Effect of Sm2O3 content on microstructure and thermal conductivity of Spark Plasma Sintered AlN ceramics

Dense aluminum nitride ceramics were prepared by Spark Plasma Sintering at a lower sintering temperature of 1700 °C with Sm₂O₃ as sintering additives. The effect of Sm₂O₃ content on the density, phase composition, microstructure and thermal conductivity of AlN ceramics was investigated. The results showed that Spark Plasma Sintering could fabricate dense AlN ceramics with superior thermal properties in a very short time. Sm₂O₃ not only facilitated the densification via the liquid-phase sintering mechanism but also improved thermal conductivity by decreasing oxygen impurity. Thermal conductivity decreased with increasing amount of Sm₂O₃ and the highest thermal conductivity was obtained for the AlN ceramics with 2 wt.% Sm₂O₃ content. During Spark Plasma Sintering process, only 2–3 wt.% sintering additives was enough to fabricate dense AlN ceramics, and the microstructures played a key role in controlling the thermal conductivity of AlN ceramics.     

Thermal conductivity of plasma-sprayed W/SiC composite for high-temperature energy applications

W/SiC metal matrix composites were produced by gas tunnel type plasma spraying (GTPS) using a mixture of 12 wt.% SiC-88 wt.% W feedstock powder. This work aimed at the optimization of the plasma gun current for deposition of a W/SiC composite with fine microstructure on AISI 304 substrate. Characterization of deposits was performed in order to assess microstructure, micro-hardness, thermal diffusivity and thermal conductivity. WO₃ was detected in the composite deposits, which indicated that the tungsten partially oxidized during plasma spraying. Also, the deposit composite was dense and nearly free of pores due to the little mismatch between the coefficient of thermal expansion (CTE) for W and SiC. Microhardness values gradually decreased as a function of input current due to the formation of WO₃ and the decomposition of SiC particles in high temperature flame region. The thermal conductivity as high as ∼ 59 W/mK was obtained at gun current 80 A. It was found that both tungsten oxide and structure imperfections have a significant influence on the thermal conductivity and mechanical properties.     

Fabrication and thermophysical properties of porous TiB2 ceramics fabricated by reactive spark plasma sintering

Titanium oxide (TiO₂) and boron carbide (B₄C) were added to TiB₂ raw powders to prepare porous TiB₂ ceramics by reactive spark plasma sintering, and the gas escape (such as CO and B₂O₃) resulted in higher porosity. X-ray Diffraction results indicated that the reduction reaction was completed after the reactive spark plasma sintering process. The porosity could be controlled by changing the ratio of synthesized TiB₂ to raw TiB₂ powders. The porosity of porous TiB₂ ceramics with 20 wt.% and 40 wt.% synthsized TiB₂ ceramics are 18.5% and 22.2%, respectively. The thermal diffusivity of the porous TiB₂ ceramics decreased with the porosity due to the low diffusivity behavior of gas and vacuum in pores, and the thermal conductivity for porous TiB₂ ceramics decreased as the temperature increased throughout the measured temperature range. The results here pointed to a potential method for fabricating porous TiB₂ ceramics with controllable thermophysical properties.     

Synthesis of ultrafine/nanocrystalline W-(30-50)Cu composite powders and microstructure characteristics of the sintered alloys

Ultrafine/Nanocrystalline W-Cu composite powders with various copper contents (30, 40 and 50 wt.%) have been synthesized by sol-spray drying and a subsequent hydrogen reduction process. The powders were consolidated by direct sintering at temperatures between 1150 and 1260 °C for 90 min. The powder characteristics and sintering behavior, as well as thermal conductivity of the sintered alloys were investigated. The results show that the synthesized powders exist in ultrafine composite particles containing numerous nanosized particles, and the composition distributed very homogeneously. As the copper contents increase, the grain size of the powders decreases. The subsequent sintered parts show nearly full density with the relative density more than 99% at the temperature of 1250 °C. The sintered parts have very fine tungsten grains embedded in a bulk matrix. With increased copper contents, the tungsten grain size decreases and the microstructural homogeneity of the sintered alloys improves further. The thermal conductivity properties, while a little lower than that of the theoretical value, depend on the copper contents.     

