Fabrication and thermal conductivity of AlN/BN ceramics by spark plasma sintering

Aluminum nitride/boron nitride (AlN/BN) ceramics with 15–30 vol.% BN as secondary phase were fabricated by spark plasma sintering (SPS), using Yttrium oxide (Y₂O₃) as sintering aid. Effects of Y₂O₃ content and the SPS temperature on the density, phase composition, microstructure and thermal conductivity of the ceramics were investigated. The results revealed that with increasing the amount of starting Y₂O₃ in AlN/BN, Yttrium-contained compounds were significantly removed after SPS process, which caused decreasing of the residual grain boundary phase in the sintered samples. As a result, thermal conductivity of AlN/BN ceramics was remarkably improved. By addition of Y₂O₃ content from 3 wt.% to 8 wt.% into AlN/15 vol.% BN ceramics, the thermal conductivity increased from 110 W/m K to 141 W/m K.     

Mechanical and thermal properties of spark plasma sintered Al2O3-graphene-SiC hybrid composites

Monolithic Al₂O₃ and Al₂O₃-graphene-SiC hybrid composites were prepared by spark plasma sintering (SPS) under vacuum atmosphere. The results show that the hybrid composites were almost completely dense (>97%). SiC content has a significant effect on the microstructure of the composites. With the increase of SiC content, the average grain size of alumina decreased gradually. The addition of SiC to alumina changed fracture mode from inter-granular fracture to mixed fracture mode of inter-granular fracture and trans-granular fracture. The Al₂O₃-0.4 wt%graphene-5 wt% SiC hybrid composite has the highest bending strength and hardness, which were 57% and 19.22% higher than those of the monolithic alumina, respectively. The room temperature (RT) thermal conductivity of the monolithic Al₂O₃ (25.5 W/m·K) was the highest. The thermal conductivity and thermal diffusivity coefficient of the composites decreased with the increase in temperature, while the specific heat of monolithic alumina and composites increased with the increase in temperature and additives. These properties were related to the microstructure of materials and the possible transport mechanisms were discussed.     

High thermal conductivity of spark plasma sintered silicon carbide ceramics with yttria and scandia

A fully dense SiC ceramic with a room‐temperature thermal conductivity of 262 W·(m·K)^?1 was obtained via spark plasma sintering β‐SiC powder containing 0.79 vol% Y₂O₃‐Sc₂O₃. High‐resolution transmission electron microscopy revealed two different SiC‐SiC boundaries, that is, amorphous and clean boundaries, in addition to a fully crystallized junction phase. A high thermal conductivity was attributed to a low lattice oxygen content and the presence of clean SiC‐SiC boundaries.     

Thermal conductivity of SiC microwires: Effect of temperature and structural domain size uncovered by 0 K limit phonon scattering

A comparative study of structure and thermal properties is reported for three 3C crystalline silicon carbide (SiC) microwires, including Sylramic, Hi-Nicalon S and a sample fabricated by laser chemical vapor deposition (LCVD). Structural characterization by Raman spectroscopy and x-ray diffraction (XRD) finds that the LCVD-based sample contains excessive silicon and smallest grains of SiC but detectable free carbon. Thermal characterization from room temperature down to 20 K uncovers the effect of nanosized grain on thermal properties. The thermal properties are correlated with the structure via structural thermal domain (STD) size, defined as the grain boundary-induced phonon mean free path at the 0 K limit. The STD size of the three samples is found as 9.35, 1.42 and 1.03?nm for the Sylramic, Hi-Nicalon S and LCVD SiC fibers, proportional to and nearly one order of magnification smaller than the corresponding crystalline size determined by XRD: 67–113, 14.6–18.4, and 5.85–7.84?nm.     

