proposed a novel biomass-derived strategy for the synthesis of SiC aerogels. Using biomass eggplant as a precursor, a lightweight and high-strength SiC aerogel with a three-dimensional network structure and in-situ grown SiC nanowires was prepared by freeze-drying, direct graphitization, and high temperature gas phase siliconizing processes. The density was 0.076 g/cm3 and the porosity was 97.6%[93]. Compared with silicon-based carbon aerogels, the compressive strength of SiC aerogels with in-situ grown SiC nanowires increases by nearly 50 times to 2. 12 MPa, and the thermal conductivity is only 0. 035 W/ (m · K).
High temperature thermal insulation is the most important application of SiC aerogel at present, and great progress has been made. The thermal conductivity at room temperature and pressure can be as low as 0.025 W/ (m · K), but the mechanical properties still need to be improved. SiC nanowire aerogel composed of one-dimensional SiC nanowires is an effective method to endow it with high bending and flexibility (as shown in Table 1). Unlike traditional oxide aerogels, which are mostly amorphous, SiC aerogels contain abundant crystals, and the thermal conduction in the SiC skeleton is mainly phonon transport, while phonon scattering is attributed to defects in the lattice, such as impurities, vacancies, oxygen content in the lattice, gaps and dislocations at room temperature, which are the key factors determining the thermal conductivity of the material[105⇓⇓~108]. At present, the research of SiC aerogels for high temperature thermal insulation is mainly focused on material preparation and performance characterization, and there are few studies on the thermal conduction mechanism and thermal insulation mechanism of SiC aerogels.

3.2 Lectromagnetic wave absorption

With the rapid development of modern electronic information technology, it not only promotes the progress of human society, but also causes new problems such as electromagnetic information leakage, electromagnetic environmental pollution and electromagnetic interference[105,109]. Moreover, electromagnetic waves in the environment will not only interfere with other electronic devices and cause malfunctions, but also damage the physical and mental health of human beings. Although traditional metal materials have good electromagnetic wave absorbing properties, they have the problems of high density and easy corrosion. Therefore, it is of great significance to design and prepare new electromagnetic interference materials with light weight, high strength, high thermal stability and excellent electromagnetic wave absorption ability[110]. Silicon carbide (SiC) is an important wide band gap semiconductor material with good dielectric properties and ideal microwave absorption properties, which has been widely studied as an electromagnetic wave absorbing material[106,111]. In recent years, SiC aerogels have attracted much attention as a new type of electromagnetic wave absorbing material, because the three-dimensional nano-network porous structure of aerogels can effectively improve the electromagnetic wave absorbing properties by increasing the number of reflections of electromagnetic waves in the nano-pores[16]. An et al prepared C/SiO2/SiC ternary aerogels using formaldehyde and catechol as carbon sources and 3-aminopropyl-3-ethoxysilane as silicon source through co-gelation, supercritical drying and high temperature carbothermal reduction process. The density of the composite aerogel is between 0.118~0.271 g/cm3, and the specific surface area is up to 628~774 m2/g. The composite aerogel has electromagnetic wave absorbing function dominated by absorption characteristics, and the electromagnetic interface shielding coefficient is 24 dB in the range of 12. 4 ~ 18.0 GHz[54].
Biomass has shown great application potential in the design and preparation of new materials due to its advantages of cheapness, reproducibility, biodegradability and environmental friendliness. As mentioned above, Liang et al prepared SiC aerogel with three-dimensional network structure and in-situ grown SiC nanowires (as shown in Figure 7) by drying, carbonizing and high temperature gas phase siliconizing process (1500 ℃) using biomass material eggplant as raw material.The synergistic effect of the SiC network skeleton and the in-situ grown one-dimensional SiC nanowires on the SiC network skeleton endows the aerogel with excellent electromagnetic wave absorption properties and mechanical properties[93]. The highly porous and cross-linked SiC network not only increases the reflection and absorption effect of electromagnetic waves, but also prolongs the thermal propagation path, while the SiC nanowires composed of numerous stacking faults and heterojunctions play an important role in reducing the energy of electromagnetic waves and enhancing the strength of the skeleton[91].
With the development of 5G technology and flexible electronic devices, the demand for flexible electromagnetic wave absorbing materials is increasingly urgent[112]. As mentioned above, the SiC nanofiber aerogel prepared by An et al. shows excellent electromagnetic wave absorption characteristics, with An effective absorption bandwidth of 9 ~ 11.5 GHz (reflection loss < -10 dB, absorbing more than 90% of the EM wave), and the minimum reflection loss value of -21.41 dB at 10.5 GHz, with a thickness of 3 mm, which can be used as electromagnetic wave absorption materials in harsh environments[15][15]. In order to further improve the electromagnetic absorbing properties of SiC aerogels, SiC is often combined with other nanostructured absorbing materials to prepare composites. Jiang et al. fabricated a new type of lightweight spongy graphene @ SiC aerogel by freeze-casting and thermal annealing. The density of the aerogel is as low as 0.072 g/cm3. The minimum reflection loss of a typical sample reaches 34.7 dB at 10.52 GHz (thickness is 3 mm), and the effective bandwidth of the reflection bandwidth ≤ -10 dB can reach 4.7 GHz[16].
It can be seen that the research on SiC aerogels as electromagnetic radiation absorbing materials is still in its infancy. In order to further improve the EM wave absorption properties of SiC aerogels, magnetic metal or oxide particles (including Fe, Fe3O4, Co, Ni, NiFe2O4 and NiO) and non-magnetic oxides (such as ZnO) can be introduced into the SiC aerogels to prepare surface modified and SiC hybrid aerogel composites, which can further improve the EM wave absorption properties of SiC aerogel through synergistic absorption. In addition, lightweight is also an important performance index to be further improved.