Micro scale 3D FEM simulation on thermal evolution within the porous structure in selective laser sintering

A micro scale 3D finite element model (FEM) with consideration of powder arrangements was developed by selective laser sintering (SLS), where a multi-layer powder stacking model with cubic powders interlaced each other was established to describe the porous powder bed. All the powders directly exposed to laser irradiations were loaded with the Gaussian function of heat flux, and the non-linear thermal conductivity and specific heat owing to temperature change and phase transformation were considered. Comparison between the modeling and experiment indicated that both the simulated length of the sintered piece and shrinkage depth of the powder bed agreed well with the experiment data. The temperature field of laser sintering was intermittent in the micro scale due to the discretely distributed particles with maximum temperature produced in the top layer of the powder bed, and two primary ways of bonding were found in the powder bed during laser sintering.     

Thermophysical and Microstructural Studies on Thermally Sprayed Tungsten Carbide-Cobalt Coatings

The development of new hardmetal coating applications such as fatigue-loaded parts, structural components, and tools for metal forming is connected with improvement of their performance and reliability. For modelling purposes, the knowledge of thermophysical, mechanical, and other material data is required. However, this information is still missing today. In this study, the thermophysical data of a WC-17Co coating sprayed with a liquid-fuelled HVOF-process from a commercial agglomerated and sintered feedstock powder from room temperature up to 700 °C was determined as an example. The dependence of the heat conductivity on temperature was obtained through measurement of the coefficient of thermal expansion, the specific heat capacity, and the thermal diffusivity. Heat conductivities ranging from 29.2 W/(mK) at 50 °C to 35.4 W/(mK) at 700 °C were determined. All measurements were performed twice (as-sprayed and after the first thermal cycle) to take into account the structural and compositional changes. Extensive XRD and FESEM studies were performed to characterize the phase compositions and microstructures in the as-sprayed and heat-treated states. Bulk samples obtained by spark plasma sintering from the feedstock powder were studied for comparison.     

Pressureless sintering of ZrC-based ceramics by enhancing powder sinterability

The sinterability of ZrC was enhanced by high-energy ball milling as well as introduction of graphite and SiC as sintering additives. Densification process and microstructure development were investigated for ZrC-based ceramics densified by pressureless sintering. As-received ZrC powder showed poor sinterability. After high-energy ball milling, ZrC powder can be sintered to 98.4% theoretical density at 2100 °C. The obtained ceramic had fine microstructure and fewer entrapped pores. Introduction of 2 wt.% graphite combined with high-energy ball milling lowered the densification temperature of ZrC. The relative density of obtained ceramic reached up to 95% at 1900 °C. Introduced SiC inhibited ZrC grain growth during sintering and consequently avoided the entrapped pores within the grains. The relative density of ZrC-SiC reached up to 96.7% at 2100 °C. ZrC-SiC composite formed an interesting intragranular structure and had high fracture strength at room temperature.     

Thermophysical properties of TiB2SiC ceramics from 300 °C to 1700 °C

In the present work, high-frequency induction heating is used to fabricate TiB₂SiC ceramics and the relative density was more than 97%, and then the thermophysical properties of TiB₂SiC ceramics were investigated in detail. The specific heat showed the weak dependence on the test temperature due to the presence of the interface gap because the relative density was not 100%. As the sintering temperature increased, the thermal diffusivity of TiB₂SiC ceramics increased, which was due to the increase of relative density and grain growth. The thermal conductivity of TiB₂SiC ceramics showed a marked increase with increasing grain size and relative density. This could be attributed to a reduction in the number of grain boundaries that interrupt the heat flow path, resulting in an increase in the mean free path of the phonons. Larger grains led to an increase of mean free path of the phonons and thus contributed to a further increase in thermal conductivity.     

