Review on synthesis, structure, physical and chemical properties and functional characteristics of porous silicon carbide

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JIEC 3283 1–14 Journal of Industrial and Engineering Chemistry xxx (2016) xxx–xxx

Contents lists available at ScienceDirect

Journal of Industrial and Engineering Chemistry journal homepage: www.elsevier.com/locate/jiec

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Review

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Review on synthesis, structure, physical and chemical properties and functional characteristics of porous silicon carbide

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Nataliya D. Shcherban*

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L.V. Pisarzhevsky Institute of Physical Chemistry, NAS of Ukraine, 31 pr. Nauky, Kyiv 03028, Ukraine

A R T I C L E I N F O

Article history: Received 26 August 2016 Received in revised form 11 December 2016 Accepted 6 February 2017 Available online xxx Keywords: Silicon carbide Porosity Template Nanocasting Support

A B S T R A C T

The available literary data on the methods of obtaining, structure, sorption properties and functional characteristics of porous silicon carbide were analyzed and summarized. The features and prospects of using of porous silicon carbide in catalysis, adsorption, electrochemistry etc. were shown. Some general comments about the state and possible directions of development of the researches in the area of physical chemistry of porous silicon carbide were presented. © 2017 The Korean Society of Industrial and Engineering Chemistry. Published by Elsevier B.V. All rights reserved.

Contents Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Methods of obtaining of porous silicon carbide . . . . . . . . . . . Electrochemical etching of massive silicon carbide . . . . Shape memory synthesis . . . . . . . . . . . . . . . . . . . . . . . . . Use of silicon as the initial substance . . . . . . . . . . . . . . . Carbothermal reduction . . . . . . . . . . . . . . . . . . . . . . . . . . Magnesiothermic reduction of carbon–silica composites Nanocasting using polycarbosilanes . . . . . . . . . . . . . . . . . Other methods of synthesis of silicon carbide . . . . . . . . Application of porous silicon carbide . . . . . . . . . . . . . . . . . . . Use of silicon carbide in catalysis . . . . . . . . . . . . . . . . . . Hydrogen adsorption on porous silicon carbide . . . . . . . Electrochemical application . . . . . . . . . . . . . . . . . . . . . . . Silicon carbide based ceramics . . . . . . . . . . . . . . . . . . . . . Other applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Conclusions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

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Introduction

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Considering the fact that most of the catalytic reactions take place at high temperatures and in aggressive media, there is a necessity of creation of catalyst supports with high thermal

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* Fax: +380 445256216. E-mail address: [email protected] (N.D. Shcherban).

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stability and chemical resistance. The energy problems of the present initiate the development of an alternative energy sources and the use of solar energy for realization of catalytic chemical reactions particularly photocatalytic. This leads to the new requirements for materials of different functional purpose – high thermal, mechanical and chemical stability, high thermal conductivity etc. Silicon carbide has almost all of these properties, so it can be considered suitable as a basis of the efficient catalysts [1].

http://dx.doi.org/10.1016/j.jiec.2017.02.002 1226-086X/© 2017 The Korean Society of Industrial and Engineering Chemistry. Published by Elsevier B.V. All rights reserved.

Please cite this article in press as: N.D. Shcherban, Review on synthesis, structure, physical and chemical properties and functional characteristics of porous silicon carbide, J. Ind. Eng. Chem. (2017), http://dx.doi.org/10.1016/j.jiec.2017.02.002

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N.D. Shcherban / Journal of Industrial and Engineering Chemistry xxx (2016) xxx–xxx

Creation of stable highly efficient catalysts and supports of catalytically active substances is topical scientific and practically important task. In industry silica and aluminum oxide and carbon materials are primarily used as supports for most of catalytically active substances. The aforesaid catalyst supports have significant drawbacks, in particular, such as low resistance to oxidation at high temperatures (carbon supports), low thermal conductivity and the ability to sintering, which leads to a decrease of the specific surface area of catalytically-active system [2–4] (supports based on oxides of silicon and aluminum). Silicon carbide among the other material is distinguished by its unique physical and chemical properties, such as high thermal conductivity, chemical, thermal and mechanical stability, low coefficient of thermal expansion, resistance to phase transitions, semiconductor nature, high electron mobility, which together determines the possibility and prospects of its various practical applications [5,6]. The aim of the current paper is to analyze the scientific approaches and technological bases of creation of new nanoscale dispersed and porous materials based on silicon carbide for adsorption, catalysis, electrochemical applications etc., determine an influence of the structure type, morphology, porosity on adsorption, catalytic, spectral, mechanical properties, find new areas of application of silicon carbide.

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Methods of obtaining of porous silicon carbide

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Among the numerous modifications (polytypes) of silicon carbide (
200) [7] cubic 3C–SiC polytype (b-SiC) is considered the most stable (up to ca. 2100  C) [8]. Primarily synthesis conditions (temperature, pressure, etc.) and the presence of impurities influence the formation of silicon carbide of the certain polytype [9]. Sublimation method (i.e., evaporation and condensation) first proposed by E.G. Acheson is used for growing of semiconductor single crystals of silicon carbide [10]. The method is based on the transport of the substance from the hot source (charge) to a seed with a lower temperature. Silicon carbide crushed powder is mainly used as a charge. Growth during the sublimation occurs at the temperatures 1800–2600  E. This method was seemed to be suitable to produce abrasives and for growing of single crystals for semiconductor electronics. However, uncontrolled form- and

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structure formation (presence of a significant number of structural defects) of SiC crystal and their contamination with impurities restrict the use of silicon carbide obtained by the described method in electronics. Lely method consists in evaporation of polycrystalline SiC at the temperature 1800–2600  E and subsequent vapor condensation on random nuclei [11]. The large number of nuclei leads to the formation of excess of the small crystals, which does not allow the growing of the large crystals. Obtaining of the bulk single crystals of silicon carbide became possible due to use of single-crystal seeds—so-called Physical Vapour Transport (PVT, LETI method) [12]. For suppression of spontaneous nucleation and formation of polycrystals condensation of supersaturated vapor on single crystals-seeds was carried out in an inert atmosphere. In order to gradually increase a rate of crystal growth an inert gas is pumped out from a cell. The methods which allow to prepare porous SiC will be considered below. For synthesis of silicon carbide different methods, including CVD-method (chemical vapor deposition), electrochemical etching, carbothermal reaction using carbon nanotubes and activated carbons, magnesiothermic reduction etc. are used. For instance, pyrolysis of carbon particles impregnated with nickel compounds in SiCl4 flow leads to the formation of silicon carbide which has the developed surface area (up to 100 m2/g) and reproduces the form of the initial carbon [13]. Pyrolysis of organosilicas allows obtaining silicon carbide with high specific surface area (over 100 m2/g) [14,15]. The obvious advantage of the mentioned method of synthesis of silicon carbide is the presence of Si C bond in the initial precursors which solves the problem of small contact in the case of use of separate sources of silicon and carbon [16]. A lot of attempts to obtain porous silicon carbide with the developed surface area were done. The proposed various approaches and methods for synthesis of porous silicon carbide are presented in the table (Table 1).

