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Achieving excellent oxidation resistance and mechanical properties of TiB2–B4C/carbon aerogel composites by quick-gelation and mechanical mixing

  • Pengfei Li , Minxian Shi , Zongyi Deng , Pengkun Han , Tingli Yang , Rui Hu , Chuang Dong , Rui Wang and Jie Ding EMAIL logo
Published/Copyright: November 5, 2022
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Nanotechnology Reviews
From the journal Nanotechnology Reviews Volume 11 Issue 1

Abstract

Thermal protection system (TPS) is of great significance to launch hypersonic flight and landing process of hypersonic vehicles, which can effectively shield the hypersonic vehicle from severe aerodynamic heating encountered. Phenolic aerogels play an important role in TPS due to their characteristics of low density, high porosity, and low thermal conductivity. However, phenolic aerogel is easy to be oxidized at elevated temperatures under oxidizing environments, which severely limits its large-scale application as thermal insulation materials in TPS. In this study, a novel TiB2–B4C/carbon (TB/C) aerogel composite was synthesized by introducing TiB2 and B4C particles into phenolic aerogels through quick-gelation and mechanical mixing. The developed aerogel composites were characterized by scanning electron microscopy, Fourier transform infrared, thermal analysis, etc., to evaluate their microstructure, oxidation resistance, and mechanical properties. Experimental evidence showed that TiB2 and B4C particles reacted with the oxygen-containing molecules to form TiO2–B2O3 layer, which effectively improved oxidation resistance and mechanical properties of phenolic aerogel composites.

Keywords: particle-reinforced composites; thermal properties; phenolic aerogel composites

1 Introduction

Phenolic aerogels were widely used in hypersonic vehicles, civil structural edifices, and industrial architectures [1,2,3]. Incorporation of inorganic particles into a phenolic aerogel matrix can significantly improve mechanical, oxidation resistance, and fire retardancy of the organic–inorganic aerogel composites. However, phenolic aerogels are usually prepared via a week-long base-catalyzed gelation process, and deionized water or anhydrous ethanol is chosen as the solvent [4,5]. It is difficult to achieve well-dispersed inorganic particles in phenolic aerogels because of inorganic particle sedimentation due to gravity and incompatibility with precursor solution [6].

At present, there are two ways to modify the surface of inorganic particles by chemical treatments to increase the affinity of the inorganic particle surface for precursor solution [7,8]. The first one is accomplished through adding modified nanoparticles into polymer aerogels. Pulci et al. achieved surface modification of ZrO2 nanoparticles with several organic acids, demonstrating that the addition of nano-ZrO2 produces an improvement of both thermal and mechanical performance compared with pristine material [9]. The second method is using silane coupling agents to modify particle surfaces, thus improving the compatibility between the particle surfaces and precursor solution. Liu et al. used trimethoxy silane to modify halloysite nanotubes (m-HNTs) and introduced m-HNTs into the phenolic aerogel [10]. The obtained aerogel composite exhibited low carbonization shrinkage (30.83%) and enhanced residue yield (73.24%) at 1,000°C protected in N2 atmosphere.

Functional inorganic particles, such as B4C, TiB2, and ZrB2 particles, are generally considered as excellent candidates for thermal oxidation applications [11,12]. Compared with traditional inorganic particles, such as TiO2, ZrO2, SiO2, and Halloysite nanotubes, functional inorganic particles can react with oxygen-containing molecules to form oxides and increase the residue yield of composite during the oxidation process [13,14]. For example, TiB2 particles react with the oxygen-containing molecules to form B2O3 and TiO2 [15]. Besides, molten B2O3 cover the oxidized surface and form protective layer, which can effectively inhibit the oxidation of phenolic aerogel in the interior [16,17]. However, these functional inorganic particles are chemically inert and cannot be chemically treated to increase the compatibility of the particle surface for the solvent. For this reason, it is extremely difficult to efficiently introduce functional inorganic particles into phenolic aerogel.

In this work, a quick-gelation approach to achieve better dispersibility of TiB2 and B4C particles in the phenolic aerogel is reported. The gelation of resorcinol with formaldehyde could be remarkably accelerated by acid catalysis because the addition of formaldehyde is an electrophilic aromatic substitution reaction [18,19,20,21]. In Table 1, this work is compared with other existing works. As can be seen from Table 1, this work has ultra-quick time of gelation. Thus, trifluoroacetic acid (CF3COOH) is used as a catalyst to accelerate gelation, which avoids the severe sedimentation of TiB2 and B4C particles over time in precursor solution. The oxidation of TiB2 and B4C particles at elevated temperatures could form a protective layer, which can effectively improve oxidation resistance and mechanical performance of aerogel composites. The introduction of TiB2 and B4C particles into phenolic aerogels in this study only requires simple mechanical mixing without complex chemical treatment, which is suitable for large-scale production.

Table 1

Comparison of gelation time of phenolic aerogels

Catalyst Solvent Molar ratio of R:F Ratio of solvent catalyst T (°C) Gelation time Ref.
Na2CO3 H2O 1:2 72.5a 85 >2 days [16,17]
HCl CH3CN 1:2 21b 80 10 min [16]
CF3COOH H2O 1:3 20b 35 15–30 s This work

R: Resorcinol; F: formaldehyde; a: the molar ratio of solvent: catalyst; b: the volume ratio of solvent:catalyst.

2 Experimental

2.1 Materials

Formaldehyde (37.0 wt% aqueous solution, AR) and resorcinol (AR) were purchased from Aladdin Industrial Inc. Deionized water was supplied in our laboratory. CF3COOH was obtained from Macklin Biochemical Co., Ltd. TiB2 and B4C particles (purity > 98%) with particle size of 1–10 μm, used as fillers, were provided by Aladdin Industrial Inc. All chemicals were used as-received with no further purification.