Comparison between the thermal properties of fully dense and porous NiTi SMAs

In this paper the results and methodology for evaluating the dependence of the thermal properties of porous and fully dense NiTi SMAs on temperature and porosity using an experimental–numerical approach is reported. In the experimental work a cylindrical NiTi sample was uniformly heated at one side and temperature histories at different positions recorded. A variety of heating rates ranging from 10 to 100 K/s and maximum temperature values of 400 K or 1400 K at the top of the NiTi sample were used to carry out experiments. The numerical code based on the 1D unsteady heat diffusion equation considers the sample as a solid featured by the average density depending on its porosity and permits the evaluation of the effective thermal properties. The total heat capacity of each sample is defined on the basis of the transformation latent heat and data reported in literature, while the thermal conductivity is obtained by comparison of the numerical results to the experimental curves. Samples featuring porosity levels of 0%, 30%, 48%, 68% have been tested and the total heat capacity and thermal conductivity dependence on temperature and porosity are defined in the temperature range from 300 K up to 1400 K.     

The effect of sintering temperature on some properties of Cu-SiC composite

Copper matrix composites reinforced with 1 wt.%, 2 wt.%, 3 wt.% and 5 wt.% SiC particles were fabricated by powder metallurgy method. Cu and Cu-SiC powder mixtures were compacted with a compressive force of 280 MPa and sintered in an open atmospheric furnace at 900-950 °C for 2 h. Within the furnace compacted samples were embedding into the graphite powder. The presence of Cu and SiC components in composites was verified by XRD analysis. Optical and SEM studies showed that Cu-SiC composites have a uniform microstructure in which silicon carbide particles are distributed uniformly in the copper matrix. The results of the study on mechanical and electrical conductivity properties of Cu-SiC composites indicated that with increasing SiC content (wt.%), hardness increased, but relative density and electrical conductivity decreased. The highest electrical conductivity of 98.8% IACS and relative density of 98.2% were obtained for the Cu-1 wt.%SiC composite sintered at 900 °C and this temperature was defined as the optimum sintering temperature.     

烧结助剂Y2O3和Pr6O11对Al2O3陶瓷相对密度和热导率的影响

采用高分子网络法制备混合纳米粉体,研究稀土氧化物Y2O3和Pr6O11加入量对Al2O3陶瓷相对密度和热导率的影响。采用阿基米德方法测定样品的体积密度,利用激光脉冲法测量试样的热扩散率并计算得出热导率。结果表明:两种添加剂都可以降低Al2O3陶瓷的烧结温度,提高Al2O3陶瓷的热导率,其中Y2O3的促进作用较强;当保温时间相同、烧结温度为1 500~1 650℃时,Al2O3陶瓷的相对密度和热导率都随烧结温度的升高而增大;当烧结温度相同、保温时间为30~120 min时,Al2O3陶瓷的相对密度和热导率也随保温时间的延长而增大。     

Sintering and annealing effects on ZnO microstructure and thermoelectric properties

The influence of different thermal treatments on zinc oxide has been investigated regarding the thermal diffusivity and structural properties of doped and undoped samples. ZnO powders having various grain sizes and morphologies, with or without aluminum doping, have been prepared under different temperatures by spark plasma sintering (SPS). The microstructural properties and thermal diffusivities of the prepared samples have been measured before and after annealing treatments in air at 800 °C. In undoped samples, the crystallite sizes increased after the annealing treatments, while it was retained in the Al-doped samples. The thermal diffusivities, microstrain and degree of preferred orientation were affected by the SPS temperature and the annealing; however, the general trends were retained after the annealing treatments. Lower maximum temperature yielded a lower degree of preferred orientation, less microstrain, higher density of grain boundaries, lower thermal diffusivities and, for Al-doped samples, lower electrical conductivity and a difference in zT-values from 0.2 to 0.3 at 800 °C. Calculations of the wavelengths and mean free paths of the phonons that contribute to the main part of the thermal conductivity have been conducted and reveal that nanostructures <12 nm are required to lower the thermal conductivity by quantum confinement.     