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Electrochemical etching of massive silicon carbide

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Porous SiC layers obtained by electrochemical etching of corresponding massive material attract special attention. This is

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Table 1 Methods of obtaining of porous silicon carbide. Initial materials for synthesis

Features of obtained silicon carbide

SBET (m2/g)

References

Electrochemical etching

Massive silicon carbide

Intense luminescence at the room temperature because of the appearance of defect sites during the etching process

Not determined

[17,18]

“Shape memory synthesis”

Activated carbon or coke and gaseous silicon monoxide

Replication of the macroscopic form of carbon during the synthesis; presence of a large number of stacking faults; formation of amorphous layer (thickness of ca. 3 nm) likely of silicon oxycarbide

20–200

[16]

Carbothermal reduction

Carbon and silicon monoxide or silicon dioxide

Possibility of varying of porosity and morphology (particles, fibers, rods, etc.) of silicon carbide

up to ca. 500

[19–21]

Magnesiothermic reduction

Carbon, silica, magnesium

Possibility of varying of porosity of silicon carbide

up to ca. 450

[22,23]

Nanocasting using polycarbosilanes

Silica matrices, polycarbosilanes

Mesoporous spatially ordered structure

up to 800

[24,25]

-Ethylene-bridged organosilica mesophases

-Wide pore size distribution

up to 620

[26]

-Carbon and silicon powder

-Replication of the carbon structure during the synthesis; possibility of varying of porosity and morphology of SiC

up to 215

[27,28]

-Use of silicon powders

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Methods of obtaining

Other approaches -Pyrolysis of organosilicas

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due to the presence of photoluminescence at the room temperature with an intensity which greatly exceeds the intensity of photoluminescence of the initial crystal in the same spectral range [17,18,29,30]. Thus, for porous silicon carbide obtained as a result of electrochemical anodization of 6H–SiC single crystals, there is a blue–green luminescence with 100 fold higher intensity than for the original material [30]. Obviously, the increased luminescence observed for these materials is due to features of the structure of a layer of porous SiC, namely an appearance of defect centers during the interaction of an electrolyte with the surface of silicon carbide [31]. The enhanced photoluminescence can be caused by the formation of SiC nanoparticles of cubic modification in a porous layer [32,33]. 6H–SiC layer of porous silicon carbide allows obtaining perfect epitaxial layers because the concentration of defects that could grow in an epitaxial layer disrupting its structure is reduced as a result of the electrochemical etching [34]. Investigation of peculiarities of the structure of porous silicon carbide layer obtained as a result of the electrochemical etching on 6H-SiC substrates (substrate – porous layer – epitaxial 6H-SiC layer) showed the presence of an intermediate layer between the porous space and silicon carbide that was not subjected to etching. This intermediate layer includes amorphous component and twodimensional defects. In addition, the mentioned layer contains an excessive amount of carbon compared with the stoichiometric composition of the substrate. Epitaxial layer of silicon carbide in a place of contact with the porous layer is characterized by an excess of carbon. Enrichment of porous layer of silicon carbide with carbon atoms is likely explained by an outlet of the part of the silicon atoms from the SiC structure into electrolyte, which ultimately can lead to partial or complete amorphization of the material (Fig. 1) [18].

Fig. 1. Cross section (11–20). Image with high resolution of the pore area with transition structure. The atomic rows with unclear contrast of individual atoms are indicated with the arrows [18].

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Shape memory synthesis

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The method of “shape memory synthesis” which involves an interaction of activated carbon or coke with gaseous silicon monoxide at the temperatures of 1200–1500  E was proposed (Fig. 2). Porous silicon carbide (specific surface area 20–200 m2/g) is formed as a result of reaction between SiO and carbon which macroscopic form is replicated during the synthesis [16,35–37]. This method foresees the use of inexpensive initial substances, and allows to pre-set form (and obviously, size) of the obtained silicon carbide particles since silicon carbide powders due to high mechanical strength are difficult to finish. The structures of silicon carbide formed in this way are characterized by a large number of stacking faults [38] along the growth axis (111) of b-SiC phase (Fig. 3). These defects may be due to the presence of a-SiC micro domains. At the same time the presence of stacking faults likely provides the formation of SiC with the developed surface due to partial disorder of the formed material. According to the researches of the obtained materials by TEM part of the samples surface is covered with an amorphous layer (thickness of ca. 3 nm) likely of silicon oxycarbide [16].

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Use of silicon as the initial substance

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Use of silicon powders as active initial reagents seems to be an alternative approach for obtaining of dispersed/porous nanostructured silicon carbide. It is expected that this process will take place at a temperature 1300  E, which is below the melting point of silicon (1420  E) resulting in the formation of nanocrystalline SiC. Nanocrystalline silicon carbide (b-modification) with high specific surface area (up to 147 m2/g) and mesoporosity (pore diameter 5–40 nm) were formed by heating of spatially ordered mesoporous carbons (carbon replicas of MCM-48, SBA-15, KIT6 silica matrices) with silicon powder at 1200–1300  E [27]. The used synthesis method can be considered a low-temperature since the reaction occurs at the temperature below the melting point of silicon (1420  E). The process is an interaction of mesoporous carbon material with gaseous silicon formed during sublimation of the powder. The obtained silicon carbide samples reproduce the morphology of the used mesoporous carbon but lose spatial ordering in mesoscale range. The authors note that the described approach can be applied to other types of carbons (films, microspheres, etc.) that will allow obtaining silicon carbide with a morphology which corresponds to such one of the initial material. Corespondence of morphology of silicon carbide and carbon obviously testifies that the carbon particles act as templates during the interaction of carbon with silicon. Impregnation of pyrolized wood with silicon at the temperatures above the melting point of Si results in obtaining of b-SiC characterized by multimodal pore size distribution [39]. Microstructure of synthesized silicon carbide corresponds to microstructure of the initial organic material. Heating of the carbon nanotubes with silicon powder at 1200  E for 100 h (Fig. 4) leads to the formation of silicon carbide nanotubes [40]. Nanotubes E–SiC which are the carbon nanotubes coated with a layer of silicon carbide are formed together with the SiC phase. An increase the SiC/E–SiC nanotubes ratio as a result of heat treatment of the obtained material in air at 600  E due to burning of unreacted carbon is observed. Heating of multiwall carbon nanotubes and silicon powders in a mixture of salts of sodium chloride and sodium fluoride at temperatures of 1100–1200  E in an inert atmosphere leads to an obtaining of silicon carbide nanorods [41]. Formed SiC nanostructures completely reproduce the morphology of the used carbon nanotubes, which, according to the authors, indicates that the carbon nanotubes during the synthesis process were not only

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Fig. 2. Laboratory scale two-stage reactor setup for the synthesis of silicon carbide according to the shape memory synthesis [16]. 192 193 194 195 196 197 198 199 200 201 202 203

the carbon source and acted as templates for the growth of nanorods too. Most of the obtained silicon carbide nanorods are characterized by a complex sequence of packages containing different forms of defects, and only some part of the formed nanostructures is a regular sequence of packages that do not contain defects. Naderi et al. have introduced simple method to produce porous SiC by thermal carbonization of porous silicon under an acetylene flow [28]. A small PL blue shift was observed after acetylene exposure, which can testifies the changing bandgap of porous silicon due to the formation of the thermally carbonized porous silicon. The obtained sample showed a relatively stable optical

Fig. 3. HRTEM micrograph of SiC obtained via “shape memory synthesis” [16].

nature under prolonged exposure to laser illumination because of the replacement of the surface metastable H terminations with the stable Si–C bonds. The prepared material showed stable electrical characteristics under prolonged green laser radiation (532 nm, 5 mW) [28]. Thin SiC layers were successfully deposited on a porous silicon (PS) substrate via radio frequency magnetron sputtering after annealing [42]. PS acted as a template for the growth of SiC with the same morphology. The highest annealing temperature (1200  C) resulted in improved uniformity of the sputtered porous-shaped SiC sample as well as in enhanced optical characteristics.

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Carbothermal reduction

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Today there is considerable interest in porous silicon carbide which can be used as a catalyst supports. The corresponding silicon carbide in addition to properties of the bulk material should

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Fig. 4. Scheme of the experimental apparatus for synthesis of SiC nanotubes [40].