2.2 Preparation of TB/C aerogel composites

Figure 1 shows schematic illustration of the preparation process of TB/C aerogel composites. In this work, resorcinol, formaldehyde, and deionized water were referred to as R, F, and W, respectively. The molar ratios of F:R and W:R were maintained at 3:1 and 1:2, respectively. The weight ratio of TiB2:B4C was 1:1. According to the method, the precursor solutions, containing R, F, and W, were mixed by a magnetic stirrer at 35°C, and the solid content of the precursor solutions was recorded as 1. Suspension was manufactured by dissolving precursor solutions (solid content is 1) and 0, 10, 30, 50, 70, and 90% of filler (mixture of TiB2 and B4C) under vigorous stirring for 30 min, and then decanted into glass molds. Second, the appropriate amount of CF3COOH was dropped into glass molds. The volume ratio of suspension:CF3COOH was 20:1. The glass molds were sealed and placed into tube holder at room temperature for gelation to form hydrogels. Typically, the gel time is about 20–40 s and the aging time is 2 h. The obtained hydrogels were directly dried in an oven at 50°C for 24 h, 70°C for 24 h, and 90°C for 24 h to obtain aerogel composites. Finally, the samples were carbonized at 1,000°C for 20 min in muffle furnace. The uncarbonized phenolic (Ph) aerogel monomers were expressed as TB/Ph-x-y, and the carbon aerogel monomers were denoted as TB/C-x-y, where x refers to the content of TiB2 and B4C in TB/Ph-x-y, and y indicates carbonization temperature.

Figure 1 Schematic illustration for the preparation process of TB/C aerogel composites.
Figure 1

Schematic illustration for the preparation process of TB/C aerogel composites.

2.3 Characterization

The morphological microstructure of the samples was characterized by scanning electron microscopy (SEM; HitachiS-4800F) at an acceleration voltage of 10 kV. The groups of aerogel composites were characterized with Fourier Transform Infrared (FT-IR) spectra and recorded on a Nexus 670 FTIR spectrometer with KBr pellets in the wave number range of 4,000–500 cm−1. Thermal stability test of the aerogel composites was performed by a NETZSCH STA449F3 thermal analyzer. Compressive strength of the cylindrical samples (r × h: 10 mm × 20 mm) was measured by electronic universal testing machine with a testing speed of 1.0 mm min−1. The XRD patterns of the TB/C aerogel composites were measured by an X-ray diffractometer, Bruker D8 Advance Discover with CuKα radiation (40 kV, 40 mA). The thermal residue of TB/C aerogel composites was also characterized by X-ray photoelectron spectroscopy (XPS). Drying and carbonization shrinkages were calculated by measuring the diameter of each cylindrical sample before and after drying and carbonization, respectively. Densities were determined through dividing weight by volume. Thermal conductivity was determined by the Hot Disk thermal protection system (TPS) 2500 thermal constant analyzer at 25°C.

3 Results and discussion

3.1 Microstructure of TB/C aerogel composites

The microstructures of the TB/C aerogel composites with different TiB2 and B4C contents are shown in Figure 2. SEM images show that TB/C aerogel composites are basically composed of well-connected microspheres, which are connected through clear neck and randomly gather together to obtain “grape string” appearance. For pure carbon aerogel without TiB2 and B4C added (Figure 2a), the diameter of carbon microspheres is about 1 μm and its surface is smooth. The morphology of samples begins to change as TiB2 and B4C particles are introduced, and in Figure 2b and c, the B2O3 layers start to appear and the TiO2 grains are primitively generated. For TB/C-90 aerogel composites (Figure 2d2), the diameter of microspheres is about 620 nm.

Figure 2 (a)–(d) SEM images of TB/C aerogel composites with different TiB2 and B4C contents: (a1), (a2) 0; (b1), (b2) 10%; (c1), (c2) 50%; and (d1), (d2) 90%.
Figure 2

(a)–(d) SEM images of TB/C aerogel composites with different TiB2 and B4C contents: (a1), (a2) 0; (b1), (b2) 10%; (c1), (c2) 50%; and (d1), (d2) 90%.

The FTIR spectra of the TB/Ph aerogel composites with different TiB2 and B4C contents are shown in Figure 3a. The TB/Ph aerogel composites exhibited typical adsorptions of Ph–OH at 3,410 cm−1 (stretching), CH2 stretching at 2,926 cm−1, C═C vibration of aromatic rings at 1,617 and 1,476 cm−1, Ph–O stretching vibrations of phenolic hydroxyl group at 1,220 cm−1, and C–O stretching vibrations of methylene ether bridges (CH2−O−CH2) at 1,090 cm−1. Bands at 1,015 cm−1 were ascribed to C–O stretching vibration of CH2OH. The TB/Ph aerogel composites exhibited absorption peak of the hydrogen bonds (OH···O) at 3,224 cm−1 (Figure 3c) [22,23,24]. Presumably, hydrogen bonds (OH···O) are generated by the residual non-hydrolyzed hydroxymethyl groups (CH2OH) and phenolic hydroxyl group (Ph-OH) [25]. As the content of TiB2 and B4C is increased, the intensity of the hydrogen bonds increases, indicating incorporation of more CH2OH and Ph–OH in the form of hydrogen bonds.

Figure 3 (a) FTIR spectra of TB/Ph aerogel composites, (b) methylene ether bridge index of TB/Ph aerogel composites, and (c) interactions of TB/Ph aerogel composites.
Figure 3

(a) FTIR spectra of TB/Ph aerogel composites, (b) methylene ether bridge index of TB/Ph aerogel composites, and (c) interactions of TB/Ph aerogel composites.