Microstructures and thermal conductivities of reaction sintered SiC ceramics

Abstract

Reaction sintered SiC ceramics were prepared by the silicon melt infiltration method over temperatures of 1450?1550°C. The effects of the carbon and silicon contents of the starting materials as well as the sintering temperature and time on the thermal conductivities and microstructures of the ceramic materials were studied. The thermal conductivities and microstructures of the samples were characterised using thermal conductivity measurements, X-ray diffraction analysis, scanning electron microscopy, energy-dispersive X-ray spectroscopy and mercury injection porosimetry. The results showed that sintering temperature and time as well as the carbon and silicon contents of the green specimens are the main factors affecting the microstructure and porosity of reaction bonded SiC ceramics. Increasing the reaction temperature and time decreased the porosity of the ceramics. This was due to the infiltration of the silicon melt into the ceramic specimens. The thermal conductivity and porosity of the sample sintered at 1550°C for 3 h in an argon atmosphere were 102·5 W m K^?1 and 0·3% respectively.     

Thermal and electrical properties of spark plasma sintered (Ti,Cr)B2 ceramics

Thermal and electrical properties were measured for TiB₂ ceramics containing varying CrB₂ contents up to 33 mol%. The room-temperature thermal diffusivity decreased with increasing Cr content from 0.330 ± 0.003 cm²/s for pure TiB₂ to 0.060 ± 0.003 cm²/s for (Ti_0.66Cr_0.33)B₂. The amount of anisotropy in the coefficients of thermal expansion increased with increasing Cr content and the c-axis had the greatest dependence on Cr addition, with an increase of more than 25% in the thermal expansion for 33 mol% CrB₂ compared to TiB₂, whereas the a-axis only increased by about 8%. The electrical conductivity was the lowest for (Ti_0.66Cr_0.33)B₂ at ∼8.5 × 10³ S/cm compared to ∼106.1 × 10³ S/cm for nominally pure TiB₂. Overall, the addition of CrB₂ as a sintering aid for TiB₂ was shown to have a significant effect on the thermal and electrical properties of TiB₂ for additions as small as 5 mol% CrB₂.     

Preparation of high-purity SiC ceramics with good plasma corrosion resistance by hot-pressing sintering

High-purity SiC ceramic devices are applied in semiconductor industry owing to their outstanding properties. Nevertheless, it is difficult to densify SiC ceramics without any sintering additive even by HP sintering. In this work, high-purity and dense SiC ceramics were fabricated by HP sintering with very low amounts of sintering aids. Residual B content was only 556 ppm and relative density was more than 99.5%. Furthermore, thermal conductivity of as-prepared SiC ceramics was improved from 155 W m^?1 K^?1 to 167 W m^?1 K^?1 by increasing holding time and their plasma corrosion resistance was promoted in the meantime. The as-prepared high-purity SiC ceramics have broad application prospects in the field of semiconductor industry.     

IR-transparent MgO-Y2O3 ceramics by self-propagating high-temperature synthesis and spark plasma sintering

A glycine–nitrate self-propagating high temperature synthesis (SHS) was developed to produce composite Y₂O₃–MgO nanopowders. Based on the thermodynamic calculations a 0.25YMg₂(NO₃)₇-0.75NH₂CH₂COOH precursor composition was selected to prepare low agglomerated uniform composite yttria-magnesia powder. Near full dense composite ceramics were fabricated based on the prepared powders by the spark plasma sintering method. IR-transmittance and hardness of the Y₂O₃–MgO ceramics were studied in correlation with sintering conditions. The best transmittance of 80.9%@5 μm and H_v = 10.2 GPa were measured for the sample obtained at 1150 °C.     

Surface microstructural changes of spark plasma sintered zirconia after grinding and annealing

Spark plasma sintered zirconia (3Y-TZP) specimens have been produced of 140 nm 372 nm and 753 nm grain sizes by sintering at 1250 °C, 1450 °C and 1600 °C, respectively. The sintered zirconia specimens were grinded using a diamond grinding disc with an average diamond particle size of about 60 µm, under a pressure of 0.9 MPa. The influence of grinding and annealing on the grain size has been analysed. It was shown that thermal etching after a ruff grinding of specimens at 1100 °C for one hour induced an irregular surface layer of about a few hundred nanometres in thickness of recrystallized nano-grains, independently of the initial grain size. However, if the ground specimens were exposed to higher temperature, e.g. annealing at 1575 °C for one hour, the nano-grain layer was not observed. The resulted grain size was similar to that achieved by the same heat treatments on carefully polished specimens. Therefore, by appropriate grinding and thermal etching treatments, nanograined surface layer can be obtained which increases the resistance to low temperature degradation.     

