High‐Hardness Diamond Composite Consolidated by Spark Plasma Sintering

A high‐hardness diamond‐based composite was synthesized by spark plasma sintering (SPS) under 100 MPa, using SiC‐coated diamond powder prepared via chemical vapor deposition (CVD). SiC layers 20–40 nm were uniformly deposited on diamond powders by a rotary CVD technique. The SiC‐coated diamond powder was consolidated with SiO powder by SPS at the sintering temperature of 1873 K, resulting in the formation of fully compacted mosaic microstructure with the Vickers hardness of 36 GPa.     

High‐Strength B4C–TaB2 Eutectic Composites Obtained via In Situ by Spark Plasma Sintering

The in situ synthesis/consolidation of B₄C–TaB₂ eutectic composites by spark plasma sintering (SPS) is reported. Samples for the evaluation of bending strength were cut from specimens with diameters of 30 mm. The sample prepared for the three‐point flexural strength test had fibers of tantalum diboride with diameter of 1.3 ± 0.4 μm distributed in the B₄C matrix, thereby reducing composites brittleness and yielding an indentation fracture toughness of up to 4.5 MPa·m^1/2. Furthermore, the Vickers hardness of B₄C–TaB₂ eutectics formed by SPS was as high as 26 GPa at an indentation load of 9.8 N. The flexural strength of the B₄C–TaB₂ system has been reported for the first time. Some steps were identified in the load–displacement curve, suggesting that micro‐ and macrocracking occurred during the flexural test. Ceramic composites with a eutectic structure exhibited a room‐temperature strength of 430 ± 25 MPa. Compared with other eutectic composites of boron carbide with transition‐metal diborides, room‐temperature strength the B₄C–TaB₂ was 40% higher than that of B₄C–TiB₂ ceramics, demonstrating advantage of the in situ synthesis/consolidation of eutectic composites by SPS.     

Processing Low‐Oxide ZrB2 Ceramics with High Strength Using Boron Carbide and Spark Plasma Sintering

A phase diagram‐assisted powder processing approach is shown to produce low‐oxygen (0.06 wt%O) ZrB₂ ceramics using minimal B₄C additions (0.25 wt%) and spark plasma sintering. Scanning electron microscopy and scanning transmission electron microscopy with elemental spectroscopy are used to identify “trash collector” oxides. These “trash collector” oxides are composed of manufacturer metal powder impurities that form discreet oxide particles due to the absence of standard Zr–B oxides found in high oxygen samples. A preliminary Zr–B–C–O quaternary thermodynamic database developed as a part of this work was used to calculate the ZrO₂–B₄C pseudobinary phase diagram and ZrB₂–ZrO₂–B₄C pseudoternary phase diagrams. We use the calculated equilibrium phase diagrams to characterize the oxide impurities and show the direct reaction path that allows for the formation of ZrB₂ with an oxygen content of 0.06 wt%, fine grains (3.3 μm) and superior mechanical properties (flexural strength of 660 MPa).     

低温放电等离子烧结法制备氮化硅陶瓷

分别以MgO-Al2O3或MgO-AlPO4作为烧结助剂,采用放电等离子体低温快速烧结方法制备了主相为α相的Si3N4陶瓷材料.采用X射线衍射和扫描电子显微镜分析了样品的物相组成和显微结构;研究了烧结助剂及其含量、烧结温度对陶瓷样品的相对密度与力学性能的影响.结果表明:当采用4%质量分数,下同)MgO-4%Al2O3烧...     

High‐temperature strength and plastic deformation behavior of niobium diboride consolidated by spark plasma sintering

Bulk niobium diboride ceramics were consolidated by spark plasma sintering (SPS) at 1900°C. SPS resulted in dense specimens with a density of 98% of the theoretical density and a mean grain size of 6 μm. During the SPS consolidation, the hexagonal boron nitride (h‐BN) was formed from B₂O₃ on the powder particle surface and residual adsorbed nitrogen in the raw diboride powder. The room‐temperature strength of these NbB₂ bulks was 420 MPa. The flexural strength of the NbB₂ ceramics remained unchanged up to 1600°C. At 1700°C an increase in strength to 450 MPa was observed, which was accompanied by the disappearance of the secondary h‐BN phase. Finally, at 1800°C signs of plastic deformation were observed. Fractographic analysis revealed a number of etching pits and steplike surfaces suggestive of high‐temperature deformation. The temperature dependence of the flexural strength of NbB₂ bulks prepared by SPS was compared with data for monolithic TiB₂, HfB₂ and ZrB₂. Our analysis suggested that the thermal stresses accumulated during SPS consolidation may lead to additional strengthening at elevated temperatures.     