Peaks at 1,617 cm−1 were assigned to the C═C vibration of aromatic rings, which were consistent in each reaction system and unaffected by the content of TiB2 and B4C particles [26]. Thus, bands at 1,617 cm−1 could be used as a standard for analysis. The excessive formaldehyde (F/R = 3) allows the conjecture that most of the 2-, 4-, and 6-positions of the resorcinol aromatic rings react and form the corresponding hydroxymethyl derivatives. Thus, the molar ratio of methylene ether bridges (CH2−O−CH2) is much higher than that of methylene bridges (CH2) in aerogel composites. Based on the absorption intensities (A 1 and A 0) of the methylene ether bridges and phenyl groups (1,090 and 1,617 cm−1, respectively), we can calculate the methylene ether bridge index (I) of the TB/Ph aerogel composites by the following relationship: I  =  A 1/A 0. As shown in Figure 3b, it is apparent that the methylene ether bridge index decreases from 1.14 to 0.91 with the increased content of TiB2 and B4C, which was attributed to the added TiB2 and B4C particles hindering the motion of organic clusters and eventually partial CH2OH and Ph-OH had not participated in the sol–gel reaction. This can result in different thermal stability and compressive strength of TB/Ph aerogel composites due to fewer methylene ether bridges [27,28,29]. All these are consistent with the FTIR spectra, TG, and comprehensive strength analysis.

3.2 Oxidation resistance and thermal stability of TB/Ph aerogel composites

3.2.1 TG-DTG analysis

As shown in Figure 4b and Table 2, the temperature of the maximum degradation rates (T max1) for pure phenolic aerogel (494.4°C) are greater than that for TB/Ph aerogel composites. These results reveal that the thermal stability of aerogels is decreased clearly with the introduction of TiB2 and B4C particles by mechanical mixing. TiB2 and B4C particles will affect the condensation between hydroxymethyl derivatives of resorcinol and lead to a reduction in the number of methylene ether bridges (CH2−O−CH2). These are consistent with the FTIR spectra analysis. Moreover, with the increase in TiB2 and B4C particle content, T max1 increases slightly, as the formation of B2O3-protected structure will increase the T max1. This should be attributed to oxidation of partial B4C particles at temperatures below 500°C [30]. Interestingly, we discover that the residue yield of TB/Ph aerogel composites at high temperatures could be evidently increased by the presence of TiB2 and B4C particles. The residue yield of pure phenolic aerogel was 5.68%, while that of TB/Ph-90 hold was 90.01% at 1,000°C, indicating the outstanding oxidation resistance of TB/Ph aerogel composites.

Figure 4 (a) TG curves of samples at a heating rate of 10°C min−1 from room temperature to 1,000°C under air atmosphere; (b) DTG curves of samples at a heating rate of 10°C min−1 from room temperature to 1,000°C under air atmosphere.
Figure 4

(a) TG curves of samples at a heating rate of 10°C min−1 from room temperature to 1,000°C under air atmosphere; (b) DTG curves of samples at a heating rate of 10°C min−1 from room temperature to 1,000°C under air atmosphere.

Table 2

Thermal decomposition characteristics of TB/Ph aerogel composites

Samples T max1/°C T max2/°C Residue yield%
300°C 600°C 1,000°C
TB/C-0 494.4 / 88.75 5.8 5.68
TB/C-10 437.0 717.3 88.04 16.51 21.45
TB/C-30 429.7 712.6 92.55 35.37 49.25
TB/C-50 458.3 706.6 95.29 51.01 70.83
TB/C-70 455.8 724.7 95.10 54.02 79.83
TB/C-90 455.8 716.5 95.03 61.97 90.01

T max1: temperature of the maximum degradation rate. T max2: temperature of the maximum mass gain rate.

As shown in Figure 4a and Table 2, the degradation processes of TB/Ph aerogel composites both can be divided into three stages [31]. Take the TB/Ph-90 for example, the first stage with little mass loss (<5%) is from room temperature to 300°C, and the mass loss of the samples is mainly due to the evaporation of the free water in the aerogels. When the temperature reaches 600°C, severe mass loss is observed in the TG curves. With the pyrolysis of phenolic aerogels, many kinds of pyrolysis volatiles including H2O, CO, CO2, H2, CH4, and other derivates are released out [32,33]. The oxygen-containing molecules, including CO, O2, CO2, and H2O, take a large proportion in the number of volatiles, and provide a source of oxidizing atmosphere. In the step of 600–1,000°C, the residue yield of the TB/Ph aerogel composites increased continuously with the increased content of TiB2 and B4C particles, which means that some weight gain reactions between TiB2 and B4C particles and oxygen-containing molecules should have occurred. As listed in Table 2, the residue yield of TB/Ph-90 aerogel composites increased from 61.97 to 90.01%, when temperature was increased from 600 to 1,000°C. Some main gain reactions are given as follows:

(1) 2 TiB 2 ( s ) + 5 O 2 ( g ) = 2 TiO 2 ( s ) + 2 B 2 O 3 ( l , s ) ,

(2) TiB 2 ( s ) + 5 CO ( g ) = TiO 2 ( s ) + B 2 O 3 ( l , s ) + 5 C ( s ) ,

(3) 2 TiB 2 ( s ) + 5 CO 2 ( g ) = 2 TiO 2 ( s ) + 2 B 2 O 3 ( l,s ) + 5 C ( s ) ,

(4) TiB 2 ( s ) + 5 H 2 O ( g ) = TiO 2 ( s ) + B 2 O 3 ( l,s ) + 5 H 2 ( g ) ,

(5) B 4 C ( s ) + 5 O 2 ( g ) = 2 CO 2 ( g ) + 2 B 2 O 3 ( l,s ) ,

(6) B 4 C ( s ) + 6 H 2 O ( g ) = C ( s ) + 2 B 2 O 3 ( l,s ) + 6 H 2 ( g ) .

3.2.2 EDS, XRD, and XPS analyses

To further verify the occurrence of the weight gain reactions, EDS and XRD analyses are employed. As shown in Figure 5a, only the C and O elements are detected on the surface of carbon microspheres without TiB2 and B4C. As shown in Figure 5c, the molar ratio of oxygen and titanium in white spot is approximately equal to 5.38, while the molar ratio of TiO2 is 2. These results implied that new substance was formed and coated on the surface of carbon microspheres. Figure 5d shows the XRD patterns of the residues for TB/C-30 aerogel composites at 25–1,200°C. There are TiB2 and B4C diffraction peaks in the non-carbonized aerogel samples. The diffraction peak of TiO2 can be evidently detected at 800°C, which confirms the oxidation of TiB2. Besides, broad peak e observed at 2θ angles of about 25° is the characteristic peak of amorphous carbon.