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Fig. 5. Scheme of carbothermal reduction for synthesis of porous SiC. 220 221 222 223 224 225 226 227 228 229 230 231 232 233 234 235 236 237 238 239 240 241 242 243 244 245 246 247 248 249 250 251 252 253 254 255 256 257 258 259 260 261 262 263 264 265 266 267 268

possess the developed porous structure and, in conditions of the matrix synthesis—spatial ordering in the nanometer range too. Carbothermal reduction of silicon oxides seems to be one of the most effective and controlled methods of synthesis of silicon carbide [19,43]. Silicon dioxide SiO2 and silicon monoxide SiO are used as the silicon source in the carbothermal reactions. This raises an idea of a matrix or exotemplate synthesis of silicon carbide using silica MMS as the initial precursor of silicon oxide and carbonized organic substance in the pores of the silica matrix as in a nanoreactor, i.e., carbon–silica composites used for the matrix synthesis of mesoporous carbons as a carbon component (Fig. 5). The formation of porous nanostructured silicon carbide according to the type of the initial silica matrix can be expected as a result of this synthesis. The main problem in the synthesis of nanoporous silicon carbide consists in a difficulty of SiC crystal growth control and formation of porous silicon carbide structure in the conditions of high temperatures. In particular, infiltration of vapors of organic substances into the pores of mesoporous silica materials is used for the synthesis of porous SiC. Thus, silicon carbide with the specific surface area of 120 m2/g was obtained as a result of infiltration of propylene into MCM-48, pyrolysis and subsequent carbothermal reduction of the carbon-silica composite (1250–1450  E) [44]. One of the ways to obtaining porous silicon carbide involves the use of sol–gel process followed by carbothermal reduction of the as-synthesized SiO2/C composite at a temperature 1250  E [45]. Polymer of phenol and formaldehyde as well as tetraethylorthosilicate were used for the preparation of binary carbon–silica gel (and xerogel after drying, respectively). Adding of nickel nitrate to these gels leads to the formation of silicon carbide with the higher porosity characteristics compared with the implementation of the carbothermal process without Ni(NO3)2 (SBET 112 vs. 47 m2/g, Vpore 0.31 vs. 0.13 cm3/g, Dpore 10 vs. 45 nm). Taking into account the change of the textural characteristics of silicon carbide in the case of synthesis in the presence of nickel nitrate, the authors consider that nickel nitrate performs a role of the pore-adjusting reagent. However, this conclusion does not seem to be quite correct, since a change in the characteristics of the porous structure is the result of changes in particle size of silicon carbide formed during the reaction. The authors showed that in the presence of nickel nitrate in the initial reaction mixture silicon carbide with smaller particles than in the absence of Ni(NO3)2 (50 vs. 1000 nm) is formed. Nickel nitrate showing catalytic action can change the course of the reaction (due to the formation of active components nickel carbide or nickel silicide, as noted by the authors) than promotes to the formation of smaller SiC crystals, and as a result— the formation of silicon carbide with the higher textural characteristics.

Later it was shown that a variation of Ni/Si molar ratio in the initial xerogels allows to adjust the characteristics of the porous structure of silicon carbide (SBET from 5 to 204 m2/g, Vpore from 0.01 to 0.34 cm3/g, Dpore from 3.5 to >100 nm) [46]. The authors rightly note that their approach consists in an aggregation of the primary colloidal particles of different size which is achieved by introducing of different amounts of nickel nitrate. Silicon carbide with a morphology of nanorods or nanowires causes considerable interest due to the fact that their elasticity and strength are much higher than those ones in the bulk SiC and SiC whiskers [47], which is important when using of silicon carbide in the strengthen composite materials [48]. Silicon carbide whiskers are characterized by high length to diameter ratio (100–200 and more); crystal diameter can be varied in considerable ranges (40–500 nm). In addition to traditional use as components of ceramics and construction materials SiC whisker are of interest for the development of the new components of hightemperature electronic devices. The advantages of using of silicon carbide for these purposes are its high thermal and corrosion stability combined with a high value of the band gap (2.4–3.3 eV, depending on SiC polytype) [49]. Heating of aligned carbon nanotubes – separate, isolated, located at a distance of ca. 100 nm from each other perpendicular to the substrate surface – with silicon monoxide at a temperature of 1400  E for 2 h allowed to obtain oriented silicon carbide nanowires [48]. Orientation, diameter (10–40 nm) and length (up to 2 mm) of the formed SiC nanostructures were completely corresponded to the similar parameters of the initial carbon nanotubes, indicating their templating role in the abovementioned reaction. Testing of the emission properties of the obtained silicon carbide nanostructures (field emission current density of ca. 10 mA/ cm2 at the applied fields 0.7–1.5 V/mm and 10 mA/cm2—at 2.5– 3.5 V/mm) showed the possibility of an application of oriented SiC nanowires for vacuum microelectronic devices [48]. The main factors that affect the kinetics of carbothermal reduction and nanostructure type of the obtained silicon carbide are porosity, E/SiO2 ratio, and the structure of the initial carbon– silica composites [50]. Mesoporous SiC was obtained as a result of pyrolysis of the dense carbon–silica composites with high E/SiO2 ratio (4.21). The proportion of nanoparticles or nanofibers in the mixed silicon carbide nanocomposites can be varied depending on the E/SiO2 ratio, and the use of infiltration with carbon. Thus, nanoparticles SiC predominate (over 70%) at the additional introduction of an organic precursor and E/SiO2 ratio 1.9, preferential formation of silicon carbide in the form of nanofibers (over 85%) occurs at E/SiO2 ratio 2.51 [50]. Intermediate SiE/;E;-48 and SiE/SBA-15 nanocomposites were obtained using chemical vapor infiltration (CVI) of dimethyldichlorosilane from the hydrogen flow as a carrier gas into

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silica mesoporous molecular sieves MCM-48 or SBA-15 and their subsequent decomposition at 750–900  E [20]. At a lower pyrolysis temperature an infiltration occurs mainly in the pores results in the formation of small crystallites that are not detected by XRD. At higher temperatures the formation of silicon carbide takes place mainly on the external particle surface of the silica matrices, resulting in the obtaining of hedgehog-like particles core-shell type, in which spatially ordered silica MCM-48 is the core and a protective coating of silicon carbide is the shell. Taking into account a decrease of the mesopore volume (from 0.46 cm3/g for the initial matrix to 0.03 cm3/g for the composite after the treatment for 5.5 h) and mesopore size (from 4.5 nm to 2.7 nm) during the CVI process for SBA-15 of hexagonal structure, formation of the SiC phase occurs in the pores of the matrix resulting in the generation of ultra-thin coating. The authors rightly note an increase of thermal stability of the initial matrices at application of infiltration process, which is probably explained by micropore filling in the early stages of the process [20]. Thin coating of silicon oxycarbide formed in the early stages of infiltration acts as an interface for further deposition of pure silicon carbide. Removal of the silica matrices from the synthesized nanocomposites leads to obtaining of X-ray amorphous low ordered mesoporous SiC-replicas with pore volume of 1 cm3/g, pore diameter 5.0–10.0 nm and specific surface area ca. 500 m2/g [20]. Comparative study of the thermal stability of silicon carbide, mesoporous silica SBA-15 and spatially ordered carbon E;K-1 within the limits of the textural parameters of these materials showed the highest resistance of the porous structure of E;K-1 carbon (after holding at 1573 K for 24 h specific surface area and mesopore volume decrease insignificantly—from 1760 m2/g to 1530 m2/g and from 1.05 cm3/g to 0.75 cm3/g, respectively) [51]. Thermal stability of silicon carbide is significantly higher than that one of mesoporous silica SBA-15. Carbothermal reduction of carbon–silica composites based on SBA-15 and sucrose results in obtaining of silicon carbide characterized by the developed surface area (120–190 m2/g) and morphology of whiskers or nanotubes [52]. Smaller duration of carbothermal process (up to 14 h) at 1250–1300  E leads to the formation of whisker with a diameter of 50–90 nm and a length of more than 20 mm. With an increase in the reaction time up to 20 h nanotubes with a diameter of 60–100 nm and a length of more than 10 mm are formed. Mesoporous silicon carbide (Dpore 2–30 nm, SBET 140 m2/g) with thorn-ball morphology was synthesized via carbothermal reduction of the carbon-silica xerogels (obtained from the reaction mixtures based on sucrose and TEOS) [53]. Carbothermal reduction of the composites gels based on resorcinol-formaldehyde and silica leads to the obtaining of monolithic mesoporous a-SiC aerogels with the developed surface area (250 m2/g) and high pore volume (
1 cm3/g) [21]. According to research results of nitrogen ad(de)sorption the limits of pore size distribution (1–27 nm) allow to attribute the synthesized materials to nanoporous ones. However, the discrepancy of porosity (90.8%) and bulk density (
0.29 g/cm3), and the presence of macropores in TEM images of the obtained samples indicates mainly the macroporous nature of the synthesized silicon carbide. Heat treatment of mesoporous carbon–silica nanocomposites (obtained from TEOS and furfuryl alcohol) at 1400  C in an inert medium results in the formation of nanostructured porous silicon carbide with a morphology of hollow spheres [54]. According to the proposed mechanism at temperatures above 800  C there is a separation of the larger part of the carbon phase from the silica matrix with the formation of the carbon spheres. At a temperature of ca. 1350  C an interaction of residual carbon in the silica matrix with silica with the formation of silicon monoxide begins. As a

