Carbide Ceramics Research Articles

High-entropy carbide (ZrNbTiCrV)C ceramic composite coating possessing good mechanical properties and wear resistance

High entropy carbide ceramics possess high hardness but suffer from low toughness and densification challenges. A dense (ZrNbTiCrV)C composite coating was fabricated through spraying ZrO2-Nb2O5-TiO2-Cr2O3-V2O5-Al-SiC powders, which was subsequently compared to a (ZrNbTiCrV)C coating produced from binary carbides. Incorporating the V element facilitated the densification and element diffusion. The coating obtained via spraying ZrO2-Nb2O5-TiO2-Cr2O3-V2O5-Al-SiC powders exhibited superior mechanical properties and wear resistance, particularly achieving a 17.2 % increase in fracture toughness and a 73.3 % reduction in wear rate compared to the coating derived from binary carbides. These improved properties were attributed to fine-grained particles and a low porosity of 1.56 %. Wear resistance was also enhanced through rolling friction and the formation of a protective oxide film.

Thermal and electrical properties of single‐phase high entropy carbide ceramics

AbstractThermal and electrical properties were investigated for five nominally phase‐pure high entropy carbide ceramics. The compositions (Hf0.2Nb0.2Ta0.2Ti0.2Zr0.2)C, (Cr0.2Hf0.2Ta0.2Ti0.2Zr0.2)C, (Hf0.2Mo0.2Ta0.2Ti0.2Zr0.2)C, (Hf0.2Ta0.2Ti0.2W0.2Zr0.2)C, and (Hf0.2Mo0.2Ti0.2W0.2Zr0.2)C were synthesized by carbothermal reduction of oxides. The thermal diffusivity and heat capacity were measured from room temperature to 1800°C. The room temperature thermal conductivity ranged from 5.1 W/mK for (Hf0.2Mo0.2Ti0.2W0.2Zr0.2)C to 9.0 W/mK for (Cr0.2Hf0.2Ta0.2Ti0.2Zr0.2)C. The thermal conductivity increased over the temperature range with maximum conductivities of 19.6 W/mK measured for (Hf0.2Mo0.2Ta0.2Ti0.2Zr0.2)C to 29.7 W/mK for (Cr0.2Hf0.2Ta0.2Ti0.2Zr0.2)C at 1800°C. The electron contribution to thermal conductivity calculated from measured electrical resistivity varied from 41% to 52% of the total thermal conductivity. The tungsten and molybdenum containing compositions had higher phonon contributions while the niobium and chromium containing compositions had nearly equal electron and phonon contributions to thermal conductivity.

Microstructure and Properties of Pressureless-Sintered Zirconium Carbide Ceramics with MoSi2 Addition.

Zirconium carbide (ZrC) ceramics have a high melting point, low neutron absorption cross section, and excellent resistance to the impact of fission products and are considered to be one of the best candidate materials for fourth-generation nuclear energy systems. ZrC ceramics with a high relative density of 99.1% were successfully prepared via pressureless sintering using a small amount of MoSi2 as an additive. The influence of the MoSi2 content on the densification behavior, microstructure, mechanical properties, and thermal properties of ZrC ceramics was systematically investigated. The results show that the densification of ZrC was significantly enhanced by the introduction of MoSi2 due to the formation of a liquid phase during sintering. In addition, the ZrC grains were refined due to the pinning effect of the generated silicon carbide. The flexural strength and Vickers hardness of ZrC ceramics with 2.5 vol% MoSi2 sintered at 1850 °C were 408 ± 12 MPa and 17.1 GPa, respectively, which were approximately 30% and 10% higher compared to the samples without the addition of MoSi2. The improved mechanical properties were mainly attributed to the high relative density (99.1%) and refined microstructure.

Warm Pressing of Organosilicon Polymer Toward Monolithic Ceramics

Warm pressing of organosilicon polymers is often challenging due to the formation of cracks due to release of volatile compounds during the warm pressing process. The focus of the present study is to warm press crosslinked SMP‐10 powders into crack‐free compacts and to pyrolyze them to get bulk SiC monoliths. Crack formation during warm pressing is addressed by optimizing the crosslinking temperature, and the loss of formability of the powders crosslinked at higher temperatures is overcome with the use of uncured polymer as a binder. The crosslinking temperature of the preceramic polymer plays a crucial role in developing crack‐free green bodies. The amount of binder used is varied to study its effect on the bulk density of the pyrolyzed product. The warm pressed green bodies pyrolyzed at 1400 °C result in the formation of bulk silicon carbide ceramics and are characterized using X‐ray diffractometer and FTIR spectroscopy. Warm pressing is performed at a lower temperature than reported in the literature, and this limits the incorporation of oxygen during the warm pressing.

