Effect of spark plasma sintering temperature on the phase equilibria and dielectric properties of BaTi2O5 ceramics

The effect of sintering temperature (ranging from 1055 to 1200 °C) on the phase ingredient and dielectric property of the nominal BaTi₂O₅ ceramics (starting with the Ba/Ti of 1:2) fabricated by a spark plasma sintering method were systematically studied. At the first stage, BaTi₂O₅ component was enhanced in the sintering temperature range of 1055–1120 °C; it turned out to be the dominant phase. For these BaTi₂O₅ phase dominated ceramics, the Curie temperature T _c rised on increasing the sintering temperature and saturated around 440 °C with the maximum dielectric constant of 500. Further increasing the sintering temperature, the decomposition of the obtained BaTi₂O₅ into BaTiO₃ extensively happened; the ceramics turned to be the BaTi₂O₅ and BaTiO₃ coexisting state. These ceramics can be characterized by two dielectric anomalies. One at ~420 °C stood for the phase transition of BaTi₂O₅ while the other at ~150 °C stood for the transition of BaTiO₃, which is exceptionally high as the normal BaTiO₃ ceramics. Further increasing the sintering temperature (until 1200 °C) would dramatically enhance the BaTiO₃ phase; the ceramics showed T _c at 130 °C with the maximum dielectric constant of 1800.     

放电等离子烧结制备Ca2Co2O5热电材料及其性能研究

以Co(NO3)2·6H2O、Ca(NO3)2·4H2O为原料,NaOH为沉淀剂,采用化学共沉淀方法制备了前驱物.该前驱物预烧后,利用SPS进行烧结获得纯相Ca2Co2O5块体.分别采用DTA-TG、XRD和SEM对前驱体的热分解过程、Ca2Co2O5的形成过程进行了表征,并对其热导率进行了测试.结果表明在Ph=13.20获得所需化学计量比的前驱物.该前驱物在700～800℃预烧2h后,采用SPS烧结.烧结温度为800℃,压力30MPa,保温时间5min,可以获得纯相Ca2Co2O5块体.断口形貌为层状,晶粒长约1.4μm.热导率随温度的升高而降低.     

Preparation of nanostructured TiO2 ceramics by spark plasma sintering

The effect of spark plasma sintering (SPS) on the densification of TiO₂ ceramics was investigated using a nanocrystalline TiO₂ powder. A fully-dense TiO₂ specimen with an average grain size of ∼200 nm was obtained by SPS at 700 °C for 1 h. In contrast, a theoretical density specimen could only be obtained using conventional sintering above 900 °C for 1 h with an average grain size of 1-2 μm.     

机械合金化和放电等离子烧结制备Y3Al5O12陶瓷

采用机械合金化和放电等离子烧结制备YAG陶瓷,研究了球磨时间对原料颗粒大小和烧结合成YAG纯度的影响,并利用x射线衍射(XRD)、扫描电镜(SEM)等手段对反应过程及产物形貌和物相进行了分析.研究结果表明,机械合金化Y2O3和Al2O3粉体,可明显细化氧化物颗粒,球磨20h后,Y2O3和Al2O3晶粒大小约为34nm和32nm.球磨处理的Y2O3和Al2O3粉体具有很高的活性,促进放电等离子烧结低温反应合成和获得致密的YAG.对球磨20h的粉体在不同温度进行放电等离子烧结,在1200℃即可获得纯YAG陶瓷,在1500℃烧结,可得到相对密度为99.5%的YAG陶瓷.1500℃烧结的块体在可见光范围内透过率为13.8%.     

放电等离子烧结(SPS)YAG陶瓷的初步研究

研究了采用放电等离子烧结(Spark Plasma Sintering SPS),利用高纯的氧化钇和氧化铝,在1500～1700℃,真空度优于10Pa,反应快速合成YAG陶瓷,但试样的致密度不高,而低气孔率是制备透明陶瓷的关键,实验表明,TEOS的掺加和粉料粒度的减小对烧结试样致密度的提高有一定的作用.     

Preparation of nano-grained zirconia ceramics by low-temperature, low-pressure spark plasma sintering

Ce- and/or Y-doped zirconia nanopowders having average particle sizes ranging 12–18 nm have been synthesized by a technique based on mechanochemical processing (MCP). Despite their small particle size, the powders had excellent compactibility with green densities exceeding 50% achieved under a moderate uniaxial pressure of 150 MPa. Nearly fully dense ceramics having grain sizes of around 100 nm were successfully produced from these powders by spark plasma sintering (SPS) at temperatures of 1,050–1,150 °C for 5 min under pressures of 50–80 MPa; these temperatures and pressures are considerably lower than those required for achieving near full density with conventional nanopowders. Hardness and fracture-toughness measurements showed that the ceramics prepared by SPS had superior mechanical properties to those prepared by conventional pressureless sintering. It is argued that the high sinterability of the MCP nanopowders is ascribed to their ability to form uniform powder compacts under relatively low pressure, and that that ability in turn originates in two features of the MCP powders: absence of hard agglomeration and pseudo-spherical particle morphology.     