result of diffusion and interaction of SiO with the carbon spheres silicon carbide shell is formed. After removal of the carbon core by calcining of the obtained material in air the hollow silicon carbide spheres are obtained. The sphere size and the thickness of the SiC shell can be varied depending on the E/SiO2 ratio and conditions of heat treatment, respectively [54]. Heat treatment of the carbon nanotubes coated with silica leads to the formation of silicon carbide nanofibers [55]. It seems that the formation of SiC nanofiber takes place on the outer layers of the carbon nanotubes leading to their coaxiality. Perspectivity of the described method for producing of silicon carbide nanofibers the authors explain by the ability to control the quantity of silica coating and conditions of the heat treatment. b-SiC in the form of the particles of submicrosized range is a result of carbothermal reduction of silica gel (Cab-O-Sil) doped with carbon particles (carbon-black) [56]. The size of the primary SiC crystallites corresponds to the size of the used carbon particles. Formation of polycrystalline aggregates (of ca. 1000 nm) is due to the surface diffusion, while the bulk diffusion occurs at higher temperatures of synthesis (1500  C). Adding of boron into the reaction mixture leads to the growth inhibition of the silicon carbide agglomerates due to the surface diffusion limitation. The interaction of so-called biocarbon obtained by pyrolysis of oak wood, with gaseous SiO at a temperatures of 1550–1600  E leads to the formation of porous b-SiC ceramic with the cellular structure which reproduces the morphology of the initial wood [57]. The synthesized silicon carbide samples contain anisotropic open pore diameter up to 1 mm, moreover the porous structure of the material can be adjusted depending on the wall thickness and cell diameter of the initial wood tissue. Carbothermal reduction using carbon–silica composites based on various types of silica MMS (SBA-15, KIT-6, MCF, SBA-3) allowed to obtain silicon carbide with the developed surface area (up to 410 m2/g) and high pore volume (up to 1.0 cm3/g) [58]. Use KIT6 MMS with 3-dimentional intercross mesopore system as a matrix, E/SiO2 ratio close to the stoichiometric one and an increased level of pore filling of silica MMS with carbon contribute to the formation of silicon carbide with high porosity parameters. The reaction of carbothermal reduction between silica and carbon involves several stages [50,59,60]:

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SiO2(s) + C(s) ! SiO(g) + CO(g)

(1)

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SiO2(s) + CO(g) ! SiO(g) + CO2(g)

(2)

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SiO(g) + C(s) ! SiC(s) + CO(g)

(3)

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SiO(g) + 3CO(g) ! SiC(s) + 2CO2(g)

(4)

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CO2(g) + C(s) ! 2CO(g)

(5)

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The overall reaction: (6)

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Silicon carbide can be formed by interaction of carbon (stage 3) or carbon monoxide (Eq. (4)) with gaseous silicon monoxide SiO, which in turn is formed by the reaction between silica and carbon (stage 1). Equilibrium in each of the above reactions is determined by temperature and partial pressures of silicon monoxide and carbon monoxide [50]. Thus, at the lower E/SiO2 molar ratios than stoichiometric one (E/SiO2 = 3 according to the overall reaction), a significant decrease in the rate of carbon monoxide formation by

431

SiO2(s) + 3C(s) ! SiC(s) + 2CO(g)

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Reactions (1) and (2) and, accordingly, difficulty of formation of crystalline silicon carbide phase [50] (or formation of SiC particles of too small size insufficient to detect by XRD) should be expected. In Ref. [58] despite the fact that for the synthesis of silicon carbide E/SiO2 ratios were lower than stoichiometric one (from 1.4 to 2.8) formation of a highly crystalline silicon carbide phase was observed for all used silica MMS. In Ref. [50] the authors showed that an additional impregnation of carbon–silica nanocomposites with the low E/SiO2 ratio (1.90 and 2.51) with the organic substance (polyfurfuryl alcohol) followed by carbonization leads to an additional formation of silicon carbide phase, while E/SiO2 ratio increases insignificantly (2.13 and 2.55, respectively). The authors explain this experimental fact by a significant increase in the local concentrations of SiO and CO due to an interaction between the walls of the carbon-silica composite and additionally infiltrated carbon [50]. All initial carbon–silica composites in Ref. [58] were obtained by double impregnation of silica MMS with sucrose. Therefore, it has been assumed that the possibility of silicon carbide formation during the carbothermal reduction depends not only on the E/SiO2 ratio but the level of the pore filling of silica MMS with carbon. Obviously sorption concentration of substance in the pores contributes to the last fact. It was shown that morphology (fibers presence) and consequently porosity characteristics of SiC are largely defined by porous structure of the carbon component in the initial carbon–silica composites, as well as the number of contact zones between silica and carbon phases [61]. In the case of mesoporous silica a contact area of silicon oxide and carbon is determined by the mesopore specific surface area. Using SEM and nitrogen physisorption an inverse relationship between an amount of silicon carbide fibers and the mesopore specific surface area of carbon materials derived from carbon–silica composites was demonstrated. An influence of synthesis conditions in particular the porosity of the initial substances etc. on the morphology and porosity of the obtained silicon carbide is shown in Fig. 6. Found dependence between SiC structure and mesopore specific surface area of the carbon component in the carbon-silica composite testifies a templating role of carbon in carbothermal reduction.

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Magnesiothermic reduction of carbon–silica composites

478

Monolithic mesoporous (SBET 232 m2/g, Vpore
0.5 cm3/g, Dpore 9.1 nm) silicon carbide was obtained via low temperature conversion (by the addition of magnesium) of the carbon–silica composites previously synthesized from the gels of the composites based on resorcinol-formaldehyde resins and silica [62]. The obtained nanocrystalline samples are b-SiC, have a lower band gap (3.2 eV) than bulk silicon carbide (5.3 eV) and exhibit photoluminescence at room temperature. Mesoporous silicon carbide was synthesized via so-called topotactic thermal reduction of the carbon–silica composites by magnesium at a relatively low temperature (
800  E) [63]. In contrast to previous considerations about the action of the silica matrices as templates the authors note that silicon carbide formed during the reaction reflects the structure of the carbon component. The porosity of the carbon influences on the crystal structure of silicon carbide too. Thus, the use of macroporogens leads to the formation of 3C–SiC cubic structure (silica source—hexagonal three-dimensional packing of Stöber silica spheres), and mesoporogens allow to obtain hexagonal 2H–SiC structure (carbon– silica composite was obtained on the basis of mesoporous MMS SBA-15). According to the authors the synthesis process involves reduction of silicon oxide with magnesium to silicon which atoms are able to diffuse into the carbon lattice (between the carbon layers). Arising Si C bonds destroy the C C bonds in C6 p system, Si atoms replace C resulting in the formation of cubic SiC with the diamond structure. Formation of the high temperature thermodynamically stable 2H–SiC phase the authors explain by the decrease in the rate of the particles growth of silicon carbide as a result of participating in the reaction of magnesium from the gas phase instead of the liquid one, as in the previous case, due to the limited pore size of the used mesostructure (radius of 3.1 nm). In the case of diffusion of magnesium in the liquid state into the macroporous Si?2-Stöber/E structure low-temperature 3C–SiC modification is formed [63]. Magnesiothermic reduction of the composites based on mesoporous silica (SBA-15 and KIT-6) and carbon at a relatively low temperature (650  E) leads to the formation of mesoporous

479

Fig. 6. An influence of synthesis conditions on the morphology and porosity of silicon carbide obtained via carbothernal reduction.

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b-SiC which is characterized by the developed surface area (ca. 2

300 m /g) [22]. The authors point out that magnesium is involved in the synthesis as a reducing agent and catalyst, and to a large extent determines the structure and properties of the final material. According to TEM data mesopore spatial ordering of the synthesized SiC samples is significantly lower than for the corresponding silica matrices, which is obviously due to the fact that silica in the synthesis of silicon carbide plays both the role of template and the role of reagent resulting in the collapse of the part of the silica mesostructure. Based on the proposed reaction mechanism magnesium at first reduces silicon dioxide to silicon, which further reacts with carbon to form silicon carbide (Fig. 7). It was shown that pure silicon obtained under the same conditions (reduction of SBA-15) in contrast to silicon carbide does not retain the spatial ordering of mesostructure of the initial silica MMS. The above mentioned indicates the important role of the carbon framework in maintaining of silica template mesostructure during the reaction [22]. Heat treatment of the nanocomposites based on MCM-48 and polyacrylamide in the presence of magnesium in the temperature range 550–600  E leads to the obtaining of nanocrystalline mesoporous (pore diameter of 2–10 nm) silicon carbide with the high specific surface area (330 m2/g) [23].