Preparation of zirconium carbide ceramic with good mechanical properties via gel-casting and pressureless sintering

In this study, high-performance zirconium carbide (ZrC) ceramics prepared by gel-casting method were reported for the first time. A water-based slurry with 40 vol% solids was prepared using TMAH and PVP as dispersants, and the resulting green body had a flexural strength of 21.11 ± 1.84 MPa after curing, which was sufficient for machining. Dense ZrC ceramics (relative density >97 %) were obtained by sintering at 2000 °C under atmospheric pressure, and a 387 ± 23.21 MPa flexural strength and 15.48 ± 0.28 GPa hardness were achieved. This study offers a new strategy for preparing ZrC ceramics with complex structures.

Microstructure, mechanical, and thermal properties of (MoTaTiVW)CX high entropy ceramics with different carbon stoichiometries

In present work, high entropy (MoTaTiVW)CX ceramics with different carbon stoichiometries (X = 3–6) were produced using spark plasma sintering. The microstructure, mechanical properties, and thermal properties of (MoTaTiVW)CX with different carbon stoichiometries were studied. At X = 3, the carbon deficiency resulted in a multiphase structure of the sample, (MoTaTiVW)C3 with a Mo-rich carbide phase. At X = 3.5, the single-phase rock salt structure was formed despite carbon vacancies of up to 30 %. The relative density of (MoTaTiVW)CX gradually decreases as the carbon stoichiometry increases from X = 3 to X = 6. The concentration of carbon vacancies affects the sintering activation energy, which can enhance mass transfer and promote the densification process. The Vickers hardness of (MoTaTiVW)CX shows an overall decreasing trend as the carbon stoichiometry increases from X = 3.5 to X = 6, peaking at 20.4 ± 0.4 GPa at X = 3.5. The fracture toughness increases and then decreases, peaking at 4.4 ± 0.2 MPa m1/2 at X = 4. The thermal conductivity of (MoTaTiVW)CX gradually increases, then decreases and finally increases with the increase of carbon stoichiometry. At room temperature, the maximum value of thermal conductivity is 6.35 ± 0.29 W/m·K of (MoTaTiVW)C5 and the minimum value is 5.32 ± 0.35 W/m·K of (MoTaTiVW)C5.5. At 1000 °C, the thermal conductivity of (MoTaTiVW)CX ranges from 15.94 ± 0.37 W/m·K to 19.56 ± 0.45 W/m·K. As the concentration of carbon vacancies decreases, the decrease in point defect concentration will reduce the degree of lattice distortion, thereby reducing phonon scattering and affecting thermal conductivity. The study suggests that carbon stoichiometry can be used to adjust the microstructure, mechanical properties, and thermal properties of high entropy carbide ceramics.

Silicon carbide ceramics formed by binder jetting: A study focusing on the printing layer thickness and the PIP densification process

Binder jetting (BJ) additive manufacturing has the advantages of high precision, fast forming speed, and no need for supporting structure, which is especially suitable for the forming of metallic and ceramic components with complex structures. In this paper, SiC ceramic parts were obtained by BJ additive manufacturing and precursor impregnation pyrolysis (PIP) cycles. It has been observed that the thickness of the printing layer significantly affects the strength of the SiC green body. The SiC green body exhibited the highest bending strength (3.1 ± 0.2 MPa) and lower dimensional deviation (0.47–1.64 %) when printed with a layer thickness of 50 μm. However, the bending strength of the SiC ceramics (after densification) had little variations when different printing layer thicknesses were utilized. In the subsequent densification process, the density, hardness, and bending strength of SiC ceramics increase as the number of PIP cycles increases obviously, and the flexural strength reached 228.7 ± 14.2 MPa after 9 PIP cycles, while the shrinkage rates in the X, Y, and Z direction were 1.9 %, 2.8 %, and 1.2 %, respectively. In addition, the influence mechanism of printing parameters on the strengths of the green bodies and SiC ceramics was also discussed. Specifically, it was found that with the layer thickness increase, the strengths of SiC ceramics also increase.