3.3 Other application

SiC aerogel not only has the characteristics of low density, large specific surface area and low thermal conductivity of aerogel, but also has the properties of high temperature resistance, oxidation resistance, corrosion resistance, high conductivity, high wave absorption and high opacity of SiC.In addition to the huge application potential in the fields of high temperature heat insulation and electromagnetic wave absorption, it also shows broad application prospects in the fields of catalyst carrier, filter, adsorption, electronics and so on[113].
Flexible SiC aerogels can be used as electrical pressure sensors in electromechanical microdevices due to their excellent electrical conductivity. Chen et al. prepared SiC nanowire aerogel (SiCN WAG) with a density in the range of 0.115~0.125 g/cm3 by carbothermal reduction of SiO2 with kitchen sugar using NH4Cl as a foaming agent[114]. SiCN-WAG has a core-shell structure. The core is composed of short and entangled SiC whiskers embedded with SiC flakes, while the shell is composed of many smooth SiCNWs hundreds of microns long. The compressive modulus of SiCNWAG is about 1.35 MPa, and it can recover after 100 cycles at 20% strain under cyclic compressive loading, so it can be used as a sensitive pressure sensor. SiCNW aerogel has excellent electromechanical sensing capability, high sensitivity, large resistance response and excellent stability, with a strain coefficient of up to 87. It also has a stable wide-range compressive response, which is hundreds of times higher than that of carbon-based composite sensors. It is a very potential pressure sensor for monitoring structural damage or capturing shocks in high temperature environments.
Due to the advantages of high specific surface area, high pore volume and high physical and chemical stability, SiC aerogels can be used as adsorbents for small gas molecules. Kong et al. designed and prepared a reusable bulk amino-functionalized SiC aerogel (AFMSiCA) by co-gelation, supercritical drying, carbothermal reduction and 3-aminopropyltriethoxysilane (APTES) loading amino process, which can be used as a carrier for CO2 adsorbents.It was found that the adsorption performance of AFMSiCA for CO2 was basically unchanged at 25 ℃ ~ 75 ℃ in 1% air flow, and it had good adaptability to temperature and good recycling performance, and the adsorption performance did not decrease significantly after 12 times[51].
The treatment of industrial wastewater from textile industry is an important issue to control the quality of wastewater. SiC aerogels with high surface area, large and uniform pore size and tunable pore structure can be used as adsorbents either directly or after selective grafting of functional groups to specific contaminants. Bruzzoniti et al. designed and prepared polymer-derived SiC aerogels from liquid allylhydrogenated polycarbosilane as adsorbents for the removal of organic dyes (methylene blue (MB) and rhodamine B (RB)) from aqueous solutions[115]. The aerogel can efficiently remove MB and RB from aqueous solutions compared to polymer-derived SiC foam and commercially available mesoporous silica, and has a higher capacity compared to SiC foam due to its higher surface area. Su et al. Prepared highly porous three-dimensional SiC nanowire aerogel by chemical vapor deposition, and obtained ultra-light and reversibly compressible SiC nanowire ceramic aerogel, which showed adsorption selectivity and high adsorption capacity (130-237 G/G) for low-viscosity organic solutions[18].
Flexible semiconductor nanowire paper is an important component in flexible electronic or optoelectronic devices, solar cells, batteries, supercapacitors and so on. As SiC is a new generation of wide band gap semiconductor material, SiC nanowire aerogel paper has attracted much attention because of its unique advantages, such as high surface area, high permeability, low density, large porosity and extraordinary flexibility and stability, which has a unique role in the field of flexible or wearable electronic or optoelectronic components. Chen et al. Synthesized SiC nanowires using carbon fibers and carbonaceous silica xerogel as raw materials by a catalyst-free carbothermal reduction method, and then expansively synthesized a new type of SiC nanowire aerogel non-woven fabric through a rolling process (as shown in Figure 8)[116,117]. The free-standing SiC nanowire aerogel non-woven fabric has high flexibility, high mechanical strength, excellent fire resistance and thermal stability, and has great application potential in the fields of hot gas filtration, energy storage, catalyst carriers, ceramic or metal matrix composites, radiation resistant fabrics, high-temperature ablation resistant materials and the like.