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Nanocasting using polycarbosilanes

540

Impregnation of silica MMS SBA-15 with a melt of lowmolecular polycarbosilanes followed by heating in an inert atmosphere at 1300  E for 2 h allowed to obtain spatially ordered mesoporous silicon carbide with the high specific surface area (650–800 m2/g) [24]. The proposed method of nanocasting using polycarbosilanes seems to be quite promising considering that these precursors already have Si–C bond in their composition,

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which obviously contributes to the formation of the silicon carbide phase during the pyrolysis process. Silicon carbide based ceramics characterized by spatial ordering and mesoporosity was obtained by matrix method using polycarbosilanes as precursors and silica MMS as solid templates [64]. Silicon carbide with three-dimensional cubic bicontinuous structure is characterized by the higher thermal stability (up to 1400  E in the nitrogen atmosphere) and the higher specific surface area (590 m2/g) and pore volume (0.7 cm3/g) compared with the two-dimensional hexagonal nanowires. Mesoporous SiC monoliths were synthesized via nanocasting and subsequent pyrolysis (in the nitrogen atmosphere at 1000  E and 1200  E) using polycarbosilane as an initial preceramic polymer and SBA-15 as a template [25]. The obtained materials are the spatially ordered two-dimensional structures of hexagonal p6mm symmetry, characterized by high values of specific surface area (560–630 m2/g) and resistance to oxidation. An increase of the pyrolysis temperature from 1000  C to 1200  C leads to the expected decrease in textural characteristics (total porosity decreases from 58% to
53.6%), and to an increase of the compression strength (from 21.4 to 33.5 MPa) which obviously due to compaction of the framework material. Foaming of the mixture of a polycarbosilane preceramic polymer with a blowing agent (azodicarbonamide) at 250–260  C under nitrogen, curing under air at 200  C followed by pyrolysis at 1000  C result in the formation of macro-cellular porous silicon carbide foams [65]. Variation of the content of blowing agent and foaming temperature allows to regulate porosity (59–85 vol%) and the cell size (416–1455 mm) of the resulting materials. Infiltration of a cellulose fibre preform with poly(methylcarbosilane) with subsequent pyrolysis at 1000  C leads to the obtaining of the amorphous SiC reproducing the structure and porosity of the cellulose fibre template [66].

Fig. 7. Schematic illustration for the synthesis of silicon carbide via magnesiothermic reduction [22].

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604

Mesoporous silicon carbide was prepared via nanocasting using polycarbosilane and uniformly sized butoxylated SiO2 nanoparticles (obtained in o-xylene from Ludox HS-30 sol) [67]. The synthesized materials possess high surface area (up to 800 m2/g), uniformly sized (11 nm) spherical pores, and large pore volume (up to 1.25 cm3/g). It was shown that the textural properties can be controlled by the polycarbosilane:SiO2 ratio in the initial composite. Porous silicon carbide possessing a granular structure with a macroporosity was prepared via soft templating approach [68]. This method involves a templating of the molecular precursor, 1,3,5-trisilacyclohexane (TSCH), by a solid network of semifluorinated alkanes (SFA). The transformation of the generated gel phase into a polysilane was performed by the polymerization of TSCH molecules around the SFA network. Then the SFA were removed from the polysilane, and the obtained material was calcined at 1000  C under argon atmosphere resulting in the SiC formation. Highly ordered SiC nanorods with high specific surface areas (240–760 m2/g) were obtained via a nanocasting method [69]. Liquid allylhydropolycarbosilane or poly-1,3,5-trisilacyclohexane (pTSCH) casted into SBA-15 (mesoporous silica template) were used as the initial pre-ceramic polymers. Silica templates were removed after the thermal conversion resulting in a formation of the SiC inverse replicas of the initial template (Fig. 8).

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Other methods of synthesis of silicon carbide

606

Nanostructured highly crystalline silicon carbide which is a virtually pure b-modification and has the developed surface area (380–620 m2/g) and high pore volume (0.35–0.9 cm3/g) with a wide pore size distribution was obtained by pyrolysis of ethylenebridged organosilica mesophases at 1300–1350  E [26]. Porous silicon carbide was prepared by cold isostatic pressing of the nanosized SiC powder followed by sintering at 1500–1800  E [70]. Raising the sintering temperature leads to an increase in the size of pores and particles, and necks formation is observed due to mass transfer of the nanosized particles from the surface. Ultra highly porous (about 86%) SiC was obtained by the method of consecutive gelation–freezing of the reaction mixtures based on gelatin, water and silicon carbide powders and their subsequent defrosting, drying and sintering at 1800  E [71]. The microstructure of the synthesized material is a unidirectional cylindrical micrometer range cells (pores), the formation of which is caused by the formation of the ice crystals during freezing. The possibility of control the cell size (within 34–147 mm) by varying the freezing temperature was shown [71]. Use of porous glasses as template in a nanocasting approach leads to the formation of nanoporous silicon carbide [72]. Replication of the nanoscopic structure of porous glasses by SiC was demonstrated. The synthesized samples are characterized by the specific surface areas of up to 477 m2/g, total pore volumes of 1.1 cm3/g in nanoscale range (10–50 nm). Conserving the particle shape of the used porous glass beads with several hundred microns in diameter by the adjustment of the infiltration strategy was

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9

shown. The authors consider the obtained nanoporous SiC samples as promising materials for application as filter, membrane or catalyst supports.

633

Application of porous silicon carbide

636

Use of silicon carbide in catalysis

637

Detailed characterization and study of the silicon carbide stability (SBET 30–80 m2/g) as a support of catalytically active compounds showed high thermal stability of SiC in non-oxidative environments (up to 1000  E in a nitrogen atmosphere) [73]. The presence of water vapor or oxygen during the heat treatment of silicon carbide at 1000  E leads to its partial oxidation to silicon dioxide. Taking into account the growth rate of this process with an increase of the specific surface area of silicon carbide the authors conclude the inability to use SiC with a developed surface area as a catalyst support in the processes which take place in oxidative environments. Catalysts on silicon carbide supports are suitable for use in the high-temperature gas-phase reactions occurring in the absence of oxygen or water vapor. An exceptional stability of SiC in aqueous solutions of hydrofluoric and nitric acids was demonstrated, which opens prospects of silicon carbide using in the liquid phase reactions occurring in highly acidic media [73]. SiC with deposited transition metals or metal oxides show high catalytic activity in various high-temperature and highly exothermic reactions. In particular, nickel sulphide supported on silicon carbide (surface area of 20–80 m2/g) shows a high catalytic activity and selectivity in the reaction of direct oxidation of hydrogen sulfide into elemental sulfur in temperature ranges of 20–40  E and 100–120  E [74]. Iron oxide on the silicon carbide support demonstrates high catalytic activity and selectivity at higher temperatures (210–240  E). The advantages of the silicon carbide use as a support in this process at the indicated temperature range are its high stability (SiC is not sulfated in contrast to the oxide supports) as well as insensitivity to water vapor and sulfur compounds. Silicon carbide nanotubes with deposited nickel sulfide particles showed high catalytic activity in the reaction of low temperature (60  E) selective oxidation of hydrogen sulfide into elemental sulfur (100% conversion and 100% selectivity) [75]. The absence of reaction by-products (in particular SO2) is explained by the process implementation at a low temperature and the absence of micropores in the silicon carbide structure (nanotubes specific surface area is 40 m2/g). In addition to high catalytic activity the synthesized materials are characterized by high sorption capacity toward solid sulfur, due to an increase in the free volume of nanotubular silicon carbide compared with conventional catalysts in the form of grains. The generated sulfur is removed from the pores of the catalytic composition mechanically under water film (condensed water on the catalyst surface) and accumulates on the hydrophobic part of the support where the water film is destroyed [16]. Thus, there is no blocking the active sites of the catalyst with the reaction products (such as sulfur). However, other traditional catalysts of this process using supports such as silica, alumina, and

638

Fig. 8. Scheme of the SiC synthesis via nanocasting using SBA-15 [69].