Figure 5 EDS analysis of aerogel composites: (a) TB/C-0; (b and c) TB/C-30; (d) XRD pattern of the TB/C-30 aerogel composites. wt%: mass fraction, At%: atomic fraction.
Figure 5

EDS analysis of aerogel composites: (a) TB/C-0; (b and c) TB/C-30; (d) XRD pattern of the TB/C-30 aerogel composites. wt%: mass fraction, At%: atomic fraction.

The oxygen, titanium, nitrogen, carbon, and boron elements are detected from the full-scan XPS spectrum of the thermal residues (Figure 6a). The high-resolution B1s XPS spectrum for the thermal residues (Figure 6b) shows a prominent peak at 193.28 eV, usually assigned to the contribution of B2O3, and the peak detected at energy (190.38 eV) corresponds to the B–O binding [34]. The diffraction peaks of B2O3 are not detected by XRD due to its amorphous form in the aerogel network, which has flowability at high temperature (melting point is 450°C) [35,36,37]. The glassy B2O3 could cover the surface of the carbon aerogel by forming a continuous protective film and improving the oxidation resistance of composites.

Figure 6 XPS spectra of TB/C-30 aerogel composites: (a) a full-scan and (b) B1s.
Figure 6

XPS spectra of TB/C-30 aerogel composites: (a) a full-scan and (b) B1s.

3.2.3 Microstructure of TB/C aerogel composites at different carbonization temperatures

Figure 7 illustrates the microstructure transformation of TB/C aerogel composites at different carbonization temperatures. As shown in Figure 7a2, the TB/C-30-800 exhibits typical aerogel network with overlapping structure, and the TiO2 grains are randomly dispersive and coated on the surface of aerogel nanospheres. The presence of B2O3 can densify the surface of aerogel nanospheres and form a protective barrier against high-temperature oxidation. As the carbonization temperature reaches to 1,200°C, the aerogel composites maintain a stable porous nanostructure and form bigger TiO2 grains with the size of 100 nm (Figure 7c2).

Figure 7 (a)–(c) SEM images of TB/C-30 aerogel composites at different carbonization temperatures: (a1), (a2) 800°C; (b1), (b2) 1,000°C; and (c1), (c2) 1,200°C.
Figure 7

(a)–(c) SEM images of TB/C-30 aerogel composites at different carbonization temperatures: (a1), (a2) 800°C; (b1), (b2) 1,000°C; and (c1), (c2) 1,200°C.

3.3 Mechanical and thermal insulation properties

As shown in Figure 8a, densities of TB/Ph aerogel composites increase remarkably from 0.379 to 0.582 g cm−3 with the increased content of TiB2 and B4C. This should be attributed to the introduction of TiB2 (4.52 g cm−3) and B4C (2.52 g cm−3) particles [38]. The density of the TB/C-90 aerogel composites increases slightly from 0.582 to 0.647 g cm−3, majorly due to some weight gain reactions during the carbonization process. Figure 8b presents the compressive strength of samples. The lowest compressive strength of TB/Ph aerogel composites is shown by TB/Ph-90, which also should be attributed to the introduction of TiB2 and B4C in aerogels. The increase of TiB2 and B4C particles will affect the sol–gel polymerization of organic clusters and eventually weaken the network skeleton of TB/Ph aerogel composites [39,40,41], which is consistent with the FTIR spectra. Interestingly, it is apparent that the compressive strength of the TB/C aerogel composites first increased from 0.62 to 1.94 MPa and then decreased from 1.94 to 1.06 MPa with a further increase in TiB2 and B4C contents (Figure 8b). This should be attributed to the formation of protective structure, which can reduce the pyrolysis of phenolic aerogel matrix and retain its strength. However, TiO2 grains and glassy B2O3 are not assembled into a solid unified structure due to the short carbonization time (only 20 min). Therefore, with the increase of TiB2 and B4C contents, the compressive strength will still show a downward trend, which is similar to the compressive performance trend of uncarbonized aerogels.

Figure 8 (a) Density of samples and (b) comprehensive strength of samples.
Figure 8

(a) Density of samples and (b) comprehensive strength of samples.

As displayed in Figure 9a, the drying shrinkage dropped remarkably from 6.03 to 1.85% with the rise of TiB2 and B4C contents. This phenomenon can be explained by particle enhancement. With the increase of TiB2 and B4C contents, TB/Ph aerogel composites can more effectively against shrinkage due to the huge capillary force generated during ambient pressure drying. Figure 9b illustrates the change of carbonization shrinkage from TB/Ph to TB/C aerogel composites during carbonization process. The carbonization shrinkage decreases dramatically from 16.18 to 3.52% when changing the content of TiB2 and B4C from 10 to 90%, revealing that the introduction of TiB2 and B4C particles can effectively restrain the oxidation and improve mechanical properties of composites due to the formation of TiO2–B2O3 layer.

Figure 9 (a) Drying shrinkage of samples and (b) carbonization shrinkage of samples.
Figure 9

(a) Drying shrinkage of samples and (b) carbonization shrinkage of samples.

