Evaluation of thermal conductivity of the constituent layers in TRISO particles using Raman spectroscopy

The thermal conductivity of individual layer in the tristructural-isotropic fuel particle was evaluated using Raman spectroscopy. In this method, laser acted simultaneously as an excitation source and a heating source. A three-dimensional point-heating model was developed to estimate the local temperature rise in the probing volume of the laser. The thermal conductivity can be evaluated based on the dependences of the Raman peak position on the temperature and laser power. The calculated thermal conductivities were 8.9 ± 0.2 W/m °C, 13.9 ± 1.5 W/m °C and 11.9 ± 0.9 W/m °C for the buffer, the inner and the outer PyC layers, respectively. Contrastly, the thermal conductivity of the SiC layer was 4.1 W/m °C, which is much lower than the reference value, e.g. 168 W/m °C reported by López-Honorato et al. (J. Nucl. Mater. 378(1) 35–39, 2008). The uncertainty of employing Raman spectroscopy to determine thermal conducitvity was discussed.     

The phase stability and thermophysical properties of InFeO3(ZnO)m (m = 2, 3, 4, 5)

The phase stability and thermophysical properties of InFeO₃(ZnO)_m (m = 2, 3, 4, 5) compounds were investigated, which are a general family of homologous layered compounds with general formula InFeO₃(ZnO)_m (m = 1–19). InFeO₃(ZnO)_m (m = 2, 3, 4, 5) ceramics were synthesized using cold pressing followed by solid-state sintering. They revealed an excellent thermal stability after annealing at 1450 °C for 48 h. No phase transformation occurred during heating to 1400 °C. InFeO₃(ZnO)₃ exhibited a thermal conductivity of 1.38 W m⁻¹ K⁻¹ at 1000 °C, which is about 30% lower than that of 8 wt.% yttria stabilized zirconia (8YSZ) thermal barrier coatings. The thermal expansion coefficients (TECs) of InFeO₃(ZnO)m bulk ceramics were in a range of (10.97 ± 0.33) × 10⁻⁶ K⁻¹ to (11.46 ± 0.35) × 10⁻⁶ K⁻¹ at 900 °C, which are comparable to those of 8YSZ ceramics.     

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.     

Preparation of nanoporous alumina superinsulator with ultra-low thermal conductivity and improved heat resistance up to 1200 °C

Nanoporous alumina superinsulator (NanoASI) with ultra-low thermal conductivity and excellent thermal stability has been prepared by a low-cost and simple dry pressing method. The thermal conductivity of the NanoASI is as low as 0.11 W/m K at 1200 °C and the linear shrinkage is less than 2% after heating at 1200 °C for 1 h. These values are superior to that of previous reported nanoporous insulation materials. Thermal conductivities of this material in the temperature range of 25–1200 °C and pressure range of 10–10⁵ Pa were firstly measured by the transient hot-plane method. The mechanism that improves the heat resistance of the NanoASI is discussed and found that the stabilization of the alumina nanoparticles contributes significantly to the thermal stability of the NanoASI.     

Electrical and thermal properties of SiC-Zr2CN composites sintered with Y2O3-Sc2O3 additives

SiC-Zr₂CN composites were fabricated from β-SiC and ZrN powders with 2 vol% equimolar Y₂O₃-Sc₂O₃ additives via conventional hot pressing at 2000 °C for 3 h in a nitrogen atmosphere. The electrical and thermal properties of the SiC-Zr₂CN composites were investigated as a function of initial ZrN content. Relative densities above 98% were obtained for all samples. The electrical conductivity of Zr₂CN composites increased continuously from 3.8 × 10³ (Ωm)⁻¹ to 2.3 × 10⁵ (Ωm)⁻¹ with increasing ZrN content from 0 to 35 vol%. In contrast, the thermal conductivity of the composites decreased from 200 W/mK to 81 W/mK with increasing ZrN content from 0 to 35 vol%. Typical electrical and thermal conductivity values of the SiC-Zr₂CN composites fabricated from a SiC-10 vol% ZrN mixture were 2.6 × 10⁴ (Ωm)⁻¹ and 168 W/m K, respectively.     

