MXene-derived TiB2 formation in B4C at high temperatures
摘要
Two-dimensional (2D) MXenes are nanometer-thick sheets of transition metal carbides, nitrides, or carbonitrides with high-temperature capabilities. MXenes can be used as nanofillers and functional additives in ceramic hybrids, enhancing sintering and mechanical and electrical properties. In this study, we systematically investigate the incorporation of titanium carbide (Ti3C2Tx) MXene into micron-sized (~ 6 μm) boron carbide (B4C) using a one-step electrostatic self-assembly method. We tuned the zeta potential of B4C and Ti3C2Tx MXene solutions, gradually added B4C into the MXene solution, and prepared green bodies with 1 to 10 vol.% Ti3C2Tx. We examined MXene phase stability, reactions, and phase transformation in B4C via direct current spark plasma sintering at 1925 °C with a pressure of 70 MPa in a vacuum. To understand the reaction pathways, we conducted stepwise sintering from 800 °C to 1800 °C in 200 °C increments. X-ray diffraction and scanning electron microscopy results revealed that Ti3C2Tx reacts with B4C at ~ 1200 °C to form TiB2, with complete conversion at 1800 °C, resulting in a TiB2-B4C structure. For samples with 4 vol.% MXene or higher, B2O3 formed above 1200 °C due to MXene oxygen terminations and disappeared above 1800 °C. The overall oxygen content in MXene-containing samples was lower than in B4C sintered without MXene, indicating its reducing nature as a 2D carbide. MXene also acts as a sintering additive and the relative density was increased by increasing the MXene content, achieving 99% with 10 vol.% MXene. The measured hardness values were 20 ± 1.6 GPa and 41 ± 0.8 GPa for B4C and B4C with 10 vol.% MXene Ti3C2 samples, respectively. This trend indicates that increasing Ti3C2Tx MXene content (1–10 vol.%) in the B4C matrix enhances hardness due to the formation of TiB2 phases, which improves densification and reinforces the B4C matrix. Compared to traditional bulk TiC, 2D MXene sheets provide a larger surface area and uniform coverage of B4C particles, lowering diffusion energy and enhancing sintering rates. This study demonstrates a new approach to using MXene as a nanometer-thick additive to form uniformly distributed TiB2 in B4C to enhance its structural properties.