The thermal conductivities of TB/Ph and TB/C aerogel composites were measured at 25°C, and the results are shown in Figure 10a. Typically, the total thermal conductivity includes solid conductivity, gas conductivity, convection transmission, and radiation transmission [42], which can be schematically illustrated in Figure 10b. As the content of TiB2 and B4C particles increases, the thermal conductivities of TB/C aerogel composites gradually increase from 0.054 to 0.081 W m−1 K−1 at 25°C. On the one hand, the solid phase thermal conductivity increases ascribed to the high thermal conductivity of TiB2 and B4C (about 60–120 W m−1 K−1) [43]. On the other hand, the aggregation of particles is beneficial to solid-phase thermal conductivity, which will provide more solid-phase thermal transport pathways with the increase in density of the composites. When the content of TiB2 and B4C is 90%, the thermal conductivity of TB/Ph-90 aerogel composites is 0.081 W m−1 K−1, which increased by 70% compared with those of pure phenolic aerogels (0.048 W m−1 K−1).

Figure 10 (a) Thermal conductivity curves at 25°C of aerogel composites; (b) schematics illustrating thermal transport pathways.
Figure 10

(a) Thermal conductivity curves at 25°C of aerogel composites; (b) schematics illustrating thermal transport pathways.

During carbonization process, the TiB2 and B4C particles gradually transform to TiO2 grains and glassy B2O3 by oxidation reaction, which will fill the gap of aerogel microspheres and further improve the solid-phase thermal conductivity of TB/C aerogel composites. When the content of TiB2 and B4C is 90%, the thermal conductivity of TB/C-90 aerogel composites is 0.188 W m−1 K−1, which increased by 132.11% compared with TB/C-90 aerogel composites (0.081 W m−1 K−1). However, due to the porous structures, the heat transfers of gaseous thermal conduction and convection in TB/C aerogel composites are inhibited effectively.

4 Conclusion

By adjusting the content of TiB2 and B4C particles, a novel TB/C aerogel composite was fabricated via the sol–gel polymerization followed by ambient pressure drying and carbonization. During carbonization process, the TiB2 and B4C particles gradually transform to TiO2 grains and glassy B2O3 layer by oxidation reduction reaction, which densify the surface of aerogel nanospheres and form a protective barrier. The resulting TB/C aerogel composites exhibited low densities between 0.331 and 0.647 g cm−3, relatively high compressive strength, ranging from 0.62 to 1.94 MPa, and low thermal conductivities of 0.097–0.188 W m−1 K−1 at room temperature. When the content of TiB2 and B4C was 90%, the residue yield of aerogel composites was 90.01% at 1,000°C in air, which increased by 84.33% compared with that of phenolic aerogels. Therefore, this work provides a significant way to improve the oxidation resistance and mechanical properties of TB/Ph aerogel composites, and it may be useful for thermal structure in TPS, such as hypersonic vehicles and civil industrial architectures.

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  1. Funding information: This research was financially supported by the Joint Fund of Ministry of Education for Equipment Pre-research (6141A02022250).

  2. Author contributions: All authors have accepted responsibility for the entire content of this manuscript and approved its submission.

  3. Conflict of interest: The authors state no conflict of interest.

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Received: 2022-06-24
Revised: 2022-07-27
Accepted: 2022-09-14
Published Online: 2022-11-05

© 2022 Pengfei Li et al., published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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https://doi.org/10.1515/ntrev-2022-0489
Keywords for this article
particle-reinforced composites; thermal properties; phenolic aerogel composites
Creative Commons
BY 4.0