4 Conclusion and prospect

As a new type of aerogel, the preparation process of bulk SiC aerogel is more complex than that of traditional oxide and carbon aerogels. The preparation process of bulk SiC aerogel is a key technology in aerogel science. At present, there are still some shortcomings in various preparation processes of SiC aerogels. For example, the carbothermal reduction method of organic and /SiO2 composite aerogels has the problems of complex process, long preparation period, high carbothermal reduction temperature and difficult preparation of large-size and special-shaped SiC aerogel components. How to solve the problems of large shrinkage and easy cracking of aerogels is the difficulty and key of this technology. SiC aerogels prepared by preceramic polymer strategy have the disadvantages of poor pore structure control ability, brittleness, no bending and poor elasticity, so it is a great challenge to further improve their mechanical properties and high temperature application properties. Chemical vapor deposition (CVD) has the problems of harsh conditions, high cost and not conducive to industrial production. It is of great significance to prepare high-quality SiC by this strategy and then accurately characterize and study its properties for the study of SiC thermal insulation and microwave absorption mechanism. High temperature vapor infiltration has the problems of high heat treatment temperature and long reaction time, but the idea of using porous carbon and carbon aerogel as templates brings more possibilities for the pore structure control of SiC aerogels. The new idea of using flexible carbon fibers as SiC support structure and growth template is an important direction for the future research of SiC aerogels. The self-assembly method of SiC nanowires has the problems of high cost, low strength and poor tensile properties of SiC nanowire aerogels, however, the prepared SiC aerogels have excellent flexibility, elasticity and high bendability, and the process is simple and easy to prepare on a large scale, which is the focus of research on high-performance SiC aerogels in the future. The application of SiC aerogels in high temperature insulation has made great progress, but the mechanical properties still need to be improved.There are few studies on the thermal conduction mechanism and thermal insulation mechanism, and the research of SiC aerogels as electromagnetic wave absorbing materials needs to be further studied. The future research directions of SiC aerogels may include the following aspects: (1) Developing simple and low-cost mass production technology to prepare SiC aerogels with high strength, flexibility and high thermal stability. Preparation is the basis of application, and the practical application of SiC aerogels can be realized only when various high-performance SiC aerogels are prepared first. (2) The heat transfer mechanism, heat insulation mechanism and electromagnetic wave absorption mechanism of SiC aerogel were studied. SiC Aerogels are different from traditional amorphous oxide aerogels in that their nanostructures contain abundant crystal structures, which inevitably leads to the fact that the traditional mechanisms of heat transfer, thermal insulation and electromagnetic wave absorption of aerogels are not fully applicable to SiC aerogels.Therefore, it is necessary to study the heat transfer mechanism, thermal insulation mechanism and electromagnetic wave absorption mechanism of SiC aerogels, and the study of the mechanism is also helpful to provide guidance for the design and preparation of SiC aerogels. And (3) expanding the application field of the SiC aerogel. SiC aerogels have both the material properties of SiC and the structural properties of aerogels, with excellent thermal stability and impact resistance, low thermal expansion, excellent mechanical strength and high chemical stability, which have great potential applications in many fields, and the new applications of SiC aerogels will help to promote the development of SiC aerogel.

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Funding

National Natural Science Foundation of China(51802347)

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