Characterization of spark plasma sintered TiC ceramics reinforced with graphene nano-platelets

This research aims to scrutinize the impact of graphene additive on the consolidation behavior, microstructure and physical-mechanical qualifications of TiC-based materials. For this purpose, two specimens, namely monolithic TiC and TiC-5 wt% graphene, were produced using the spark plasma sintering (SPS) method at 1900 °C. An external pressure of 40 MPa was applied during the sintering, and the ceramics were held at the maximum temperature for 10 min. The characteristics of SPSed samples were studied using scanning electron microscopy (SEM) and X-ray diffraction (XRD). Although adding graphene had no notable effect on the sinterability of TiC, it led to an increment in the flexural strength of graphene-doped sample. The microstructural assessment revealed the positive influence of graphene additive on obtaining a finer microstructure. The phase analysis confirmed the appearance of a non-stoichiometric hexagonal TiC_x and different allotropes of carbon in the samples. Finally, the highest values for Vickers hardness (~3130 HV_0.1Kg) and flexural strength (~530 MPa) were attained for the monolithic TiC and graphene-reinforced samples, respectively.     

Microstructural and mechanical characterization of spark plasma sintered TiC ceramics with TiN additive

This investigation intends to study the influence of titanium nitride (TiN) additive on the sintering behavior, mechanical features and microstructural development of TiC-based substances. For this objective, two different samples, namely monolithic TiC and TiC-5 wt% TiN, were sintered at 1900 °C using the SPS method. The specimens were held at the ultimate temperature for 10 min under 40 MPa. X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) were implemented to characterize the as-produced specimens. Introducing TiN increased the relative density of TiC by around 1.5%, standing next to 97%. The assessments revealed the creation of non-stoichiometric TiC_1-x along with some graphitized carbon phases in the undoped ceramic. By contrast, TiN additive completely dissolved into the TiC matrix in the composite sample and a new in-situ phase (C₃N₄) appeared. Finally, a Vickers hardness of ~2750 HV_0.1 and a flexural strength of ~450 MPa were achieved for the TiN-doped specimen.     

Thermal conductivity of liquid-phase sintered silicon carbide ceramics: A review

Silicon carbide (SiC) exhibits excellent thermal conductivity. Recently, thermal conductivity that amounts to 261.5 W/m-K has been obtained in polycrystalline SiC ceramic liquid-phase sintered (LPS) with Y₂O₃-Sc₂O₃ additives at 2050 °C under a nitrogen atmosphere. From the additive used to the sintering atmosphere selected, many factors affect the thermal conductivity of the SiC. In this review, important factors that are known to determine the thermal conductivity of LPS-SiC (lattice oxygen/nitrogen content, porosity, grain size, grain boundary structure, phase transformation, and additive composition) have been evaluated. While reviewing the impact of each factor on thermal conductivity, hidden correlations among different factors are also discussed. Among the factors that are claimed to be important, we suggest a few factors that are more critical to thermal conductivity than others. Based on the most critical factors on the thermal conductivity of LPS-SiC, a complete engineers’ guide for high thermal conductivity LPS-SiC is proposed.     

Effect of grain growth on the thermal conductivity of liquid-phase sintered silicon carbide ceramics

The effect of grain growth on the thermal conductivity of SiC ceramics sintered with 3 vol% equimolar Gd₂O₃-Y₂O₃ was investigated. During prolonged sintering at 2000 °C in an argon or nitrogen atmosphere, the β → α phase transformation, grain growth, and reduction in lattice oxygen content occurs in the ceramics. The effects of these parameters on the thermal conductivity of liquid-phase sintered SiC ceramics were investigated. The results suggest that (1) grain growth achieved by prolonged sintering at 2000 °C accompanies the decrease of lattice oxygen content and the occurrence of the β → α phase transformation; (2) the reduction of lattice oxygen content plays the most important role in enhancing the thermal conductivity; and (3) the thermal conductivity of the SiC ceramic was insensitive to the occurrence of the β → α phase transformation. The highest thermal conductivity obtained was 225 W(m K)⁻¹ after 12 h sintering at 2000 °C under an applied pressure of 40 MPa in argon.     