Articles in the same Issue

  1. Research Articles
  2. Theoretical and experimental investigation of MWCNT dispersion effect on the elastic modulus of flexible PDMS/MWCNT nanocomposites
  3. Mechanical, morphological, and fracture-deformation behavior of MWCNTs-reinforced (Al–Cu–Mg–T351) alloy cast nanocomposites fabricated by optimized mechanical milling and powder metallurgy techniques
  4. Flammability and physical stability of sugar palm crystalline nanocellulose reinforced thermoplastic sugar palm starch/poly(lactic acid) blend bionanocomposites
  5. Glutathione-loaded non-ionic surfactant niosomes: A new approach to improve oral bioavailability and hepatoprotective efficacy of glutathione
  6. Relationship between mechano-bactericidal activity and nanoblades density on chemically strengthened glass
  7. In situ regulation of microstructure and microwave-absorbing properties of FeSiAl through HNO3 oxidation
  8. Research on a mechanical model of magnetorheological fluid different diameter particles
  9. Nanomechanical and dynamic mechanical properties of rubber–wood–plastic composites
  10. Investigative properties of CeO2 doped with niobium: A combined characterization and DFT studies
  11. Miniaturized peptidomimetics and nano-vesiculation in endothelin types through probable nano-disk formation and structure property relationships of endothelins’ fragments
  12. N/S co-doped CoSe/C nanocubes as anode materials for Li-ion batteries
  13. Synergistic effects of halloysite nanotubes with metal and phosphorus additives on the optimal design of eco-friendly sandwich panels with maximum flame resistance and minimum weight
  14. Octreotide-conjugated silver nanoparticles for active targeting of somatostatin receptors and their application in a nebulized rat model
  15. Controllable morphology of Bi2S3 nanostructures formed via hydrothermal vulcanization of Bi2O3 thin-film layer and their photoelectrocatalytic performances
  16. Development of (−)-epigallocatechin-3-gallate-loaded folate receptor-targeted nanoparticles for prostate cancer treatment
  17. Enhancement of the mechanical properties of HDPE mineral nanocomposites by filler particles modulation of the matrix plastic/elastic behavior
  18. Effect of plasticizers on the properties of sugar palm nanocellulose/cinnamon essential oil reinforced starch bionanocomposite films
  19. Optimization of nano coating to reduce the thermal deformation of ball screws
  20. Preparation of efficient piezoelectric PVDF–HFP/Ni composite films by high electric field poling
  21. MHD dissipative Casson nanofluid liquid film flow due to an unsteady stretching sheet with radiation influence and slip velocity phenomenon
  22. Effects of nano-SiO2 modification on rubberised mortar and concrete with recycled coarse aggregates
  23. Mechanical and microscopic properties of fiber-reinforced coal gangue-based geopolymer concrete
  24. Effect of morphology and size on the thermodynamic stability of cerium oxide nanoparticles: Experiment and molecular dynamics calculation
  25. Mechanical performance of a CFRP composite reinforced via gelatin-CNTs: A study on fiber interfacial enhancement and matrix enhancement
  26. A practical review over surface modification, nanopatterns, emerging materials, drug delivery systems, and their biophysiochemical properties for dental implants: Recent progresses and advances
  27. HTR: An ultra-high speed algorithm for cage recognition of clathrate hydrates
  28. Effects of microalloying elements added by in situ synthesis on the microstructure of WCu composites
  29. A highly sensitive nanobiosensor based on aptamer-conjugated graphene-decorated rhodium nanoparticles for detection of HER2-positive circulating tumor cells
  30. Progressive collapse performance of shear strengthened RC frames by nano CFRP
  31. Core–shell heterostructured composites of carbon nanotubes and imine-linked hyperbranched polymers as metal-free Li-ion anodes
  32. A Galerkin strategy for tri-hybridized mixture in ethylene glycol comprising variable diffusion and thermal conductivity using non-Fourier’s theory
  33. Simple models for tensile modulus of shape memory polymer nanocomposites at ambient temperature
  34. Preparation and morphological studies of tin sulfide nanoparticles and use as efficient photocatalysts for the degradation of rhodamine B and phenol
  35. Polyethyleneimine-impregnated activated carbon nanofiber composited graphene-derived rice husk char for efficient post-combustion CO2 capture
  36. Electrospun nanofibers of Co3O4 nanocrystals encapsulated in cyclized-polyacrylonitrile for lithium storage
  37. Pitting corrosion induced on high-strength high carbon steel wire in high alkaline deaerated chloride electrolyte
  38. Formulation of polymeric nanoparticles loaded sorafenib; evaluation of cytotoxicity, molecular evaluation, and gene expression studies in lung and breast cancer cell lines
  39. Engineered nanocomposites in asphalt binders
  40. Influence of loading voltage, domain ratio, and additional load on the actuation of dielectric elastomer
  41. Thermally induced hex-graphene transitions in 2D carbon crystals
  42. The surface modification effect on the interfacial properties of glass fiber-reinforced epoxy: A molecular dynamics study
  43. Molecular dynamics study of deformation mechanism of interfacial microzone of Cu/Al2Cu/Al composites under tension
  44. Nanocolloid simulators of luminescent solar concentrator photovoltaic windows
  45. Compressive strength and anti-chloride ion penetration assessment of geopolymer mortar merging PVA fiber and nano-SiO2 using RBF–BP composite neural network
  46. Effect of 3-mercapto-1-propane sulfonate sulfonic acid and polyvinylpyrrolidone on the growth of cobalt pillar by electrodeposition
  47. Dynamics of convective slippery constraints on hybrid radiative Sutterby nanofluid flow by Galerkin finite element simulation
  48. Preparation of vanadium by the magnesiothermic self-propagating reduction and process control
  49. Microstructure-dependent photoelectrocatalytic activity of heterogeneous ZnO–ZnS nanosheets
  50. Cytotoxic and pro-inflammatory effects of molybdenum and tungsten disulphide on human bronchial cells
  51. Improving recycled aggregate concrete by compression casting and nano-silica
  52. Chemically reactive Maxwell nanoliquid flow by a stretching surface in the frames of Newtonian heating, nonlinear convection and radiative flux: Nanopolymer flow processing simulation
  53. Nonlinear dynamic and crack behaviors of carbon nanotubes-reinforced composites with various geometries
  54. Biosynthesis of copper oxide nanoparticles and its therapeutic efficacy against colon cancer
  55. Synthesis and characterization of smart stimuli-responsive herbal drug-encapsulated nanoniosome particles for efficient treatment of breast cancer
  56. Homotopic simulation for heat transport phenomenon of the Burgers nanofluids flow over a stretching cylinder with thermal convective and zero mass flux conditions
  57. Incorporation of copper and strontium ions in TiO2 nanotubes via dopamine to enhance hemocompatibility and cytocompatibility
  58. Mechanical, thermal, and barrier properties of starch films incorporated with chitosan nanoparticles
  59. Mechanical properties and microstructure of nano-strengthened recycled aggregate concrete
  60. Glucose-responsive nanogels efficiently maintain the stability and activity of therapeutic enzymes