Hardness of single phase high entropy carbide ceramics with different compositions

Five high entropy carbide ceramics, (Hf0.2,Nb0.2,Ta0.2,Ti0.2,Zr0.2)C, (Cr0.2,Hf0.2,Ta0.2,Ti0.2,Zr0.2)C, (Hf0.2,Mo0.2,Ta0.2,Ti0.2,Zr0.2)C, (Hf0.2,Ta0.2,Ti0.2,W0.2,Zr0.2)C, and (Hf0.2,Mo0.2,Ti0.2,W0.2,Zr0.2)C, were synthesized by carbothermal reduction of oxides and direct current sintering. The five high entropy carbide ceramics were determined to be nominally phase-pure with relative densities of more than 98.9% and mean grain sizes of less than 5 μm. Average Vickers hardness values ranged from 19.2 ± 0.4 GPa for (Hf0.2,Nb0.2,Ta0.2,Ti0.2,Zr0.2)C at a load of 2 kgf to 43.5 ± 0.4 GPa for (Hf0.2,Mo0.2,Ti0.2,W0.2,Zr0.2)C at a load of 0.05 kgf. Hardness generally increased with increasing the valence electron concentration and strain as measured by the Williamson–Hall analysis. However, neither correlation was conclusive enough to be a clear indicator of hardness. Instead, it was determined that a combination of effects that includes the valence electron concentration, lattice strain, and grain size all contribute to the hardness of high entropy carbide ceramics.

Phase composition, structure and properties of B<sub>4</sub>C–TiB<sub>2</sub> ceramics produced by hot pressing

Composite ceramic materials based on B4C with the addition of TiB2 in amounts of 0, 10, 20, 25 and 30 mol. % have been studied. Titanium diboride was synthesized from TiO2 powder and nanofibrous carbon using the boron carbide method in an induction furnace at 1650 °C in an argon atmosphere. The samples were produced by hot pressing at 2100 °C and 25 MPa in an argon environment. The phase composition was determined, and the apparent density and open porosity of the experimental materials were measured. The microstructure was assessed using optical and scanning electron microscopy. The investigations revealed that an increase in the TiB2 content reduces the open porosity while concurrently enhancing the relative density of the boron carbide ceramics. For a sample containing 30 mol. % TiB2 , the open porosity and relative theoretical density were 1.6 and 99 %, respectively. Using XRD and XRS analyses established that the synthesized materials are comprised of two phases: B4C and TiB2 . The average grain size of TiB2 was 0.85 ± 0.02 µm for the sample with 10 mol. % TiB2 and 8.90 ± 0.25 µm for the material with 30 mol. % TiB2 . It was found that at higher TiB2 concentrations, large clusters of grains are formed. The destruction pattern of B4C grains is intragranular, while TiB2 grains are characterized by intergranular destruction. For a sample containing 30 mol. % TiB2 , the fracture toughness was 4.97 ± 0.23 MPa∙m0.5, and the hardness was 3320 ± 120 HV0.5 . Therefore, the addition of TiB2 at these specified concentrations facilitated a 30 % enhancement in fracture toughness relative to single-phase B4C while preserving a high level of hardness.

First-principles study on the structure, mechanical and thermodynamic properties of (Ti, Hf, Nb, Ta)C high-entropy carbide ceramics

High-entropy carbide ceramics (HECCs) have demonstrated extraordinary properties and broad application potential. However, the action mechanisms of metallic elements on the properties have not been understood in depth. In this study, the structural stability and the mechanical and thermodynamic properties of (Ti, Hf, Nb, Ta)C HECCs across a broad composition spectrum were systematically analyzed based on the density functional theory and Debye–Grüneisen model. The crystal structure was constructed and validated through experimental testing. The mechanical properties such as elastic moduli, ductility, hardness, and Poisson's and Pugh's ratios were calculated. Furthermore, the temperature dependence of bulk moduli, thermal expansion coefficients, and heat capacities of the HECCs were investigated. To interpret the elastic and toughening mechanisms of non-equiatomic HECCs, the electronic structures were investigated. The results indicate that the HECCs with a single solid solution phase of the FCC rock-salt structure are thermodynamically stable. The HECCs containing higher Nb and Ta contents have greater strength and stiffness, and those containing higher Ti and Hf contents exhibit greater hardness and brittleness than the equiatomic HECC. In addition, non-equiatomic HECCs containing higher Nb and Ta contents have larger bulk moduli and lower linear thermal expansion coefficients, which can be attributed to the stronger covalent interaction among metallic elements and carbon. This study is expected to have an impact on designing ideal HECCs for high-temperature applications under extreme environments.