Improvement on the phase stability,mechanical properties and thermal insulation of Y2O3-stabilized ZrO2 by Gd2O3 and Yb2O3 co-doping

Gd₂O₃ and Yb₂O₃ co-doped 3.5 mol% Y₂O₃–ZrO₂ and conventional 3.5 mol% Y₂O₃–ZrO₂ (YSZ) powders were synthesized by solid state reaction. The objective of this study was to improve the phase stability, mechanical properties and thermal insulation of YSZ. After heat treatment at 1500 °C for 10 h, 1 mol% Gd₂O₃–1 mol% Yb₂O₃ co-doped YSZ (1Gd1Yb-YSZ) had higher resistance to destabilization of metastable tetragonal phase than YSZ. The hardness of 5 mol% Gd₂O₃–1 mol% Yb₂O₃ co-doped YSZ (5Gd1Yb-YSZ) was higher than that of YSZ. Compared with YSZ, 1Gd1Yb-YSZ and 5Gd1Yb-YSZ exhibited lower thermal conductivity and shorter phonon mean free path. At 1300 °C, the thermal conductivity of 5Gd1Yb-YSZ was 1.23 W/m K, nearly 25% lower than that of YSZ (1.62 W/m K). Gd₂O₃ and Yb₂O₃ co-doped YSZ can be explored as a candidate material for thermal barrier coating applications.     

High temperature physical and mechanical properties of large-scale Ti2AlC bulk synthesized by self-propagating high temperature combustion synthesis with pseudo hot isostatic pressing

The electrical, thermal, and mechanical properties as well as the effect of the temperature of large-scale Ti₂AlC bulk synthesized by self-propagating high temperature combustion synthesis with pseudo hot isostatic pressing were investigated in detail. With increasing temperature, the lattice defects contribute to the decreasing phonon thermal conductivity, and the electrical resistivity increases linearly from room temperature (RT) to 900 °C. The RT flexural strength, compressive strength, fracture toughness, work of fracture, and Vickers hardness were measured to be 606 ± 20 MPa, 1057 ± 84 MPa, 6.9 ± 0.2 MPa m^1/2, 158 ± 12 J/m², and 4.7 ± 0.2 GPa, respectively. With increasing temperature, the flexural and compressive strengths both keep almost unchanged in the zone of brittle failure, but decrease sharply as the plastic deformation occurs. The brittle-plastic transition temperature under flexure (900–950 °C) is higher than compression (700–800 °C). Interestingly, a non-catastrophic failure is observed in the SENB test, with the high work of fracture (158 ± 12 J/m²).     

Porous anorthite ceramics with ultra-low thermal conductivity

Porous anorthite ceramics with an ultra-low thermal conductivity of 0.018 W/m K have been fabricated by hydrous foam-gelcasting process and pressureless sintering method using γ-alumina, calcium carbonate and silica powders as raw materials. Microstructure and phase composition were analyzed by SEM and XRD respectively. Properties such as porosity, pore size distribution and thermal conductivity were measured. High porosity (69–91%) and low thermal conductivity (0.018–0.13 W/m K) were obtained after sintering samples with different catalyst additions at 1300–1450 °C. Porosity, pore size, pore structure and grain size had obvious effect on heat conduction, resulting in the low thermal conductivity. The experimental thermal conductivity data of porous anorthite ceramics were found to be fit well with the computed values derived from a universal model.     