放电等离子烧结制备透明AlN陶瓷

采用放电等离子烧结(spark plasma sintering,SPS)技术,添加不同含量CaF2为烧结助剂,成功制备了透明氮化铝(AlN)陶瓷.SPS技术具有烧结快速,烧结体致密度高的特点,是制备透明AlN的有效方法.CaF2的加入量的提高,有利于烧结体的致密度和透过率的提高.当CaF2加入量为3%(质量分数)时,烧结体致密度不再继续提高,但仍有利于透过率的提高,此时烧结体透过率最高为54.7%.SEM、XRD、TEM和EDX结果表明烧结体具有很高的致密度、纯度,均匀的晶粒形状和尺寸,晶界及三角晶界处观察不到第二相的存在,从而保证了烧结体良好的光学性能.     

Properties of Mn-doped BaTi4O9-ZnO-Ta2O5 ceramics

In Part I, the reaction sequence, microstructural analysis and microwave dielectric properties of manganese-doped BaTi₄O₉ + ZnO + Ta₂O₅ ceramics are discussed. This composition undergoes complex intermediate reactions during calcination. However, the final crystal phases after the sintering process were identical regardless of calcination temperature. Meanwhile, different calcination temperatures affect the relative volume fractions of the BaZn₂Ti₄O₁₁ phase and result in variations in T _f values. To analyse the microstructure, SEM, TEM and EDS analysis were performed. Mn dopants greatly enhanced the Q factor, up to 11000 at 4.5 GHz, whereas undoped ceramics indicated a high loss, probably due to the formation of Ti³⁺ during sintering in air.     

Transparent ceramics prepared from ultrapure magnesium aluminate spinel nanopowders by spark plasma sintering

We have studied the properties of transparent magnesium aluminate spinel ceramics prepared by spark plasma sintering (SPS) of ultrapure nanopowders. The starting powders, of ? 99.98% purity, ranging in specific surface area from 30 to 160 m²/g, were prepared through the hydrolysis of alcoholic solutions of magnesium aluminum alkoxide complexes, followed by calcination at temperatures from 900 to 1100°C. SPS was carried out at 1450°C, with the holding time at the highest temperature not longer than 15 min. The transparent ceramic samples thus prepared have a transmission of up to 73% in the visible and IR spectral regions (λ = 2.5–5.0 µm). The crystallite size in the ceramics is 0.2–0.4 µm, and their microhardness is HV0.1 = 14.8–16.2 GPa.     

放电等离子烧结技术制备复合梯度靶材的研究

采用放电等离子烧结技术制备了TbFeCo／Ti和Bi2O3／Cu复合梯度靶材,利用扫描电子显微镜和能谱分析仪对材料的微观组织形貌及成分进行了分析。结果表明,合成的复合梯度靶材具有宏观组织不均匀性和微观组织连续性的特征,显微组织中不存在微裂纹。与单一靶材相比,TbFeCo／Ti复合梯度靶材解决了在制造和使用过程中容易碎裂的问题,Bi2O3／Cu复合梯度靶材解决了在溅射过程中的散热问题。     

Synthesis and characterization of Cr2AlC ceramics prepared by spark plasma sintering

The investigation of bulk Cr₂AlC ceramic fabricated by Spark Plasma Sintering (SPS) from coarse powders (CAC10) and fine powders (NCAC10) in the temperature range of 1100-1400 °C was carried out. The XRD results indicate that Cr₂AlC, as major phase, always appears with minor and trace amount of Cr₇C₃ and Cr₂Al respectively in both NCAC10 and CAC10 samples and the amounts of later two phases decrease with increase in temperature. However, the Cr₂AlC phase content in NCAC10 is higher than that of CAC10 sintered at the same temperature. The micrographs of back-scattered SEM show that grains with smaller size and pores with fewer amounts appear in SPSed NCAC10 in comparison to that of CAC10. As consequence, the higher hardness (5.6 GPa) of NCAC10 than that (3.9 GPa) of CAC10 was obtained. The patterns of XRD, microstructure and hardness of samples HPed at 1400 °C for the same composition were also presented for comparison.     

Densification mechanisms in spark plasma sintering of nanocrystalline ceramics

Effect of the particle size on the possible electric discharge during the SPS was examined. Nanoparticle compacts enable accumulation of high electric charge, and discharge under conventional voltages used for the SPS. The critical particle size for the electric discharge is both morphological and material dependent. The early stages of densification of the nanocrystalline powder compact proceed either by the plastic deformation or grain-rotation coalescence and sliding, aided by softening of the particle surfaces. The active densification mechanism depends on the changes both in the mechanical and electrical properties with temperature. Densification of 11 nm nc-MgO particles with low yield stress proceeds by plastic deformation already at 700 °C. However, densification of 34 nm nc-YAG particles with high yield stress proceeds by nano-grain rotation aided by particle surface softening. Densification at the final stages of SPS is associated with diffusional processes, where curvature driven grain growth predominates.     