Thermal conductivity studies on Si/SiC ceramic composites

Ceramic heat exchangers are increasingly used in many nuclear power plants. Silicon carbide has been treated as a promising material for heat exchanger application since it has good thermal conductivity and corrosion resistance. In this work, four different types of Si/SiC ceramic composites were prepared by liquid silicon infiltration technique. Thermal conductivities of these ceramic composites at different temperatures are measured by the laser flash thermal conductivity method. Results show that the presence of free carbon and voids are notably affecting the thermal conductivity of these materials.     

Densification improvement of spark plasma sintered TiB2-based composites with micron-, submicron- and nano-sized SiC particulates

Taguchi design of experiments methodology was used to determine the most influential spark plasma sintering (SPS) parameters on densification of TiB₂–SiC ceramic composites. In this case, four processing factors (SPS temperature, soaking time, applied external pressure and SiC particle size) at three levels were examined in order to acquire the optimum conditions. The statistical analysis identified the sintering temperature as the most effective factor influencing the relative density of TiB₂–SiC ceramics. A relative density of 99.5% was achieved at the optimal SPS conditions; i.e. temperature of 1800?°C, soaking time of 15?min and pressure of 30?MPa by adding 200-nm SiC particulates to the TiB₂ matrix. The experimental measurements and predicted values for the relative density of composite fabricated at the optimum SPS conditions and reinforced with the proper SiC particle size were almost similar. The mechanisms of sintering and densification of spark plasma sintered TiB₂–SiC composites were discussed in details.     

Combined role of SiC whiskers and graphene nano-platelets on the microstructure of spark plasma sintered ZrB2 ceramics

This research explores the sintering behavior and microstructure of ZrB₂-based materials containing graphene nano-platelets (GNPs) and SiC whiskers (SiC_w). Spark plasma sintering (SPS) process at 1900 °C was implemented to sinter the specimen, leading to a composite with 100% relative density. High-resolution transmission electron microscopy (HRTEM), field emission scanning electron microscopy (FESEM), X-ray photoelectron spectroscopy (XPS), field emission-electron probe microanalyzer (FE-EPMA), and high-resolution X-ray diffractometry (HRXRD) were employed to study the SPSed sample, along with the thermodynamics predictions. According to the HRXRD result and microstructural observations, the sintering process was non-reactive, which was endorsed with the XPS analysis. Furthermore, graphene presented a beneficial role for eradicating the oxide impurities in the sample during the sintering. Such oxide impurities were reduced to the original phases of SiC and ZrB₂, contributing to porosity removal. Nanostructural investigations revealed the formation of ultrathin amorphous interfaces (~10 nm) between ZrB₂/graphene phases, disordered atomic planes in graphene platelets, and dislocations in ZrB₂ grains. One reason for generating crystalline defects in the microstructure was found out to be the mismatches amongst the elastic properties of the available compounds in the system.     

Mechanical and optical properties of spark plasma sintered transparent Y2O3 ceramics

Commercial Y₂O₃ nanopowder was used to fabricate transparent Y₂O₃ ceramics by spark plasma sintering under the pressure of 100 MPa for 20 min with the heating rate of 100 °C/min. The microstructures, mechanical and optical properties of the Y₂O₃ ceramics sintered at different temperatures were investigated in detail. Densification occurred up to a sintering temperature of 1500 °C, and above 1500 °C, rapid grain growth and pore growth occurred. The highest relative density of 99.58% and the minimum average grain size of 0.58±0.11 µm were obtained at 1500 °C. The flexural strength, hardness and fracture toughness of the optimal spark plasma sintered Y₂O₃ ceramic were 122 MPa, 7.60 GPa and 2.06 MPa.m^1/2, respectively. The Y₂O₃ ceramic sintered at 1500 °C had the in-line transmission of about 11–54% and 80% in the wavelength range of 400–800 nm and 3–5 µm, respectively.     