Linear thermal expansion coefficients of relaxor-ferroelectric 0.57Pb(Sc1/2Nb1/2)O3–0.43PbTiO3 ceramics in a wide temperature range

The objective of this work was to examine linear thermal expansion of virgin and poled 0.57Pb(Sc_1/2Nb_1/2)O₃–0.43PbTiO₃ ceramics between 30 °C and 600 °C by contact dilatometry. The thermal expansion dL/Lo of the virgin ceramic increases with increasing temperature until approximately 260 °C. The physical and technical thermal expansion coefficients were determined. At 260 °C the physical thermal coefficient is 2.08 × 10^?6 K^?1. Between 260.0 °C and 280.0 °C an anomaly in the thermal expansion vs. temperature and an endothermic peak in the differential scanning calorimetry curves correspond to the phase transition region from tetragonal to cubic phase. At temperatures from 280 °C to 600 °C the thermal expansion dL/Lo increases again.In the derivative of the dL/Lo heating curves of the poled ceramics, additionally to the anomaly at 270 °C, also the anomaly at 160 °C is observed, which is associated with the depolarization of the material during heating.     

Study on preparation of thermal storage ceramic by using clay shale

Shale was used as main raw material for developing thermal storage ceramics. The samples were fabricated via semi-dry pressing followed by pressureless sintering. The result showed that the sample (75% shale, 10% kaolin, 10% potash feldspar and 5% soda feldspar) fired at 1080 °C exhibited the best comprehensive performance. Ocular examination reveals that no cracks were observed after 30 cycle times thermal shock tests (wind cooling from 600 °C to room temperature). The results presented that the high bending strength remained after 20 cycle times thermal shock tests but plummeted at the thirtieth time. Other properties were given as follows: bulk density: 2.60 g/cm³; thermal conductivity: 2.33 W/(m °C); and heat storage density: 578.50 mJ/m³. XRD analysis indicated that the quartz and hematite were the main solid phases in the sample. Some isolated pores, quartz crystals, granular hematite crystals and needle-like mullite crystals were observed in the matrix according to the SEM (Scanning Electron Microscope) analysis. More pores were found with temperature rizing according to SEM analysis. The relatively high content of Fe₂O₃ contributed to the formation of the vitreous phase and favored the densification. Overall, the introduction of shale effectively reduced the firing temperature and performed the better thermal storage properties.     

High thermal conductivity in pressureless densified SiC ceramics with ultra-low contents of additives derived from novel boron–carbon sources

In order to attain high thermal conductivity, SiC was doped with ultra-low amounts of B and C as sintering additives using boric acid together with d-fructose as boron–carbon sources. The contents of in situ generated B and C were both tailored as low as 0.4 wt.%, which can significantly reduce the impurities induced phonon scattering effect. The SiC ceramics were pressureless densified at 2150 °C for 1 h, and some samples experienced subsequent annealing at 1950 °C for 4 h. High thermal conductivities of 180.94 W/(m K) for the as-sintered SiC ceramics and 192.17 W/(m K) for the annealed specimens at room temperature were achieved. The reasons for the high thermal conductivity in the polycrystalline SiC ceramics were specified, based on the close correlation with microstructure.     

Microstructure and dielectric properties of amorphous BaSm2Ti4O12 thin films for MIM capacitor

BaSm₂Ti₄O₁₂ (BST) film grown at room temperature was amorphous, while the film grown at 300 °C was also amorphous but contained a small amount of crystalline Sm₂Ti₂O₇ (ST). The crystalline BST phase was formed when the film was grown at 700 °C and subjected to rapid thermal annealing (RTA) at 900 °C. On the other hand, the ST phase was formed in the film grown at 300 °C and subjected to RTA at 900 °C. A high capacitance density of 2.12 fF/μm² and a low leakage current density of 1.15 fA/pF V were obtained from the 150 nm-thick BST film grown at 300 °C. Its capacitance density could conceivably be further increased by decreasing the thickness of the film. It had linear and quadratic coefficients of capacitance of −785 ppm/V and 5.8 ppm/V² at 100 kHz, respectively. Its temperature coefficient of capacitance was also low, being approximately 255 ppm/°C at 100 kHz.     