Effect of the Carbon Component on the Strength of Reaction-Sintered Silicon–Carbide Ceramics

Effect of the Carbon Component on the Strength of Reaction-Sintered Silicon–Carbide Ceramics

B4C ceramics with increased dislocation density fabricated by reactive spark plasma sintering via carbon nanotubes–boron mixture

Boron carbide with high relative density was prepared in situ using spark plasma sintering. Research on the in-situ reaction of boron and carbon nanotubes reveals that the reaction exhibits high reactivity at 1200 °C. Beyond this temperature, increasing the external pressure was beneficial for particle rearrangement, gas release, and dislocation formation. The result of mechanical properties shows that, the flexural strength and fracture toughness of the boron carbides are 656 ± 9 MPa and 5.0 ± 0.3 MPa m1/2, respectively, when sintered at 1750 °C under continuous pressure ramping conditions–an increase of 64.1% and 46.6% compared to that prepared under constant pressure conditions. Increasing the magnitude of the external stress during the in-situ reaction process can also enhance the particle rearrangement efficiency, inducing the formation of twinning and stacking faults in boron carbide ceramics. High–density twinning and stacking faults dominated the toughening mechanisms of ceramic materials.

Grinding Force Model and Experimental Study on Ultrasonic Assisted Spiral Grinding of Silicon Carbide Ceramic Materials

In order to reveal the mechanical properties of silicon carbide ceramic materials during the drilling process, based on the indentation fracture mechanics theory, a grinding force model of ultrasonic assisted spiral grinding for hole making was established, and the experimental results of ultrasonic assisted spiral grinding for hole making verified the mechanical model. The results showed that the experimental results had the same change trend as the predicted results of the established mechanical model, and the values were close to each other, indicating the accuracy of the established prediction model. The influence of different process parameters on the size accuracy of the hole inlet and outlet aperture after machining is analyzed. It is found that it should be selected as large rotation speed, moderate axial feed speed and small feed pitch to ensure the accuracy of the aperture and effectively suppress the aperture defects during ultrasonic assisted spiral grinding.

Effects of die geometry and insulation on the energy and electrical parameters analyses of spark plasma sintered TiC ceramics

This work conducts a numerical simulation to investigate the temperature and electric current distribution during the spark plasma sintering (SPS) process using the finite element method (FEM) carried out in COMSOL Multiphysics software. The main goal is to optimize the SPS process for titanium carbide (TiC) ceramics, with a particular focus on the effects of insulation and die geometry (height and thickness). For the TiC material, the ideal sintering temperature is set at 2000 °C. The study analyzes eight case studies, involving a base case, an insulating case, and six cases with various thicknesses and heights, in order to evaluate the effectiveness of the suggested optimization. The results show that using insulation on the die surface reduces heat transfer from the die surface significantly, which leads to a 63% decrease in input power consumption when compared to the basic scenario. Based on a correlation study between energy and electricity, increasing die thickness raises the cross-sectional area of the electric current, which raises the amount of electric power required to attain the 2000 °C sintering temperature. The results indicate the temperature distribution in the sample is more sensitive to changes in die height than to changes in die thickness.

Preparation of high-performance (ZrHfTaNbTiMo)C–10Co ceramic by SPS using self-synthesized fine high-entropy carbide powders

A series of high-entropy carbide ceramics with high-performance were successfully prepared by SPS using self-synthesized fine high-entropy carbides powders as hard phase and metal Co as the binder. The effects of Ti and/or Mo addition on densification, grain size and mechanical properties of (ZrHfTaNb)C–10Co ceramic were investigated. The results showed that the addition of Mo improved the wettability between the ceramic phase and Co phase, and significantly increased the densification degree of the ceramics. In addition, the average grain size decreased and the microstructure became more uniform after adding Ti and/or Mo. Compared with the mechanical properties of (ZrHfTaNb)C–10Co ceramic, those of (ZrHfTaNbTiMo)C–10Co ceramic were greatly enhanced under the action of high-entropy effect and solid solution strengthening. The hardness and fracture toughness of the (ZrHfTaNbTiMo)C–10Co ceramic achieved the satisfactory values of 20.37 GPa and 8.59 MPa m1/2, respectively.