Thermal conductivity and mechanical properties of Si3N4 ceramics with binary fluoride sintering additives

Silicon nitride (Si₃N₄) ceramics were fabricated by gas pressure sintering (GPS) using four sintering additives: Y₂O₃–MgO, Y₂O₃–MgF₂, YF₃–MgO, and YF₃–MgF₂. The phase composition, grain growth kinetics, mechanical properties, and thermal conductivities of the Si₃N₄ ceramics were compared. The results indicated that the reduction of YF₃ on SiO₂, induced a high Y₂O₃/SiO₂ secondary phase ratio, which improved the thermal conductivity of the Si₃N₄ ceramics. The depolymerization of F atom reduces the diffusion energy barrier of solute atom and weakens the viscous resistance of anion group, which was beneficial to grain boundary migration. Besides exhibiting a lower grain growth exponent(n = 2.5)and growth activation energy (Q = 587.94 ± 15.35 kJ/mol), samples doped with binary fluorides showed excellent properties, including appreciable thermal conductivity (69 W m⁻¹ K⁻¹), hardness (14.63 ± 0.12 GPa), and fracture toughness (8.75 ± 0.18 MPa m^1/2), as well as desirable bending strength (751 ± 14 MPa).     

Improved thermal conductivity and mechanical properties of SiC/SiC composites using pitch-based carbon fibers

Pitch-based carbon fibers were assembled in horizontal and thickness directions of SiC/SiC composites to form three-dimensional heat conduction networks. The effects of heat conduction networks on microstructures, mechanics, and thermal conductivities were investigated. The results revealed the benefit of introducing heat conduction networks in the densification of composites. The maximum bending strength and interlaminar shear strength of the modified composites reached 568.67 MPa and 68.48 MPa, respectively. These values were equivalent to 18.6% and 69.4% increase compared to those of composites without channels. However, channels in thickness direction destroyed the continuity of fibers and matrix, creating numerous defects. As the volume fraction of heat conduction channels rose, the pinning strengthening effect of channels and influence of defects competed with each other to result in first enhanced mechanical properties followed by a decline. The in-plane thermal conductivity was found anisotropic with a maximum value reaching 86.20 W/(m·K) after introducing pitch-based carbon unidirectional tapes. The thermal conductivity in thickness direction increased with volume fraction of pitch-based carbon fibers and reached 19.13 W/(m·K) at 3.87 vol% pitch-based carbon fibers in the thickness direction. This value was 90.75% higher than that of composites without channels.     

Electrical conductivity and thermal properties of spark plasma sintered Al2O3-SiC-CNT hybrid nanocomposites

In this study, we report the electrical conductivity and thermal properties of Al₂O₃-SiC-CNT hybrid nanocomposites processed via ball milling (BM) and spark plasma sintering (SPS). The initial powders and consolidated samples were characterized using transmission electron microscopy (TEM) and field emission scanning electron microscopy (FE-SEM), respectively. A multifunction calibrator and a high-resolution digital multimeter were used to measure the electrical conductivity. The thermal properties were measured using a thermal constants analyser. The SiC and CNT-reinforced alumina hybrid nanocomposites exhibited a significant increase in their room-temperature electrical conductivity, which made them suitable for electrical discharge machining. The Al₂O₃-5SiC-2CNTs had a high electrical conductivity value of 8.85 S/m compared to a low value of 6.87×10⁻¹⁰ S/m for the monolithic alumina. The addition of SiC and CNTs to alumina decreased its room-temperature thermal properties. The increase in temperature resulted in a decrease in the thermal conductivity and thermal diffusivity but an increase in the specific heat of the monolithic alumina and the hybrid nanocomposites. These properties were correlated with the microstructure, and possible transport mechanisms were discussed.