The effects of heat treatment and gas atmosphere on the thermal conductivity of APS and EB-PVD PYSZ thermal barrier coatings

The effects of heat treatment and gas atmosphere on thermal conductivity of atmospheric plasma sprayed (APS) and electron beam physical vapor deposited (EB-PVD) partially Y₂O₃ stabilized ZrO₂ (PYSZ) thermal barrier coatings (TBCs) were investigated. Two-layer samples that had an EB-PVD coating deposited on bond coated nickel-base superalloy IN625 substrates, free-standing APS and EB-PVD coatings as well as a quasi-free-standing EB-PVD PYSZ coating (coating on semitransparent sapphire) were included in the study. Thermal diffusivity measurements for determining thermal conductivity were made from room temperature up to 1150 °C in vacuum and under argon gas using the laser flash technique. To investigate the effect of heat treatment on thermal conductivity, coatings were annealed at 1100 °C in air. For both the APS and EB-PVD PYSZ coatings the first 100 h heat treatment caused a significant increase in thermal conductivity that can be attributed to microstructural changes caused by sintering processes. Compared to the measurements in vacuum, the thermal conductivity of APS coatings increased by about 10% under argon gas at atmospheric pressure, whereas for the EB-PVD coatings, the influence of gas on thermal conductivity was relatively small. The effect of gas on the thermal conductivity of APS and EB-PVD PYSZ coatings can be attributed to amount, shape, and spatial arrangement of pores in the coating material.     

A new synthesis reaction of Ti3SiC2 through pulse discharge sintering Ti/SiC/TiC powder

Ti₃SiC₂ was synthesized by pulse discharge sintering 4Ti/2SiC/TiC mixture powder in a temperature range of 1250–1450 °C. The purity of Ti₃SiC₂ was improved to 92 vol% at a sintering temperature of 1350 °C. The microstructure in the synthesized samples was controlled to be fine, coarse and duplex grains, depending on the sintering temperature and time.     

基于包混和复合添加工艺的多孔碳化硅陶瓷的制备和性能

采用包混工艺合成核-壳结构的硅-树脂先驱体粉体,引入Al2O3-SiO2-Y2O3复合添加剂,通过成型、炭化和烧结工艺制备多孔碳化硅陶瓷。分析多孔碳化硅陶瓷样品的物相、形貌、孔隙率、热导率、热膨胀系数和抗热震性能。结果表明：复合添加能够在较低的温度下制得多孔碳化硅陶瓷;陶瓷样品的晶粒较小,明显增强了多孔碳化硅陶瓷的导热性能;复合添加提高了碳化硅陶瓷的抗热震性能,添加Al2O3-SiO2-Y2O3并且在1650℃下烧结制备的多孔碳化硅陶瓷经过30次热震后的抗弯强度损失率为6.5%;陶瓷样品的孔壁更加光滑,孔分布更均匀;复合添加对多孔碳化硅陶瓷热膨胀系数的影响较小。     

High Electrical and Thermal Conductivity of Nano-Ag Paste for Power Electronic Applications

The nano-Ag paste consisted of Ag nanoparticles and organic solvents. These organics would be removed by evaporation or decomposition during sintering. When the sintering temperature was 300 °C, the resistivity of sintered bulk was 8.35×10^-6 Ω cm, and its thermal conductivity was 247 W m^-1 K^-1. The Si/SiC chips and direct bonding copper (DBC) substrates could be bonded by this nano-Ag paste at low temperature. The bonding interface, sintered microstructure and shear strength of Si/SiC chip attachment were investigated by scanning electron microscopy, transmission electron microscopy and shear tests. Results showed that the sintered Ag layer was porous structure and tightly adhered to the electroless nickel immersion gold surface of DBC substrate and formed the continuous Ag-Au interdiffusion layer. The shear strength of Si and SiC chip attachments was higher than 35 MPa when the sintering pressure was 10 MPa. The fracture occurred inside the sintered Ag layer, and the fracture surface had obvious plastic deformation.     