Ultrafast high-temperature sintering and densification of ZrC-based ceramics

Zirconium carbide (ZrC) ceramics are promising candidates for high-temperature structural components and nuclear reactors. However, their poor sinterability has limited widespread application. This study explored the sintering and densification of ZrC-based ceramics with graphite or B4C additive using ultrafast high-temperature sintering (UHS). A nearly fully dense ZrC ceramic (> 98%) could be obtained by adding 2.5 wt% B4C additive via ultrafast high-temperature sintering at 2300 °C within 3 min. Additionally, the results revealed that adding graphite into ZrC was beneficial to reduce the grain size but detrimental to densification. Compared to ZrC ceramics sintered using conventional pressureless sintering (PLS) at 2400 °C for 60 min, ZrC-based ceramics with 2.5 wt% B4C sintered via UHS at 2400 °C for 30 s exhibited higher relative densities, smaller grain sizes, and greater Vickers hardness due to faster heating rates and shorter sintering processes.

Influence of (Ta Nb Ti V) C powders synthesized by molten salt at low temperature on densification and properties of high entropy carbide ceramics

AbstractPowder synthesis is crucial for achieving the densification and facilitating widespread applications of high entropy carbide (HEC). Specifically, the production of fine particle‐size powders is essential to enhance the densification of HECs. Consequently, this paper proposes the molten salt method for synthesizing HEC powders. The synthesis process successfully yielded (Ta Nb Ti V) C powders with a particle size of only 0.44 µm at 1400°C, exhibiting a uniform distribution of each element. Subsequent densification of (Ta Nb Ti V) C within the 1700–1900°C temperature range was carried out using spark plasma sintering. It was observed that as the densification temperature increased, the densification and mechanical properties of HEC significantly improved. This study presents innovative ideas for the preparation of HEC at lower temperatures.

Evolutions of microstructural defects in high-entropy carbide ceramics under ion irradiations at room temperature

This work studied and compared the evolutions of irradiation-induced microstructural defects in five high-entropy carbide ceramics (HECCs) at room temperature to reveal the irradiation resistances of HECCs and corresponding underlying mechanisms. The five HECCs exhibit high phase stabilities and no amorphization is observed up to 40 dpa. In-situ 800 keV Kr ion irradiation reveals similar evolutions of irradiation-induced defects. The densities of dislocation loops show non-monotonic variations, which reach the maximum at ∼ 2 dpa and then decrease due to the interactions with each other. In contrast, the sizes of dislocation loops increase monotonically with dose. (NbTaZrW)C exhibits the lowest defect densities and highest defect sizes, which is probably due to the high lattice distortion and its induced high defect recombination efficiencies. Based on the characterization results, it is deduced that the species of constituent elements play more important role in the defect behaviors than the number of constituent elements.

Microstructure and Properties of Hot Pressing Sintered SiC/Y3Al5O12 Composite Ceramics for Dry Gas Seals.

Silicon carbide (SiC) ceramics with high bending strength were prepared by hot pressing sintering (HPS) with yttrium aluminum garnet (Y3Al5O12, YAG) as sintering additive, and the effects of YAG content and sintering temperature on the sintering behavior, microstructure and mechanical properties of SiC ceramics were investigated in detail. The uniform distribution of YAG to form a liquid phase and the driving force provided by hot pressing sintering decrease the sintering temperature, improve the densification of SiC ceramics, and refine the crystal size. By means of suitable sintering conditions with the additional amount of YAG of 5 wt%, the sintering temperature of 1950 °C and a pressure of 30 MPa, the resultant SiC/YAG composite ceramics possesses high sintering and mechanical properties with the relative density of 98.53%, the bending strength of 675 MPa, the Vickers hardness of up to 17.92 GPa, and the elastic modulus of 386 GPa. The as-prepared SiC/YAG composite ceramics are promisingly used as the dry gas seal materials in the centrifugal compressors.

Advancements in the research of high-temperature gas-cooled reactor fuel via additive manufacturing techniques

Recent advances in high-temperature gas-cooled reactor fuel research have captured the global spotlight, as modern operating contexts demand innovative responses to unprecedented challenges. This article offers an overview of contemporary directions in high-temperature gas-cooled reactor fuel design worldwide, pinpointing the shared operational demands and development patterns characteristic of these advanced fuels. It presents an innovative advanced fuel design, which incorporates multi-layer coated particles to boost safety and employs high-temperature-resistant silicon carbide (SiC) ceramics, seamlessly integrated with cutting-edge additive manufacturing (AM) techniques. This design heralds a shift toward modular fuel element solutions that are easily scalable, supporting the diverse array of advanced reactors and marking a significant step forward in the quest for high-temperature gas-cooled reactor fuel technologies.