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activated carbon, compared with silicon carbide suffer from rapid deactivation (a function of sulfur deposition) until the complete blocking of active centers. Detected high catalytic activity of the obtained materials the authors explain by the inner partial pressure concept as well as a defectiveness of the silicon carbide surface. The essence of the inner partial pressure concept consists in a significant growth of hydrogen sulfide partial pressure inside the silicon carbide nanotubes, apparently due to the microcapillarity phenomenon. In addition, the external surface of the silicon carbide nanotubes is characterized by a high density of defects (silica, silicon oxycarbide). Hydrophilic nature of the nanotube surface will also enhance the microcapillarity phenomenon [75]. Preparation of molybdenum oxycarbide supported on silicon carbide (SBET 19 m2/g) leads to an increase (in order) of its catalytic activity in the reaction of isomerization of n-hexane and n-heptane compared with the use of g-Al2O3 (SBET 180 m2/g) as a support [76]. Decrease of catalytic activity when using aluminum oxide as the support is explained by the strong interaction between the catalyst and the support. Mono- and dibranched molecules are primarily the isomerization products, while the formation of cyclic products does not occur. An influence of water vapor does not lead to the catalyst deactivation, obviously due to an inertness of the SiC support. Higher catalytic activity of molybdenum oxycarbide supported on silicon carbide compared with aluminum oxide is caused by two factors. First, due to the high thermal conductivity of silicon carbide the heat release during the reaction does not lead to sintering of the support and the active phase. Second, the chemical inertness of SiC inhibits its interaction with the active phase and allows easily separate it from the composite [76]. Use of pure silicon carbide and silicon carbide doped with cerium as the supports of platinum–rhodium allows to increase the catalytic activity of such systems in the process of neutralization of vehicle exhaust (a synthetic mixture containing carbon monoxide, nitric oxide, hydrocarbons and nitrogen as an example) [77]. Doping of silicon carbide with cerium provides good dispersion of the noble metals particles and increases their resistance to sintering, which together leads to an increase of reactivity of the catalytic system in the reaction of oxidation of carbon monoxide and nitrogen oxide compared with the industrial catalysts. Easy separation of the active phase of the catalyst and the support by washing with acid is possible due to the chemical inertness of the SiC support. The use of b-SiC with relatively developed surface (over 20 m2/ g) prepared by the “shape memory synthesis” as a support of vanadyl pyrophosphate (VPO) catalyst in the reaction of butane direct oxidation into maleic anhydride allows to increase the yield of the target product (from 24 to 54%) due to the temperature control of the catalyst surface [78]. Stably high selectivity toward maleic anhydride (74–78%) enables the use of high partial pressures of butane. VPO supported on silicon carbide is characterized by higher yield and selectivity toward maleic anhydride compared with the bulk analogue. The achievement of high selectivity toward the target product is due to the absence of micropores in the support and, more importantly, high thermal conductivity of the support, that allows avoiding the local overheating of the catalytic centers and protects the reaction product from further oxidation into CO and CO2. Porous SiC ceramics was obtained via sintering of the silicon carbide powder and carbon pellets at 1450  E in air [79]. The carbon particles inside silicon carbide can act as the matrices during formation of the porous structure. Porous silicon carbide grains are linked together by silica and silicon oxycarbide generated during calcination. In situ growth of ZSM-5 zeolite in the pores of SiC leads to the formation of the composite, which after doping with molybdenum is active in the methane

dehydroaromatization reaction and characterized by higher selectivity toward the desired products (benzene, toluene, and xylene) than separately taken zeolite. Combining core–shell nanoparticles synthesis with the nanocasting approach allowed preparing porous silicon carbide containing encapsulated and catalytically active CeO2 nanoparticles [80]. This structure preventes the catalyst nanoparticles from sintering even at pyrolysis temperatures of 1300  C. The obtained matarials are characterized by high catalytic activity in the methane oxidation with onset temperatures of the reaction 270 K below the onset of the homogeneous reaction. The proposed synthesis scheme using core-shell particles is an attractive approach for design of the active sintering-resistant nanoparticles supported on silicon carbide for different catalytic applications. Ni supported on nanoporous silicon carbide as well as on controlled oxidized SiC demonstrates high catalytic activity in the carbon dioxide reforming of methane [81]. The oxidized SiC is characterized by an increase of the catalytic performance compared with the initial silicon carbide due to the SiO2 layer on the oxidized sample preventing the formation of nickel silicide at temperatures up to 850  C. The prepared catalysts showed a stable conversion level over the whole time on stream of 8 h. Some interaction of the palladium nanoparticles with the silicon carbide support, which is manifested in a 1-eV higher energy of the Pd3d5/2 level compared with the bulk palladium is noted [82]. Such model Pd/SiC catalysts in terms of the surface palladium atoms are characterized by higher activity in the 1,3butadiene hydrogenation reaction compared with pure Pd. A high photocatalytic activity of b-SiC nanowires coated with a layer of amorphous SiO2, in the photocatalytic decomposition of acetic aldehyde in the gas phase (into carbon dioxide) was revealed [83]. Silicon carbide nanowires with a diameter 8–20 nm and length up to 10 mm were obtained as a result of thermal treatment (high-frequency induction heating) of the silicon monoxide powders and activated carbon fibers. The bandgap of the synthesized nanostructures is 2.5 eV which indicates a slight hypsochromic shift compared with the bulk silicon carbide. The authors showed that as-synthesized silicon carbide coated with a layer of amorphous silica exhibits higher photocatalytic activity in the studied reaction than silicon carbide treated with hydrofluoric acid (in order to remove silicon oxide). Found fact the authors explain by the increased acetaldehyde adsorption on the structures coated with amorphous silica or a high probability of capture of the excited electrons in the conductive band of SiC coated with SiO2, and holes of the valence band of silicon carbide [83]. Mesoporous silicon carbide nanofibers with in situ embedded graphitic carbon demonstrates high activity in co-catalyst-free photocatalytic hydrogen evolution [84]. The hydrogen evolution production of the obtained photocatalyst is significantly increased under both simulated solar light and visible light irradiation in high-pH solution (180.2 mmol/g h and 31.0 mmol/g h, respectively). According to the authors the embedded carbon can swiftly transfer the photogenerated electrons and improve light absorption. Use of high-pH solution allows accelerating the holes trapping by the additional hydroxyl anions. Furthermore successful application of silicon carbide as a porous support in other catalytic reactions such as Friedel–Crafts benzoylation and Fischer–Tropsch synthesis, where traditional catalysts have shown their weaknesses, was described [1].

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Hydrogen adsorption on porous silicon carbide

811

Considerable interest to researchers is caused by the features of hydrogen adsorption on the silicon carbide based materials [85– 90].

812

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For example, silicon carbide nanotubes obtained by the interaction of multiwall carbon nanotubes with silicon at 1573 K, are able to adsorb 0.2 wt.% of hydrogen at 5.1 MPa and 298 K [86], which is almost two fold higher than the adsorption capacity of multiwall carbon nanotubes. It should be noted that the silicon carbide nanotubes compared with the carbon ones are characterized by a higher density (2.9 vs. 2.0 g/cm3), less developed surface (60 vs. 200 m2/g), and have larger external and internal diameters due to an interaction of the external carbon layer with silicon and removal of unreacted internal carbon layer after reaction. At a pressure less than 1.7 MPa silicon carbide does not absorb hydrogen but the quantity of the absorbed hydrogen at higher pressures grows faster than for the carbon nanotubes, exceeding the value for them already at 3 MPa. Considering generally less suitable parameters of the silicon carbide structure than the carbon one for hydrogen adsorption, the authors suggest differences in the mechanisms of hydrogen adsorption on such materials [86]. Based on calculations performed at the density functional level of theory (DFT) the binding energy of hydrogen with the silicon carbide nanotubes is 20% higher compared with pure carbon nanotubes [85]. The reason for this change the authors see in the partially heteropolar binding nature of the SiC bonds. Point charges contained on the walls of the silicon carbide nanotubes can induce dipoles on the hydrogen molecule, resulting in more efficient hydrogen binding [85]. The prospects of use of systems based on silicon carbide are shown by the calculations (according to DFT) of an interaction of the hydrogen molecules with lithium-doped silicon carbide nanotubes [87]. The binding energy of the hydrogen molecule with SiC nanotubes increases significantly as a result of their doping with lithium (from 0.086 to 0.211 eV), which can be explained by the transfer of a charge from lithium on the nanotube. According to the theoretical calculations SiC nanotubes doped with lithium can attach up to four hydrogen molecules (per one lithium atom), and the average binding energy is 0.165 eV. The obtained results the authors explain by the fact that Li atom partially transfers its valence electron to SiC nanotubes, which increases the polarization of the Si C bonds and increases the interaction between hydrogen molecules and lithium-doped silicon carbide surface [87]. According to quantum mechanical calculations presented in Ref. [88] the single-walled silicon carbide nanotubes are characterized by higher adsorption capacity toward hydrogen (2.19 wt.%) than single-walled silicon (1.88 wt.%) and carbon (1.11 wt.%) nanotubes (77 K, 3 MPa). Doping of the silicon carbide nanotubes with potassium leads to a significant increase in their sorption capacity toward hydrogen (ca. 0.37 wt.%, 100 bar, room temperature) compared with nondoped (ca. 0.30 wt.%) and especially carbon nanotubes (0.175 wt.%) [89]. This increase in hydrogen adsorption the authors explain by the charge transfer from potassium on the silicon and carbon atoms. It is noted that non-doped silicon carbide nanotubes

