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Preparation of Carbon Fiber Reinforced Boron Nitride Composite Ceramics by using Phase Transformation Assisted Sintering Technology
Journal of Ceramics 2025, 46(4): 777-785
Published: 01 August 2025
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Background and purposes

Hexagonal boron nitride (h-BN) ceramics exhibit outstanding high-temperature stability, corrosion resistance, electrical insulation and self-lubricating properties, making them highly promising for applications in aerospace, electronics, metallurgy and mechanical manufacturing. However, due to their strong covalent bonding and low self-diffusion coefficient, achieving full densification remains challenging, even under high-temperature or pressure-assisted sintering conditions. A common approach to improve the densification involves the addition of sintering aids, such as B2O3. However, the incorporation of sintering additives can degrade high-temperature performance of the ceramics and should therefore be avoided. Cubic boron nitride (c-BN), a polymorphic form of h-BN, has crystal structure and lattice constant similar to those of diamond. Under ambient pressure conditions, c-BN can transform into h-BN. Since c-BN has a higher density than h-BN, this phase transition results in volumetric expansion, which can fill the voids between h-BN platelets. Utilizing phase transformation-assisted sintering, highly dense ceramics with a relative density of up to 97.6% can be obtained. Nevertheless, the mechanical properties of monolithic h-BN ceramics remain relatively low, limiting their practical applications. Incorporating a secondary phase is an effective strategy for enhancing the strength and toughness of ceramic materials. Carbon fibers, known for their low density, high tensile modulus and strength, low thermal expansion coefficient and excellent thermal conductivity, are widely used as one-dimensional reinforcement materials in ceramic, metal and polymer composites. In this study, carbon fibers were employed as the secondary phase to fabricate high-performance composite ceramics, aiming to advance BN ceramic processing technology and broaden its practical applications.

Methods

BN powder (consisting of 80% hexagonal boron nitride and 20% cubic boron nitride) and carbon fibers were used as raw materials. The BN and carbon fiber powders were precisely weighed, mixed, stirred and dried through rotary evaporation. The prepared powder was then sintered using spark plasma sintering (SPS). The heating rate was 100 ℃·min-1 and the temperature was held at 1700 ℃ for 5 min to obtain CF/BN composite ceramics. Phase composition and its evolution during heat treatment were analyzed using X-ray diffraction (XRD). Bulk density of the samples was measured using the Archimedes method. A universal testing machine was used to evaluate flexural properties and stress-strain behavior of the BN ceramics containing 3%, 5%, 10% and 15% carbon fiber with different fiber mesh sizes. A nanoindentation system was employed to measure elastic modulus and microhardness of the composite ceramics. The morphology of the carbon fiber powders and the fracture surfaces of the composite ceramics were examined using scanning electron microscopy (SEM).

Results

As the carbon fiber content was increased, relative density and flexural strength of the composite ceramics initially increased and then decreased. The optimal performance was achieved at a carbon fiber content of 5%, with a flexural strength of 130.5 MPa. Additionally, its fracture strain reached 1.1%, more than twice that of the sample without carbon fiber. However, with increasing carbon fiber content, both Young’s modulus and microhardness exhibited a decreasing trend. With 3% carbon fiber, the average Young’s modulus reached 30.09 GPa, while the microhardness was 0.43 GPa. As the fiber mesh size increased, relative density and flexural strength of the composite ceramics decreased, with the optimal performance observed at a fiber mesh size of 300. Conversely, Young’s modulus and microhardness increased significantly with increasing fiber mesh size, reaching 30.18 GPa and 0.49 GPa, respectively, at a mesh size of 800. Controlling the carbon fiber content within an appropriate range is critical for maximizing the composite material’s mechanical performance. When the carbon fiber content is too low, the reinforcement effect is insufficient, whereas excessive fiber content leads to agglomeration and overlapping, diminishing the strengthening effect. Additionally, fiber size plays a crucial role in mechanical performance. Larger carbon fibers interlock with multiple BN platelets, enhancing mechanical interlocking and stress transfer, thereby improving flexural properties. Conversely, smaller carbon fibers exhibit better dispersion within the matrix, which enhances material uniformity. This uniform dispersion effectively distributes and absorbs externally applied stress, leading to improvements in Young’s modulus and hardness.

Conclusions

CF/BN composite ceramics were successfully fabricated at a relatively low sintering temperature of 1700 ℃ using phase transformation-assisted sintering, with carbon fibers as the reinforcing phase. The effects of carbon fiber content and fiber size on microstructure and mechanical properties of the composite ceramics were systematically studied. Comprehensive characterization via XRD, SEM and mechanical testing provided insights into the influence of carbon fiber parameters on phase composition, morphology and mechanical performance of the CF/BN composites, establishing correlations between fiber content, fiber size and the resulting properties. The findings indicate that the optimal composition for CF/BN composite ceramics is 5% carbon fiber with a fiber mesh size of 300, achieving a relative density of 95.6% and a flexural strength of 130.5 MPa. Additionally, the fracture strain reached 1.1%, more than twice that of samples without carbon fiber. The incorporation of carbon fibers significantly enhanced both the strength and toughness of BN ceramics, which holds substantial promise for their practical applications.