放电等离子烧结技术制备熔融石英陶瓷

以熔融石英陶瓷粉体为原料,采用放电等离子烧结(SPS)技术制备了熔融石英陶瓷材料。文章讨论了SPS方法制备熔融石英陶瓷材料的烧结行为和烧结机理,计算了熔融石英陶瓷的析晶温度并与实际测试结果进行了比较。结果表明:利用SPS方法,在短时间内其析晶温度在1150℃以上,且烧结温度为1150℃时,材料的致密度达到了99.7%,熔融石英的烧结是表层熔融烧结机制,烧结过程中压力对致密度的提高贡献很大。     

Spark Plasma Sintering of Alumina

A systematic study of various spark plasma sintering (SPS) parameters, namely temperature, holding time, heating rate, pressure, and pulse sequence, was conducted to investigate their effect on the densification, grain-growth kinetics, hardness, and fracture toughness of a commercially available submicrometer-sized Al₂O₃ powder. The obtained experimental data clearly show that the SPS process enhances both densification and grain growth. Thus, Al₂O₃ could be fully densified at a much lower temperature (1150°C), within a much shorter time (minutes), than in more conventional sintering processes. It is suggested that the densification is enhanced in the initial part of the sintering cycle by a local spark-discharge process in the vicinity of contacting particles, and that both grain-boundary diffusion and grain-boundary migration are enhanced by the electrical field originating from the pulsed direct current used for heating the sample. Both the diffusion and the migration that promote the grain growth were found to be strongly dependent on temperature, implying that it is possible to retain the original fine-grained structure in fully densified bodies by avoiding a too high sintering temperature. Hardness values in the range 21–22 GPa and fracture toughness values of 3.5 ± 0.5 MPa·m^1/2 were found for the compacts containing submicrometer-sized Al₂O₃ grains.     

Rapid Reactive Synthesis and Sintering of Submicron TiC/SiC Composites through Spark Plasma Sintering

Submicrometer TiC/SiC composites were fabricated by a rapid reactive sintering process through spark plasma sintering (SPS) technique using the carbon, titanium, and nanosized-SiC powders without any additive. It was found that the composite could be sintered in a relatively short time (8 min at 1480°C) to 97.9% of theoretical density. After sintering, the phase constituents and microstructures of the samples were analyzed by X-ray diffraction techniques and observed by scanning electron microscopy. The effect of nanosized and microsized SiC additives on the microstructure of TiC/SiC composites was investigated.     

Translucent Yttria‐ and Silica‐Doped Mullite Ceramics with Anisotropic Grains Produced by Spark Plasma Sintering

Translucent, high‐performance, mullite ceramics with anisotropic grains were prepared by the spark plasma sintering (SPS) of a powder mixture consisting of commercial mullite powder, which already contained small amounts of alumina (θ and α) and silica (cristobalite) (≤3 wt% in total), to which 2 and 1 wt% of yttria and amorphous silica was admixed, respectively. The combination of low‐viscosity Y₂O₃–Al₂O₃–SiO₂ transient liquid formation and SPS sintering provided enhanced densification, also provoking anisotropic grain growth (which became exaggerated after 20 min of SPS dwell time), at a relatively low sintering temperature of 1370°C. In this way, it was possible to meet the conflicting demands for obtaining a dense mullite ceramic with anisotropic grains, ensuring good mechanical properties, while preserving a noticeable light transmittance. In terms of mechanical and optical properties, the best results were obtained when SPS dwell times of 5 and 10 min were employed. The as‐sintered samples possessed densities in the range 3.16–3.18 g/cm³, anisotropic grains with an aspect ratio (AR) of 7 and a grain thickness of approximately 0.45 μm, a flexural strength between 350 and 420 MPa, a Vickers indentation toughness and a hardness of approximately 2.45 MPa·m^1/2 and 15 GPa, respectively, and an optical transmittance of between 30% and almost 50% in the IR range.     