Microstructure and thermal conductivity of spark plasma sintering AlN ceramics

Abstract

Dense aluminium nitride ceramics were prepared by spark plasma sintering at a lower sintering temperature of 1700°C with Y₂O₃, Sm₂O₃ and Dy₂O₃ as sintering additives respectively. The effects of three kinds of sintering additives on the phase composition, microstructure and thermal conductivity of AlN ceramics were investigated. The results showed that those sintering additives not only facilitated the densification via the liquid phase sintering mechanism, but also improved thermal conductivity by decreasing oxygen impurity. Sm₂O₃ could effectively improve thermal conductivity of AlN ceramics compared with Y₂O₃ and Dy₂O₃. Observation by scanning electron microscopy showed that AlN ceramics prepared by spark plasma sintering method manifested quite homogeneous microstructures, but AlN grain sizes and shapes and location of secondary phases varied with the sintering additives. The thermal conductivity of AlN ceramics was mainly affected by the additives through their effects on the growth of AlN grain and the location of secondary phases.     

Mechanochemical synthesis and spark plasma sintering of hafnium carbonitride ceramics

Submicron powder of non-stoichiometric hafnium carbonitrides (HC_0.5N_0.2) was fabricated by the mechanochemical synthesis method. It was shown that during the first milling stages, primarily reaction between hafnium and carbon took place. The nitridation occurred later when fresh metal surfaces started to form through defragmentation of the brittle layer of a carbon-solid solution. The synthesized powder was consolidated by spark plasma sintering approach to producing dense bulk hafnium carbonitride ceramics. Hardness and fracture toughness measured on consolidated samples were 20.8 ± 1 GPa и 3.5 ± 0.2 MPa?m^1/2, respectively. The obtained results were compared with previously reported data.     

Synthesis and mechanical properties of Ti3AlC2 by spark plasma sintering

In this paper, spark plasma sintering (SPS), after hot isostatically pressing (HIP) method was reported as a new approach to prepare bulk polycrystalline samples of Ti₃AlC₂. The ternary carbide was fabricated by spark plasma sintering (SPS) at a pressure of 22 MPa and temperature of 1250°C. The raw materials, elemental powders of Ti, Al and activated carbon, were pretreated in the following different ways prior to SPS: one way was to obtain porous Ti₃AlC₂ by self-propagating high-temperature synthesis (SHS) from mixture of Ti, Al and C, and then densify the product by SPS; the second way was to synthesize Al₄C₃ from Al and C firstly, and then mix powders of Ti and C with synthesized Al₄C₃ to fabricate bulk Ti₃AlC₂ by SPS. Obtained polycrystalline Ti₃AlC₂ ceramics had excellent mechanical properties: density was 4.24 ± 0.02 g/cm³, flexural strength was 552 ± 30 MPa and fracture toughness (K _IC) was 9.1 ± 0.3 MPa · m^1/2. It could be concluded that SPS method was a useful method to synthesize bulk Ti₃AlC₂ with excellent properties in a very short time and easily sintering process. The optimal conditions to synthesize Ti₃AlC₂ were also discussed.     

Orientation dependence of dielectric and relaxor behaviour in Aurivillius phase BaBi2Nb2O9 ceramics prepared by spark plasma sintering

Grain-oriented Aurivillius phase BaBi₂Nb₂ O₉ ceramics were fabricated using Spark Plasma Sintering (SPS). Their relaxor behaviour was confirmed by a strong frequency dispersion of the dielectric response. The dielectric behaviour has been fitted using different relaxor models. The relaxor parameters are isotropic, while the dielectric constants are highly anisotropic. The piezoelectric constant d ₃₃ is zero perpendicular and parallel to the hot pressing direction, and the P–E response is dominated by losses. The inability to pole the samples at room temperature is consistent with the T _f temperature (∼ ∼115 K) estimated from fitting the experimental data to the Vogel–Fulcher model. This suggests that it may be possible to observe piezoelectric and ferroelectric properties at very low temperatures.     

放电等离子体烧结诱发燃烧反应快速制备MoAlB陶瓷材料

采用Mo/Al/B单质混合粉末为原料,进行放电等离子体烧结（SPS）以制备MoAlB材料。采用XRD和SEM等技术研究了产物的物相组成以及显微形貌。结果表明,以1Mo/1.1Al/1B粉末为原料,在900℃进行烧结,会诱发燃烧反应,生成MoAlB、MoB、Al₈Mo₃等构成的样品。产物中存在较多不规则的、几十微米尺度的气孔。晶粒非常细小,约为亚微米级别。此外有少量的晶须形成。提高烧结温度会促进MoB、Al₈Mo₃等转变为MoAlB材料。同时促进烧结致密化,MoAlB晶粒发育成板条状的细小晶粒。优化原料配比（1Mo/1.2Al/1.05B）和烧结制度（1 150℃,保温5 min）会得到单相的、致密（相对密度为98%）的MoAlB材料。提出一个SPS诱发燃烧反应制备MoAlB的反应机制。首先,当温度升高到Al的熔点以上时,形成Al液相。然后,Mo首先与Al发生化学反应,生成富Al的AlMoX相。反应放出的热量较少,需要在SPS的加热辅助作用下,会诱发燃烧反应的发生。大量的Mo与B也会发生化学反应生成M...