  61. Tunning matrix rheology and mechanical performance of ultra-high performance concrete using cellulose nanofibers
  62. Flexible MXene/copper/cellulose nanofiber heat spreader films with enhanced thermal conductivity
  63. Promoted charge separation and specific surface area via interlacing of N-doped titanium dioxide nanotubes on carbon nitride nanosheets for photocatalytic degradation of Rhodamine B
  64. Elucidating the role of silicon dioxide and titanium dioxide nanoparticles in mitigating the disease of the eggplant caused by Phomopsis vexans, Ralstonia solanacearum, and root-knot nematode Meloidogyne incognita
  65. An implication of magnetic dipole in Carreau Yasuda liquid influenced by engine oil using ternary hybrid nanomaterial
  66. Robust synthesis of a composite phase of copper vanadium oxide with enhanced performance for durable aqueous Zn-ion batteries
  67. Tunning self-assembled phases of bovine serum albumin via hydrothermal process to synthesize novel functional hydrogel for skin protection against UVB
  68. A comparative experimental study on damping properties of epoxy nanocomposite beams reinforced with carbon nanotubes and graphene nanoplatelets
  69. Lightweight and hydrophobic Ni/GO/PVA composite aerogels for ultrahigh performance electromagnetic interference shielding
  70. Research on the auxetic behavior and mechanical properties of periodically rotating graphene nanostructures
  71. Repairing performances of novel cement mortar modified with graphene oxide and polyacrylate polymer
  72. Closed-loop recycling and fabrication of hydrophilic CNT films with high performance
  73. Design of thin-film configuration of SnO2–Ag2O composites for NO2 gas-sensing applications
  74. Study on stress distribution of SiC/Al composites based on microstructure models with microns and nanoparticles
  75. PVDF green nanofibers as potential carriers for improving self-healing and mechanical properties of carbon fiber/epoxy prepregs
  76. Osteogenesis capability of three-dimensionally printed poly(lactic acid)-halloysite nanotube scaffolds containing strontium ranelate
  77. Silver nanoparticles induce mitochondria-dependent apoptosis and late non-canonical autophagy in HT-29 colon cancer cells
  78. Preparation and bonding mechanisms of polymer/metal hybrid composite by nano molding technology
  79. Damage self-sensing and strain monitoring of glass-reinforced epoxy composite impregnated with graphene nanoplatelet and multiwalled carbon nanotubes
  80. Thermal analysis characterisation of solar-powered ship using Oldroyd hybrid nanofluids in parabolic trough solar collector: An optimal thermal application
  81. Pyrene-functionalized halloysite nanotubes for simultaneously detecting and separating Hg(ii) in aqueous media: A comprehensive comparison on interparticle and intraparticle excimers
  82. Fabrication of self-assembly CNT flexible film and its piezoresistive sensing behaviors
  83. Thermal valuation and entropy inspection of second-grade nanoscale fluid flow over a stretching surface by applying Koo–Kleinstreuer–Li relation
  84. Mechanical properties and microstructure of nano-SiO2 and basalt-fiber-reinforced recycled aggregate concrete
  85. Characterization and tribology performance of polyaniline-coated nanodiamond lubricant additives
  86. Combined impact of Marangoni convection and thermophoretic particle deposition on chemically reactive transport of nanofluid flow over a stretching surface
  87. Spark plasma extrusion of binder free hydroxyapatite powder
  88. An investigation on thermo-mechanical performance of graphene-oxide-reinforced shape memory polymer
  89. Effect of nanoadditives on the novel leather fiber/recycled poly(ethylene-vinyl-acetate) polymer composites for multifunctional applications: Fabrication, characterizations, and multiobjective optimization using central composite design
  90. Design selection for a hemispherical dimple core sandwich panel using hybrid multi-criteria decision-making methods
  91. Improving tensile strength and impact toughness of plasticized poly(lactic acid) biocomposites by incorporating nanofibrillated cellulose
  92. Green synthesis of spinel copper ferrite (CuFe2O4) nanoparticles and their toxicity
  93. The effect of TaC and NbC hybrid and mono-nanoparticles on AA2024 nanocomposites: Microstructure, strengthening, and artificial aging
  94. Excited-state geometry relaxation of pyrene-modified cellulose nanocrystals under UV-light excitation for detecting Fe3+
  95. Effect of CNTs and MEA on the creep of face-slab concrete at an early age
  96. Effect of deformation conditions on compression phase transformation of AZ31
  97. Application of MXene as a new generation of highly conductive coating materials for electromembrane-surrounded solid-phase microextraction
  98. A comparative study of the elasto-plastic properties for ceramic nanocomposites filled by graphene or graphene oxide nanoplates
  99. Encapsulation strategies for improving the biological behavior of CdS@ZIF-8 nanocomposites
  100. Biosynthesis of ZnO NPs from pumpkin seeds’ extract and elucidation of its anticancer potential against breast cancer
  101. Preliminary trials of the gold nanoparticles conjugated chrysin: An assessment of anti-oxidant, anti-microbial, and in vitro cytotoxic activities of a nanoformulated flavonoid
  102. Effect of micron-scale pores increased by nano-SiO2 sol modification on the strength of cement mortar
  103. Fractional simulations for thermal flow of hybrid nanofluid with aluminum oxide and titanium oxide nanoparticles with water and blood base fluids
  104. The effect of graphene nano-powder on the viscosity of water: An experimental study and artificial neural network modeling
  105. Development of a novel heat- and shear-resistant nano-silica gelling agent
  106. Characterization, biocompatibility and in vivo of nominal MnO2-containing wollastonite glass-ceramic
  107. Entropy production simulation of second-grade magnetic nanomaterials flowing across an expanding surface with viscidness dissipative flux
  108. Enhancement in structural, morphological, and optical properties of copper oxide for optoelectronic device applications
  109. Aptamer-functionalized chitosan-coated gold nanoparticle complex as a suitable targeted drug carrier for improved breast cancer treatment
  110. Performance and overall evaluation of nano-alumina-modified asphalt mixture
  111. Analysis of pure nanofluid (GO/engine oil) and hybrid nanofluid (GO–Fe3O4/engine oil): Novel thermal and magnetic features
  112. Synthesis of Ag@AgCl modified anatase/rutile/brookite mixed phase TiO2 and their photocatalytic property
  113. Mechanisms and influential variables on the abrasion resistance hydraulic concrete
  114. Synergistic reinforcement mechanism of basalt fiber/cellulose nanocrystals/polypropylene composites
  115. Achieving excellent oxidation resistance and mechanical properties of TiB2–B4C/carbon aerogel composites by quick-gelation and mechanical mixing
  116. Microwave-assisted sol–gel template-free synthesis and characterization of silica nanoparticles obtained from South African coal fly ash
  117. Pulsed laser-assisted synthesis of nano nickel(ii) oxide-anchored graphitic carbon nitride: Characterizations and their potential antibacterial/anti-biofilm applications
  118. Effects of nano-ZrSi2 on thermal stability of phenolic resin and thermal reusability of quartz–phenolic composites