Spark Plasma Sintering (SPS) of NASICON Ceramics

Spark plasma sintering (SPS) method was used to obtain dense NASICON ceramics with a high-electrical conductivity, which was compared with conventional solid-state sintering. The fully dense NASICON was achieved at a relatively low-sintering temperature of 1100°C, whereas the apparent density of the specimen prepared by conventional sintering was 74% of the theoretical density. The highest conductivity of 1.8 × 10⁻³ Scm⁻¹ at 25°C, which is comparable to the best value reported, was achieved using the SPS process. Considering the phase, density, and microstructure, it appears that there is more room for improved conductivity by controlling the amount of monoclinic zirconia and the resistive grain-boundary glass phase.     

SPS烧结制备新型荧光玻璃材料

以实验室自制SiO2粉体和商用Ce∶YAG荧光粉为玻璃原料,采用放电等离子体烧结（SPS）技术,在1 200℃保温2 min烧结得到有望用于白光LED封装的Ce∶YAG荧光玻璃。用X射线衍射仪（XRD）、荧光光谱（PL）等方法对制备获得的荧光玻璃样品进行表征。结果显示,烧结并没有破坏Ce∶YAG荧光粉的晶体结构,且荧光玻璃主体相仍为玻璃体,该荧光玻璃在460nm具有强吸收峰,在此波长激发下发射出530 nm左右的黄光。研究结果表明,本实验制备的Ce∶YAG荧光玻璃是一种具有重要应用前景的LED封装用新型荧光材料。     

Dense Iodoapatite Ceramics Consolidated by Low‐Temperature Spark Plasma Sintering

Pb_9.85(VO₄)₆I_1.7, a potential waste form for long‐lived I‐129 immobilization, experiences phase decomposition and thus iodine loss at an elevated temperature above 400°C, presenting a significant challenge for effective management of radioactive iodine. In this work, we report low‐temperature consolidation of dense iodoapatite pellets with above 95% theoretical density by spark plasma sintering (SPS) at temperatures as low as 350°C for 20 min without iodine loss. Microstructure analysis indicates a nanocrystalline ceramic with an average grain size less than 100 nm. Grain growth dominates the sintered microstructure at higher temperatures and longer durations. The dense nanoceramics have significantly‐improved fracture toughness as compared with bulk coarsened grain structures. The effects of sintering temperatures (350°C, 400°C, 500°C, and 700°C) and durations (0–20 min) on microstructure, density, fracture morphology, and mechanical properties including Young's modulus and hardness of bulk samples were investigated. Low temperature densified iodoapatites suggest immense potential of SPS as an advanced materials fabrication technology for the development of waste forms for immobilization of volatile radionuclides including radioactive iodine.     

Deposition of Silicon Carbide/Titanium Carbide Laminar Ceramics by Electrophoresis and Densification by Spark Plasma Sintering

SiC/TiC laminar ceramic composites were fabricated using electrophoretic deposition (EPD) from acetone-based suspensions. The growth rate of the SiC was almost twice that of the TiC at the same deposition voltage and solids loading. Pressureless sintering and spark plasma sintering (SPS) of the composites were investigated. SiC in the composites without sintering additives could not be densified using pressureless sintering, even at 2000°C. SPS, however, could densify the SiC/TiC composites at 1800°C and 35 MPa. The relative density of the SPS sample was 98.9%.     

Preparation of Dense MgB2 Bulk Superconductors by Spark Plasma Sintering

Fully dense MgB₂ bulk specimens (∼higher than 99% dense) were prepared using spark plasma sintering (SPS) at 1250°C for 15 min. Microstructure analyses revealed that faceted MgO particles of ∼8% volume fraction were dispersed in the MgB₂ matrix. A sharp superconducting transition with an onset temperature of 38.5 K was confirmed by both magnetization and resistivity measurements.     