11

Fig. 9. Hydrogen adsorption by silicon carbide, silica and carbon samples [90].

(obviously in a case of the close texture parameters) are characterized by the higher sorption capacity towards hydrogen than carbon nanotubes, which is caused by the charge transfer from the silicon atoms to carbon atoms in the SiC structure. However, the presence of the adsorption sites with high energy in K-doped silicon carbide nanotubes leads to the necessity of raising the release temperature of the adsorbed hydrogen which is a disadvantage from an energy standpoint of its storage [89]. Silicon carbide samples obtained by carbothermal reduction of carbon–silica composites show high adsorption capacity toward hydrogen (up to 1.24 wt.% at 77 K and 1 atm for a sample prepared from silica MMS KIT-6) at a low level of the adsorption energy (up to 2.3 kJ/mol) compared, in particular, with carbon (ca. 5.0 kJ/mol) [90]. There is a significant increase in the specific hydrogen adsorption on the surface of the investigated silicon carbide (up to ca. 15 mmol/m2) compared with silica (
3 mmol/m2) and even carbon (5–6 mmol/m2) (Fig. 9). Probably the revealed effect can be explained by already expressed in the literature assumption about the ability of the Si C bonds to induce the hydrogen dipoles and perhaps by an additional participation of the surface defects of silicon carbide as the adsorption sites for the hydrogen molecules. The calculated values of the specific hydrogen adsorption for the obtained silicon carbide samples (up to
15 mmol/m2) correspond to almost complete filling of the surface with hydrogen and therefore to the limit value of its adsorption. The obtained results open the possibility of a significant increase of the adsorption capacity of the silicon carbide based materials towards hydrogen providing corresponding the development of the surface area (for SiC example with the specific surface area of 410 m2/g total hydrogen adsorption is 1.24 wt.%) [90]. Eomparison of the above data on the hydrogen adsorption indicating the processing method, the specific surface area and an amount of adsorbed hydrogen is presented in Table 2 (theoretical calculations of H2 adsorption on SiC were not taken into account).

Table 2 Hydrogen adsorption on porous silicon carbide. SiC sample

Processing method

Specific surface area

Hydrogen adsorption (conditions)

References

SiC nanotubes

Use of silicon powders (the interaction of multiwall carbon nanotubes with Si at 1300  E)

60 m2/g

0.2 wt.% (5.1 MPa and 298 K)

[86]

K-doped SiC nanotubes

Carbothermal reduction (SiO vapour + carbon nanotubes, 1200  E)

Not determined

0.37 wt.% (100 bar, room temperature)

[89]

Porous SiC

Carbothermal reduction (carbon–silica composites based on silica MMS, in particular KIT-6)

410 m2/g

1.24 wt.% (77 K and 1 atm)

[90]

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902

Electrochemical application

903

Template method and further carbonization using the aerosol spray drying method ollowed to obtain 3D hierarchical micro and mesoporous SiC spheres [91,92]. The self-assembly of the surfactants (cetyltriethylammonium bromide (CTAB), polyethylene glycol hexadecyl (Brij56), and poly(ethylene glycol)-block-poly (propylene glycol)-block-poly(ethylene glycol) (P123)) leads to the mesopore formation and the partial evaporation of Si atoms during carbonization results in the micropore generation. SiC obtained using Brij56 demonstrated the highest electrochemical performance with a specific capacitance of 253.7 F/g (a scan rate of 5 mV/ s) and 87.9% rate performance from 5 to 500 mV/s (electrolyte—1 M Na2SO4). The obtained results the authors explaned by a synergistic effect ensured by the dual-pore system. In general, for an ideal porous electrical double layer capacitor (EDLC) [93] the nanopore structure has a short ion diffusion distance, providing fast ion transport pathways [91]. The excellent electrochemical properties of the obtained SiC materials the authors explain by the following reasons. Firstly, mesopores provide low-resistant pathways for ion diffusion and good charge propagation resulting in an improved capacitive activity. Secondly, the abundant micropores play an essential role in optimizing the electrical double layer surfaces and strengthening the value of capacitance. Besides the high values of surface area and pore volume of the prepared SiC, owing to the dualpore micro/mesoporous system, provide the electrochemically available surface area for the charge accumulation and facilitating the transport of electrolyte ions, remarkably improving the electrochemical performance [91]. Thus mesopores effectively reduces the resistant pathways for ion diffusion and provides an accessible large surface area for ion transport/charge storage [91] while micropores provide a continuous increase of charge accommodation [92]. Hierarchical micro/mesoporous SiC flakes with a high specific surface area (1376 m2/g) were obtained via one-step carbonization of waste Si wafer without chemical or physical activation [94]. The mesopores were generated due to the integration of neighboring micropores. The obtained materials demonstrate high charge storage capacity (a specific capacitance of 203.7 F/g at a scan rate of 5 mV/s, electrolyte—1 M KCl). The proportion of micro- and mesopores in similar hierarchical SiC-based frameworks can be controlled by the carbonization temperature by controlling the amount of evaporated Si atoms [94,95]. Using of a Brij56 as the mesopore template and carbonization at 1250  C allow to obtaine material with a high charge storage capacity (a specific capacitance of 259.9 F/g at a scan rate of 5 mV/s, electrolyte—1 M KCl). According to the authors [94,95] a high electrochemical performance is due to the synergistic effect of both the enhanced electric double layer properties (caused by micropores) and reduced resistant pathways for ion diffusion through the pores and an accessible large surface area for ion transport/charge storage (caused by mesopores). Functionalization of the surface of the micro- and meso-porous silicon carbide spheres [91] and flakes [94] with oxygencontaining groups (introduced via oxidation of SiC with hydrogen peroxide) leads to an increase of the total super-capacitive performance up to 301.1 F/g [96] and 243.3 F/g [97], respectively. The obtained capacitive performance of such oxidized materials includes both the electric double layer capacitance and the pseudo-capacitance related to the oxygen-containing functional groups. Porous carbons obtained from porous silicon carbide can also be applied as materials for supercapacitors. For example, chlorination of the ordered mesoporous SiC obtained via magnesiothermic reduction of carbon–silica precursors leads to the formation of micro/mesoporous carbon [98]. Their investigation as an electrode

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material for supercapacitors showed gravimetric capacitance of 80 F/g and 90% of capacity retention at 1 V/s. The authors consider such hierarchical porous carbons very promising for high power supercapacitors due to a low intrinsic resistance, high ion accessibility of the hierarchical micro/mesoporous structure and a low relaxation time. Chlorination of silicon carbide nano-powder (a particle diameter ca. 60) with subsequent activation with KOH allowed to obtaine the nanoscale microporous carbide-derived carbon [99]. The resulting material exhibits an increased specific capacitance (141 F/g) compared with the initial carbon (54 F/g) due to the higher specific surface area, a hierarchical micro- and meso-porous structure, and the shorter inherent ion transport distance.