  119. Benzaldehyde derivatives on tin electroplating as corrosion resistance for fabricating copper circuit
  120. Mechanical and heat transfer properties of 4D-printed shape memory graphene oxide/epoxy acrylate composites
  121. Coupling the vanadium-induced amorphous/crystalline NiFe2O4 with phosphide heterojunction toward active oxygen evolution reaction catalysts
  122. Graphene-oxide-reinforced cement composites mechanical and microstructural characteristics at elevated temperatures
  123. Gray correlation analysis of factors influencing compressive strength and durability of nano-SiO2 and PVA fiber reinforced geopolymer mortar
  124. Preparation of layered gradient Cu–Cr–Ti alloy with excellent mechanical properties, thermal stability, and electrical conductivity
  125. Recovery of Cr from chrome-containing leather wastes to develop aluminum-based composite material along with Al2O3 ceramic particles: An ingenious approach
  126. Mechanisms of the improved stiffness of flexible polymers under impact loading
  127. Anticancer potential of gold nanoparticles (AuNPs) using a battery of in vitro tests
  128. Review Articles
  129. Proposed approaches for coronaviruses elimination from wastewater: Membrane techniques and nanotechnology solutions
  130. Application of Pickering emulsion in oil drilling and production
  131. The contribution of microfluidics to the fight against tuberculosis
  132. Graphene-based biosensors for disease theranostics: Development, applications, and recent advancements
  133. Synthesis and encapsulation of iron oxide nanorods for application in magnetic hyperthermia and photothermal therapy
  134. Contemporary nano-architectured drugs and leads for ανβ3 integrin-based chemotherapy: Rationale and retrospect
  135. State-of-the-art review of fabrication, application, and mechanical properties of functionally graded porous nanocomposite materials
  136. Insights on magnetic spinel ferrites for targeted drug delivery and hyperthermia applications
  137. A review on heterogeneous oxidation of acetaminophen based on micro and nanoparticles catalyzed by different activators
  138. Early diagnosis of lung cancer using magnetic nanoparticles-integrated systems
  139. Advances in ZnO: Manipulation of defects for enhancing their technological potentials
  140. Efficacious nanomedicine track toward combating COVID-19
  141. A review of the design, processes, and properties of Mg-based composites
  142. Green synthesis of nanoparticles for varied applications: Green renewable resources and energy-efficient synthetic routes
  143. Two-dimensional nanomaterial-based polymer composites: Fundamentals and applications
  144. Recent progress and challenges in plasmonic nanomaterials
  145. Apoptotic cell-derived micro/nanosized extracellular vesicles in tissue regeneration
  146. Electronic noses based on metal oxide nanowires: A review
  147. Framework materials for supercapacitors
  148. An overview on the reproductive toxicity of graphene derivatives: Highlighting the importance
  149. Antibacterial nanomaterials: Upcoming hope to overcome antibiotic resistance crisis
  150. Research progress of carbon materials in the field of three-dimensional printing polymer nanocomposites
  151. A review of atomic layer deposition modelling and simulation methodologies: Density functional theory and molecular dynamics
  152. Recent advances in the preparation of PVDF-based piezoelectric materials
  153. Recent developments in tensile properties of friction welding of carbon fiber-reinforced composite: A review
  154. Comprehensive review of the properties of fly ash-based geopolymer with additive of nano-SiO2
  155. Perspectives in biopolymer/graphene-based composite application: Advances, challenges, and recommendations
  156. Graphene-based nanocomposite using new modeling molecular dynamic simulations for proposed neutralizing mechanism and real-time sensing of COVID-19
  157. Nanotechnology application on bamboo materials: A review
  158. Recent developments and future perspectives of biorenewable nanocomposites for advanced applications
  159. Nanostructured lipid carrier system: A compendium of their formulation development approaches, optimization strategies by quality by design, and recent applications in drug delivery
  160. 3D printing customized design of human bone tissue implant and its application
  161. Design, preparation, and functionalization of nanobiomaterials for enhanced efficacy in current and future biomedical applications
  162. A brief review of nanoparticles-doped PEDOT:PSS nanocomposite for OLED and OPV
  163. Nanotechnology interventions as a putative tool for the treatment of dental afflictions
  164. Recent advancements in metal–organic frameworks integrating quantum dots (QDs@MOF) and their potential applications
  165. A focused review of short electrospun nanofiber preparation techniques for composite reinforcement
  166. Microstructural characteristics and nano-modification of interfacial transition zone in concrete: A review
  167. Latest developments in the upconversion nanotechnology for the rapid detection of food safety: A review
  168. Strategic applications of nano-fertilizers for sustainable agriculture: Benefits and bottlenecks
  169. Molecular dynamics application of cocrystal energetic materials: A review
  170. Synthesis and application of nanometer hydroxyapatite in biomedicine
  171. Cutting-edge development in waste-recycled nanomaterials for energy storage and conversion applications
  172. Biological applications of ternary quantum dots: A review
  173. Nanotherapeutics for hydrogen sulfide-involved treatment: An emerging approach for cancer therapy
  174. Application of antibacterial nanoparticles in orthodontic materials
  175. Effect of natural-based biological hydrogels combined with growth factors on skin wound healing
  176. Nanozymes – A route to overcome microbial resistance: A viewpoint
  177. Recent developments and applications of smart nanoparticles in biomedicine
  178. Contemporary review on carbon nanotube (CNT) composites and their impact on multifarious applications
  179. Interfacial interactions and reinforcing mechanisms of cellulose and chitin nanomaterials and starch derivatives for cement and concrete strength and durability enhancement: A review
  180. Diamond-like carbon films for tribological modification of rubber
  181. Layered double hydroxides (LDHs) modified cement-based materials: A systematic review
  182. Recent research progress and advanced applications of silica/polymer nanocomposites
  183. Modeling of supramolecular biopolymers: Leading the in silico revolution of tissue engineering and nanomedicine
  184. Recent advances in perovskites-based optoelectronics
  185. Biogenic synthesis of palladium nanoparticles: New production methods and applications
  186. A comprehensive review of nanofluids with fractional derivatives: Modeling and application
  187. Electrospinning of marine polysaccharides: Processing and chemical aspects, challenges, and future prospects
  188. Electrohydrodynamic printing for demanding devices: A review of processing and applications
  189. Rapid Communications
  190. Structural material with designed thermal twist for a simple actuation
  191. Recent advances in photothermal materials for solar-driven crude oil adsorption
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