Issue
Design and Performance Regulation of MOFs-derived Carbon Composites for Electromagnetic Wave Absorption
Journal of Ceramics 2023, 44(4): 651-661
Published: 01 August 2023
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It is of great significance to develop lightweight and efficient electromagnetic wave (EMW) absorption materials to counter the problems of electromagnetic interference, information security and national defense security. In recent years,nanoporous carbon composites derived from metal-organic frameworks (MOFs) have gained numerous attentions in the field of EMW absorption. Benefited from the highly adjustable pore structures and the tailored components and microstructures of MOFs, the in-situ generated metallic microwave absorption units in carbon matrix result in rich interfaces as well as compositions. Together with the cross-linked conductive network, the microwave loss mechanisms can be greatly enriched,leading to enhanced EMW absorption capability. The rational design of various components and the controllable construction of microstructures are the key to regulate the electromagnetic parameters. The rational design and performance regulation strategy of MOFs-derived carbon-based EMW absorbers in recent years are reviewed regarding incorporated metal types and spatial arrangement, heterogeneous structure of MOFs and porous structure of carbon matrix. Finally, the challenges and perspectives of MOFs-derived carbon composites in the application of EMW absorption are also presented.

Issue
Construction and Electromagnetic Wave Absorption Properties of MXene Modified Conductive MOF Composites
Journal of Ceramics 2024, 45(4): 739-749
Published: 01 August 2024
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With the popularization of high-frequency communication technology, the problem of electromagnetic radiation has received increasing attention. The construction of novel electromagnetic wave (EMW) absorption materials based on conductive metal-organic frameworks (MOFs) has become a research hotspot in recent years. In this work, MXene modified MOF/polypyrrole (PPy) was proposed, with which high-performance EMW absorption materials with broadband and strong absorption were successfully obtained through the cooperative optimization of dielectric loss of the three components. When the filling content is only 10 wt.%, the minimum reflection loss (RLmin) of the composites can reach -56.21 dB at a thin thickness of 1.98 mm, while the maximum effective absorption bandwidth (EAB) can be up to 7.12 GHz (10.88-18.00 GHz), which is superior to the conductive MOF-based microwave absorbers reported in the open literture. By analyzing the components and microstructure of the materials, it is found that the excess PPy is not only polymerized in-situ in the pores and outer surface of UiO-66, but also loaded on the MXene substrate, which effectively builds up conductive network and promotes the conductive loss. Meanwhile, the ternary heterogeneous interface composed of UiO-66, PPy and MXene greatly enhanced the interfacial polarization loss, which further promoted the attenuation of electromagnetic waves. In addition, the simple preparation process and high yield of MXene/UiO-66/PPy have strong potential for large-scale production, which is promising to be applied in the field of electromagnetic protection.

Open Access Research Article Issue
Sintering and mechanical properties of carbon bulks from ordered mesoporous carbon and nano diamond
Journal of Advanced Ceramics 2022, 11(11): 1815-1823
Published: 26 October 2022
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Powder metallurgy is important in material preparation. Due to the inertness of carbon materials, however, sintering powdered carbon into physically coherent bulks has been a great challenge even at a high temperature (2000 ℃). Improving the sintering activity of carbon powders is the key to the success of the consolidation of the carbon powders. Here ordered mesoporous carbon (OMC) is used as the starting material to produce highly homogeneous novel carbon bulks. During sintering at 1800 ℃, the huge specific surface area of the OMC greatly promotes the migration of carbon atoms and thus the sintering of the OMC by surface diffusion mechanism. When nanodiamond (ND) is added, the volume expansion associated with the phase transformation of diamond to graphite facilitates the densification of the powder compacts. The strong connection between the OMC and the graphite onions derived from the ND bestows the as-prepared carbon bulks with excellent mechanical properties. The current research pioneers a novel way to prepare high-strength carbon materials at relatively low temperatures.

Open Access Research paper Issue
Mechanically exfoliated MoS2 nanoflakes for optimizing the thermoelectric performance of SrTiO3-based ceramic composites
Journal of Materiomics 2022, 8(4): 790-798
Published: 12 February 2022
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As a semiconducting material with relatively low thermal conductivity, MoS2 nanoflake has the potential to serve as a modulator for optimizing the performance of thermoelectric (TE) materials. However, the low yield of MoS2 nanoflakes prepared by conventional methods has constrained the development of MoS2 optimized TE materials. We propose a mechanical exfoliation method for mass production of MoS2 nanoflakes using attrition mill. After mixed with La and Nb co-doped SrTiO3 (SLNT) powder, the MoS2/SLNT composites are fabricated by spark plasma sintering. It is found that the heterojunctions formed at MoS2/SLNT interfaces with proper band offset can effectively scatter the low-energy electrons, resulting in enhanced Seebeck coefficient without significantly undermining the electrical conductivity. The power factor of composites is improved when the MoS2 content is lower than 1.5 vol%. Meanwhile, the thermal conductivity of composites is significantly decreased due to the phonon scattering induced large thermal resistance at MoS2/SLNT interfaces, which is much higher than that in graphene embedded SrTiO3 composites. Consequently, a maximum ZT = 0.24 is obtained at 800 K in 1.5 vol% MoS2/SLNT composite, which is ~26 % higher compared with pristine matrix. This work paves the way for application of TE materials modulated by transition metal dichalcogenides.

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