Controlling heat radiation for development of high-temperature insulating materials

Conventional industrial insulating materials have a porous structure, and provide good resistance to conduction. However, at high temperatures greater than 1000 °C, this structure permits heat transfer through radiation. In recent years, many high-performance insulating materials have been developed that consist of nanosized particles and pores. Such materials have a thermal conductivity less than 0.1 W/(m K) up to 800 °C. However, it has very less heat resistance over 1000 °C.In this study, we have developed an insulating material which has a great suppress radiation and its thermal conductivity was less than 0.3 W/(m K) at 1500 °C. The insulating material was considered to be porous magnesium aluminate spinel of two different pore sizes, 0.05–1 and 1–5 μm, with a porosity of 78%. Among the two pores, the 1–5 μm pores were more efficient to restrain heat transfer through radiation.     

Densification of nanocrystalline Y2O3 ceramic powder by spark plasma sintering

Nanocrystalline Y₂O₃ powders with 18 nm crystallite size were sintered using spark plasma sintering (SPS) at different conditions between 1100 and 1600 °C. Dense specimens were fabricated at 100 MPa and 1400 °C for 5 min duration. A maximum in density was observed at 1400 °C. The grain size continuously increased with the SPS temperature into the micrometer size range. The maximum in density arises from competition between densification and grain growth. Retarded densification above 1400 °C is associated with enhanced grain growth that resulted in residual pores within the grains. Analysis of the grain growth kinetics resulted in activation energy of 150 kJ mol^?1 and associated diffusion coefficients higher by 10³ than expected for Y³⁺ grain boundary diffusion. The enhanced diffusion may be explained by combined surface diffusion and particle coarsening during the heating up with grain boundary diffusion at the SPS temperature.     

Examining structure property relationships in coatings based on substituted linear aromatic polycyanurates

Three series of halogenated and non-halogenated polycyanurates are prepared in good yield and purity, and fully characterised. Many of the resulting polymers, formed at room temperature using phase transfer catalysis, can be cast into films with good resilience and high thermal stability (some examples suffer no mass loss when held isothermally at 190 °C and only display appreciable losses when held continuously at 300 °C). Char yields of 35–65% are achieved in nitrogen depending on backbone structure. Some problems were encountered with solubility, particularly with heavily halogenated dichlorotriazines, which limited molecular weights (M_n = 2000–4000 g mol^?1 depending on backbone structure) although when the phase volume ratio was altered to 0.25 higher molecular weights (M_n = 10,000–30,000 g mol^?1) were possible. Best solubility was achieved by using aromatic diols with at least two equivalent phenylene units per dichlorotriazine unit. DSC reveals polymerisation exotherms with maxima at 190–260 °C (ΔH_p = 35–57 kJ/mol) followed by embrittlement and shrinkage (when heated to 300 °C). These phenomena may be due to the formation of poorly formed crystallites (activation energies span 155–380 kJ/mol) combined with thermal isomerisation.     

Preparation and properties of B6O/TiB2-composites

B₆O/TiB₂ composites with varying compositions were produced by FAST/SPS at temperatures between 1850 and 1900 °C following a non-reactive or a reactive sintering route. The densification, phase and microstructure formation and the mechanical and thermal properties were investigated. The comparison to an also investigated pure B₆O material showed that the addition of TiB₂ in a non-reactive sintering route promotes the B₆O densification. Further improvement was obtained by sintering reactive B–TiO₂ mixtures which also results in materials with a finer grain size and thus in enhanced mechanical properties. The fracture toughness was significantly improved in all composites and is up to 4.0 MPa m^1/2 (SEVNB) and 2.6–5.0 MPa m^1/2 (IF method) while simultaneously a high hardness of up to 36 GPa (HV_0.4) and 28 GPa (HV₅) could be preserved. The high temperature properties at 1000 °C of hardness, thermal conductivity and CTE were up to 20 GPa, 18 W/mK and 6.63 × 10^?6/K, respectively.     