967

Silicon carbide based ceramics

980

Due to unique combination of physical and chemical properties, chemical stability, fire resistance, wear resistance SiC-ceramics is widely demanded in mechanical engineering, nuclear power engineering, on the enterprises of defense, metallurgical, food, chemical, petroleum and refining industries [100–103]. In recent decades an intensive researches on the development of the composite materials based on non oxide compounds— carbon, silicon carbide and silicon nitride etc. in which these compounds can be both a matrix and reinforcing filler in the form of continuous or discrete fibers, whiskers, plates (E/E, E/SiC, SiC/ SiC composites) are conducted. Such materials have high strength characteristics, heat resistance, low density, which allows their use in aviation and space technology as high-temperature constructional materials, for manufacturing of the elements of gas turbines, diesel engines, heat exchangers, in tribo-engineering. Ceramics based on porous silicon carbide which is characterized by high values of mechanical strength (60 MPa on flexure, 240 MPa on compression) and thermal conductivity (2 W/mK) was obtained via stepped pyrolysis of polysiloxane in the presence of carbon using hollow polymethylmethacrylate microspheres [104]. Carbothermal reduction of polysiloxane-derived SiOC in the presence of polymer microbeads poly(methylmethacrylate-coethylene glycol dimethacrylate) followed by sintering results in the formation of porous ceramics based on silicon carbide [105]. The porosity of the resulting material varies between 32–64% by adjusting the sintering temperature and the SiC powder: polysiloxane-derived SiC ratio in the initial reaction mixture. Sintering of a SiC ceramic bonded carbon in vacuum (by spark plasma sintering) with subsequent volatilization of the carbon particles by heating in air at 1000  C without shrinkage leads to the obtaining of the porous SiC ceramics [106]. The synthesized material possess a honeycomb structure which involves pores of
20 mm resulting from carbon removal and open pores of 2.1 mm formed in the sintered SiC shell. The obtained SiC ceramics demonstrates high strength, in particular the bending strength is 26 MPa and compressive one is 105 MPa. Porous SiC membrane is another good potential candidate for many advanced engineering applications (ceramic hot gas filters, gas separation etc.) [5,107–112]. The nanoporous hydrogen selective SiC membranes could be used in membrane reactors for the water gas shift and steam reforming reactions [107]. SiC microporous membranes prepared by the pyrolysis of thin allyl-hydridopolycarbosilane films coated, using a combination of slip-casting and dip-coating techniques, on tubular silicon carbide macroporous supports exhibite an ideal H2/CO2 selectivity in the range of 42–96, and the H2/CH4 ideal selectivity in the range of 29– 78 [108]. Nanoporous silicon carbide membranes prepared by periodic and alternate coatings of polystyrene sacrificial interlayers and silicon carbide pre-ceramic layers on the top of slip-casted tubular

981

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982 983 984 985 986 987 988 989 990 991 992 993 994 995 996 997 998 999 1000 1001

Q2 1002 1003 1004 1005 1006 1007 1008 1009 1010 1011 1012 1013 1014 1015 1016 1017 1018 1019 1020 1021 1022 1023 1024 1025 1026 1027 1028 1029 1030

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SiC supports, exhibit single gas ideal separation factors of He and H2 over Ar in the ranges 176–465 and 101–258, respectively, which is 2–3 fold higher than those of SiC membranes prepared by conventional techniques. The improved membrane characteristics the authors refer to the sacrificial interlayers filling the pores in the underlying structure and preventing their blockage by the preceramic polymer [109].

1038

Other applications

1039

1066

The other applications of silicon carbide based materials are also possible. For example, the perspective of using of porous monolithic multi-channeled honeycomb silicon carbide structures as open volumetric receivers of concentrated solar radiation was showed [113]. There is a significant increase of SiC hardness and compressive strength after irradiation. The growing interest in recent years to silicon carbide as a promising semiconductor material for sensitive elements of the gas sensors (for hydrocarbons) is caused by the peculiarities of its structure and electrophysical parameters. The efficiency of such gas sensitive sensors significantly increases upon using a porous silicon carbide with a relatively high specific surface area and allows to achieve high sensitivity of sensors, selectivity and rapid recovery in the conditions of extreme environmental parameters [114]. An impregnation of carbonized wood monoliths with polycarbosilane followed by pyrolysis and high-temperature chlorine treatment results in the formation of biomorphic carbide-derived carbon materials with hierarchical pore structure [115]. A higher amount of the infiltrated polymer into the wood monolith (achieved by an increase of concentration, time, and number of impregnation cycles) leads to a higher specific surface areas of the resulting materials (up to 940 m2/g). The other important areas of practical applications of silicon carbide are creation of membranes, porous burners, Li-ion batteries, methanol fuel cells, microbial fuel cells etc. which is described in Ref. [5].

1067

Conclusions

1068

Silicon carbide is an important semiconductor material with unique physical and chemical properties such as high thermal conductivity, thermal and mechanical stability, hardness, chemical inertness. In this regard, obtaining of silicon carbide based dispersed, porous, chemically and thermally stable sorbents, supports, catalysts, photocatalysts and materials of other functional purposes is an important task. The analysis of literature data regarding only some issues and aspects of the chemistry of silicon carbide, shows that, despite the significant number of works and apparent success, the research of the conditions of synthesis, properties, and possible areas and ways of using of porous silicon carbide remain current and promising. Many different approaches to the synthesis of porous silicon carbide, which include electrochemical etching of massive SiC, carbothermal/magnesiothermic reduction of carbon–silica composites, nanocasting involving polycarbosilanes etc. were developed. Silicon carbide obtained from polycarbosilanes by nanocasting has the highest porosity characteristics, and possesses spatial ordering in the nanometer range too which makes this method the most promising one. The approach using catalysts to reduce the temperature of the synthesis, in particular magnesiothermic reduction is also interesting. However, perphaps using of nanocasting involving polycarbosilanes and magnesiothermic reduction at this stage in practice is limited due to expensive

1032 1033 1034 1035 1036

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13

precursors or the necessity of multiple postsynthetic treatments to remove the catalyst, respectively. Considering this, carbothermal reduction of carbon-silica composites remains for the practice the most optimal method of obtaining of porous silicon carbide. In view of the above, careful selection of the initial composites, which carbon components are characterized by the most developed surface area including the mesopore specific surface area is necessary to achieve the highest porosity characteristics. Further development of the methods for preparation of porous silicon carbide can include synthesis of hierarchical or micromesoporous materials, particularly using mesoporous zeolites. The research of the conditions of obtaining and physical and chemical properties of silicon oxycarbide SiCO seems to be an interesting and informative, but not yet fully implemented. This material can also be a promising initial material-reagent for creating of new dispersed and porous derivatives as a basis of adsorbents, catalysts and photocatalysts etc. Porous silicon carbide with deposited metals and metal oxides nanoparticles exhibits high catalytic ability in various catalytic processes such as reaction of direct oxidation of butane into maleic anhydride, isomerization of linear saturated hydrocarbons, selective oxidation of hydrogen sulfide into elemental sulfur, hydrogenation of butadiene, methane oxidation, neutralization of exhaust gases of the cars, the carbon dioxide reforming of methane and other high-temperature and highly exothermic reactions. Silicon carbide modified with some substances (such as silica, carbon etc.) is very promising as new stable, high efficiency and even co-catalyst-free photocatalyst. Further researches should be devoted to the study of the adsorption properties of silicon carbide, in particular, its adsorption capacity toward hydrogen. Considering the theoretical calculations and the obtained practical results on hydrogen adsorption of SiC based materials, the indicated direction seems to be promising. In this regard clarification of the reasons of high hydrogen adsorption in particular study of the features of the silicon carbide surface, hydrogen adsorption mechanism etc. is relevant. New direction of use of silicon carbide as a material for supercapacitors is topical and promising. Considering the shown high capacitance characteristics the indicated direction will develop rapidly, particularly as for clarifying the influence of the structure, texture parameters, SiC surface nature etc. on electrochemical performance. Furthermore, porous silicon carbide can be used as a template or starting material for synthesis of other nanostructures, such as carbon as a result of chlorination of nanoporous SiC. Of course, traditional applications of SiC, particularly as ceramics components etc., which also have the potential for further development can not be rejected. The presented review undoubtedly does not include all aspects of the chemistry of silicon carbide, and, obviously, the researches in this area will be developed.

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