Preparation and Properties of Lead Zirconate Stannate Titanate Sintered by Spark Plasma Sintering

Lanthanum-doped lead zirconate stannate titanate ceramics were successfully compacted to full density by spark plasma sintering (SPS). SPS samples densified at 900° or 950°C exhibit nearly full density and fine grain size (about 300 nm). Compared with samples from conventional sintering (CS), SPS samples show larger permittivity accompanied by a deterioration in dielectric loss and special strain hysteresis loops similar to those of ferroelectric relaxors, with a diffuse AFE–FE phase transition and less field-induced longitudinal strain. The differences in the properties of SPS and CS materials are attributed to the variations of the resultant microstructures, especially the grain size, of the ceramics.     

Preparation of Textured Bismuth Titanate Ceramics Using Spark Plasma Sintering

Textured bismuth titanate ceramics were successfully produced using spark plasma sintering and platelike bismuth titanate particles prepared using a molten-salt method. The microstructure and dielectric properties of the samples were investigated. The results showed that the dielectric property of the textured bismuth titanate ceramics was anisotropic in various directions and that spark plasma sintering was an effective sintering technology to obtain textured, dense bismuth titanate ceramics at a low temperature.     

Spark plasma sintering of ZrB2- and HfB2-based Ultra High Temperature Ceramics prepared by SHS

The combination of the SHS technique and the Spark Plasma Sintering (SPS) technology was adopted in this work for the fabrication of fully dense MB₂-SiC and MB₂-MC-SiC (M = Zr, Hf) Ultra High Temperature Ceramics (UHTCs). Specifically, Zr or Hf, B₄C, Si, and (for the cases of ternary systems) graphite powders were first reacted by SHS to successfully form the desired composites. The resulting powders were then subjected to consolidation by SPS. In particular, by setting a dwell temperature level of 1800°C, a mechanical pressure of 20 MPa, and a non-isothermal heating time of 10 min, products with relative densities ≥98.5% were obtained for the all systems investigated within 30 min of total processing time. The characteristics of the resulting dense UHTCs, i.e. hardness, fracture toughness, and oxidation resistance, are similar to, and in some cases superior than, those related to analogous products synthesized by alternative, less rapid, methods. The article is published in the original.     

放电等离子烧结致密单相钛三铝碳二的反应机理

以3Ti/1.1Al/1.9C混合粉末为原料,采用放电等离子烧结(SPS)技术,利用X射线衍射仪、扫描电子显微镜和透射电子显微镜等分析方法,研究了致密单相Ti3AlC2三元层状化合物的合成机理,详细探讨了烧结温度对产物合成的影响,提出了一种SPS制备致密单相Ti3AlC2的反应机理。结果表明:利用SPS技术,在1 350℃保温10min的条件下,可以获得致密度大于99%的层状致密单相Ti3AlC2材料。最终产物中TiC的残留与原料中C含量有密切关系,适当降低原料中C含量有利于最终产物中TiC的消除。致密单相三元层状化合物Ti3AlC2的合成过程中,AlTi3和TiAl是形成TiC和Ti2AlC的主要中间相,而Ti3AlC2是由TiC与Ti2AlC反应生成的。     

放电等离子烧结Si3N4陶瓷

本文用放电等离子烧结法制备Si3N4陶瓷,通过排水法测定密度,X射线衍射法测定物相变化,透射电镜进行微观形貌的观察。发现在烧结过程中,当高于1450℃时MgO—CeO2与氮化硅粉末表面的SiO2反应形成硅酸盐液相,促进烧结致密化,冷却后形成玻璃相留在品界,氮化硅的致密化在1500℃接近完成,但高于1550℃时,出现MgO自析晶,微观形貌为相互交织的等轴状的α—Si3N4和柱状的β—Si3N4晶粒。     

放电等离子合成Ti_4AlN_3块体的相形成及显微结构

采用放电等离子烧结和热处理工艺制备相对密度为99.6%的Ti4AlN3块体材料。用X射线衍射、扫描电子显微镜和能谱仪等分析测试手段研究Ti4AlN3的相形成及显微结构。结果表明：在900℃以下,Ti和Al反应生成金属间化合物TiAl3;在900～1200℃,TiAl3和TiN反应生成Ti2AlN;在1200～1300℃...