High temperature thermo-physical properties and thermal shock behavior of metal–diborides-based composites

The thermo-mechanical properties and thermal shock resistance of two metal diborides composites, HfB₂ with 20 vol.% SiC and HfB₂ with 20 vol.% SiC and 10 vol.% AlN, were investigated. Results showed that the composite HfB₂–SiC–AlN had a higher specific heat capacity than that of composite HfB₂–SiC. However, the occurrence of a Si–Al–O phase in the grain boundaries increased the heat flow resistance at grain boundaries, resulting in decrease thermal diffusivity and thermal conductivity. The calculated thermal shock resistance parameters indicated that the addition of AlN increased the resistance against crack initiation and crack propagation of composite, corresponding to the increase in critical thermal shock temperature difference from 400 to 600 °C.     

The effect of sintering temperature on densification of nanoscale dispersed W–20–40%wt Cu composite powders

Nanoscale dispersed particles of W–20–40%wt Cu were synthesized using a chemical procedure including initial precipitating, calcining the precipitates and reducing the calcined powders. The powders were characterized using X-ray diffraction and map analyses. The effect of sintering temperature was investigated on densification and hardness of the powder compacts. Relative densities more than 98% were achieved for the compacts which sintered at 1200 °C. The results showed that in the case of W–20%wt Cu composite powders, the hardness of the sintered compacts increased by elevating the sintering temperature up to 1200 °C while for the compacts with 30 and 40%wt Cu, the sintered specimens at 1150 °C had the maximum hardness value. The microstructural evaluation of the sintered compacts by scanning electron microscopy showed homogenous dispersion of copper and tungsten and a nearly dense structure. A new proposal for the variation of the mean size and morphologies of W-particles with volume percent of copper melt within the composites has been suggested.     

Low conductivity plasma sprayed thermal barrier coating using hollow psz spheres: Correlation between thermophysical properties and microstructure

Life and thermal properties of plasma sprayed TBCs - widely used in gas turbine engines - are closely related to the microstructure of the ceramic top coating. Especially, the thermal behaviour of this coating is induced by the void shapes and networks which are in turn determined by both the spraying conditions and the feedstock material.A specific hollow yttria partially stabilised zirconia powder was produced in a one-step process by spray drying and an experimental statistical design study was conducted to investigate the influence of spraying variables (primary and secondary gas flow rates, arc current, spraying distance, spraying angle and traverse speed) on structure and properties of resulting plasma sprayed coatings. The coatings were characterized with respect to deposition efficiency, roughness, porosity and thermal conductivity. A reduction of 25% of the thermal conductivity was achieved by improving the spray and powder parameters. A quantitative characterization of the porous structure using image analysis of polished cross-sections was implemented. The parameters that have relevant influence on the coating porous structure were identified, and their relative importance was determined. An attempt was made to identify morphological criteria of the porous network (coarse/fine porosity ratio, cracks total length, cracks orientation) correlating with the thermal conductivity values.     

Si粉粒径及其添加量对SiC陶瓷材料结构和性能的影响

将平均粒径为75 μm和48 μm、质量分数为0%~8%的Si粉分别添加到SiC陶瓷材料中,在1550℃下保温3 h烧成,研究Si粉粒径及其添加量对SiC陶瓷材料烧结性能、力学性能和显微结构的影响。结果表明:添加不同粒径及质量分数的Si粉可改善SiC陶瓷材料的显微结构,提高其烧结性能和力学性能;在一定范围内,较小粒径的Si粉更有利于形成均匀、致密的SiC烧结体,大幅提升SiC陶瓷材料的性能;当Si粉粒径为48 μm且添加的质量分数为4%时,SiC陶瓷材料的烧结性能和力学性能较优,其体积密度和显气孔率分别为2.58 g/cm3和13.5%,抗弯强度和洛氏硬度分别为25 MPa和115 HRB。