Thermal properties of La2O3-doped ZrB2- and HfB2-based ultra-high temperature ceramics

Thermal properties of La₂O₃-doped ZrB₂- and HfB₂-based ultra high temperature ceramics (UHTCs) have been measured at temperatures from room temperature to 2000 °C and compared with SiC-doped ZrB₂- and HfB₂-based UHTCs and monolithic ZrB₂ and HfB₂. Thermal conductivities of La₂O₃-doped UHTCs remain constant around 55–60 W/mK from 1500 °C to 1900 °C while SiC-doped UHTCs showed a trend to decreasing values over this range.     

Densification and mechanical properties of hot-pressed ZrN ceramics doped with Zr or Ti

The densification of hot-pressed ZrN ceramics doped with Zr or Ti have been investigated at 1500–1700 °C. It is shown that either Zr or Ti additive can facilitate the densification process. ZrN with 20 mol% Zr or Ti (named ZNZ and ZNT) sintered at 1700 °C can achieve above 98% relative densities whereas densification temperature up to 2000 °C is necessary for pure ZrN. The densification improvements are attributed to solid solution of Zr or Ti into ZrN to form non-stoichiometric ZrN_1?x or (Zr, Ti)N_1?x. The microstructures and mechanical properties of ZNZ and ZNT samples have been examined. Large grain size and flat fracture surface existed in ZNT sample sintered at 1700 °C, which lead to poor toughness as low as 2.3 MPa m^1/2. On the contrary, the fracture toughness of ZNZ sample sintered at 1700 °C was up to 5.9 MPa m^1/2, attributed to fine and uniform grain size distribution.     

Direct thermal diffusion bonding of Nd:YAG/YAG composite transparent ceramics by vacuum sintering

Nd:YAG/YAG transparent ceramics were prepared by vacuum sintering at 1780 °C for 40 h and annealed at 1450 °C for 20 h in air. Two separately polished Nd:YAG/YAG samples were bonded into monolithic and uniform composite-material followed by vacuum sintering at 1790 °C for 50 h under uniaxial pressure of 60 MPa, and then annealed at 1450 °C for 100 h in air. The fracture strength of bonded samples at the bonding interface is higher than that of as-prepared Nd:YAG/YAG samples. Meanwhile, the extinction coefficient of bonded samples is 0.0305 cm⁻¹ which is an improvement over as-prepared samples. The microstructure of the contact interface reveals the disappearance of the contact layer at the bond due to the grain growth and coalescence mainly based on grain boundary diffusion at higher temperatures and longer heat-treated time, which indicates that the bonding technology is beneficial to the fabrication of the thick composite materials.     

Fabrication of porous SiO2/C composite from rice husks

Porous SiO₂/carbon composites were fabricated by heating pellets composed of rice husk (RH) powders in small (<74 μm), medium(74–175 μm) and large(150–300 μm) sizes. The contents of the small RH were fixed at 30 mass% and the RH pellets molded at 10, 15, and 30 MPa were heated at 800–1150 °C in an inert atmosphere. The weight loss due to the thermal decomposition of the organic materials in the pellet peaked at 1000 °C, whereas the specimen heated at 1000 °C showed the lowest carbon content and density, 29 mass% and 0.40 g cm⁻³, respectively. The SiO₂ phase of the specimens were amorphous at 800 and 1150 °C, but a cristobalite phase was visible at 1000 °C. The specimen fire at 1000 °C showed a higher compressive strength than the others, and the large RH particles were seen to increase the strength of the product while an increase in molding pressure decreased the medium pore size, from 17 to 7 μm, and increased the strength, from 0.25 to 3.52 MPa. The specific surface area (SSA) of the specimen peaked at 450 m² g⁻¹, at 1000 °C and finally, the mesopore size of the specimens was similar throughout, at ∼2 nm.