壳核式Al2O3-Y2O3 /ZrB2复合粉体的放电等离子烧结行为研究

ZrB2具有优良的物理特性和化学稳定性而应用于许多领域,但是ZrB2难以烧结致密和在高温条件下容易被氧化.为了充分发挥ZrB2的优点,改善ZrB2的缺点,本文采用共沉淀法制备壳核式Al2O3-Y2O3 /ZrB2复合粉体,通过放电等离子烧结法制备高致密的ZrB2-YAG陶瓷.在相同实验条件下得到的纯ZrB2陶瓷的相对密度都很低,在85%以下.通过此种方法加入少量YAG后,烧结密度得到明显提高,随YAG添加量的增加相对密度增加.添加量超过30wt%后,可以达到几乎完全致密的ZrB2-YAG陶瓷.     

Spark Plasma Sintering of Nanocrystalline Niobium Nitride Powders

Nanocrystalline niobium nitride (NbN) powders were sintered by spark plasma sintering under a nitrogen atmosphere at temperatures from 1040° to 1230°C. Fully dense bulk NbN ceramic with grain sizes of 0.5–1.0 μm was obtained at 1130°C. The effects of sintering temperature on the density, phase content, electrical conductivity, Vickers hardness, and microstructure of the NbN ceramic were discussed.     

Consolidation of Nano-Sized TiN Powders by Spark Plasma Sintering

Nano-sized TiN powders with an average particle size of 19 nm were synthesized via a new method, reduction–nitridation reaction in liquid ammonia. A consolidation procedure using spark plasma sintering (SPS) was used, and a dense TiN ceramic (>98% of theoretical) with mean grain size of 100–150 nm was obtained at 1380°C. The influence of sintering temperature on grain growth and microstructural evolution was also discussed.     

放电等离子烧结制备Ti/Al2O3复合材料

Ti基金属复合材料是一种新型高温结构材料.本文利用放电等离子烧结技术,在温度1250℃、压力30MPa、真空度6Pa,保温时间10min条件下,制备了相对致密度较高的Ti/Al2O3复合材料.借助XRD,SEM,EDS等测试手段对该复合材料的物相组成、界面反应、微观结构以及致密度进行了观察与分析.结果表明:利用SPS技术制备Ti/Al2O3的复合材料,晶粒细小且分布均匀,结构致密、2相之间结合状态良好,相对致密度随材料中陶瓷相含量的增多而有所降低.Ti,Al2O32相之间无明显界面化学反应发生.     

Effects of hBN and Y2O3 Addition on Mechanical and Tribological Behavior of SiC Ceramic Matrix Composites Prepared by Spark Plasma Sintering

Silicon - The objective of the present work is to study the mechanical and tribological properties of SiC-hBN such as hardness, density, fracture toughness, friction and wear behavior with and...     

Consolidation of Nanostructured β-SiC by Spark Plasma Sintering

Nanostructured β-SiC, with crystallite size in the range of 5–20 nm in agglomerates of 50–150 nm, was formed by reactive high-energy ball milling and consolidated to a relative density of 98% by sintering at 1700°C without the use of additives. X-ray line broadening analysis gave a crystallite size of 25 nm, while transmission electron microscopy observations showed the crystallite size to be in the range of 30–50 nm. Evidence demonstrating the role of a disorder–order transformation in the densification process is provided by changes in the diffraction peak patterns and in the integral width with temperature.     

Fabrication of Nanostructured Hydroxyapatite via Hydrothermal Synthesis and Spark Plasma Sintering

Hydrothermal synthesis has been used to produce hydroxyapatite (HA) particles with high crystallinity. Such particles of nanorods were used to fabricate HA ceramic by using spark plasma sintering. X-ray diffraction, transmission electron microscope, scanning electron microscope, and the BET method have been used to examine crystallite size, crystallite shape, and the surface area of particles, and grain size of sintered HA ceramics. It was found that the morphology of the nanorods in the HA particles changed to a more equiaxed shape during sintering.     

Spark Plasma Sintering Behavior of Nano-Sized (Ba, Sr)TiO3 Powders: Determination of Sintering Parameters Yielding Nanostructured Ceramics

Nano-powders of BaTiO₃, SrTiO₃, Ba_0.6Sr_0.4TiO₃ (BST64), and a mixture of the composition (BaTiO₃)_0.6(SrTiO₃)₀₄ with particle sizes in the range of 60–80 nm were consolidated by spark plasma sintering (SPS). An experimental procedure is outlined that allows the determination of a "kinetic window," defined as the temperature interval within which the densification process can be kinetically separated from the grain growth one, enabling preparation of dense nanostructured ceramics. The width of this window varied from almost zero for BST64 to 125°C for the (BaTiO₃)_0.6(SrTiO₃)_0.4 mixture. During the densification (sintering) of the (BaTiO₃)_0.6(SrTiO₃)₀₄ mixture, BST64 is formed. The main part of this reaction occurs in a fully densified body through which suggesting that the constitutional phase(s) have a self-pinning effect on the grain growth.     

Spark Plasma Sintering of Al2O3-Ceramic Workpieces for Small End Milling Cutters

Refractories and Industrial Ceramics - Features of the effect of sintering temperature, pressure and duration of isothermal exposure during spark plasma sintering on the structure of Al2O3 ceramics...     

热压烧结与放电等离子脉冲烧结Al2O3-SrFe12O19复相陶瓷的研究

以Al2O3为基体掺人SrFe12O19,在温度为1200℃和1400℃、压力为30MPa下分别采用热压烧结(HP)和放电等离子脉冲烧结(SPS)制备Al2O3—SrFe12O19。采用X射线衍射仪(XRD)、扫描电子显微镜(SEM)分析了产物的物相和微观结构,同时对它们作了力学性能测试。试验结果表明．与HP法相比,采用SPS法制备的Al2O3—SrFe12O19复相陶瓷微观结构更致密,力学性能更好。     

Si3N4-MgO-Al2O3的SPS制备及其力学性能

利用氧化镁(MgO)和氧化铝(Al2O3)作为烧结助剂,采用放电等离子烧结(SPS)方法制备α-Si3N4陶瓷材料。讨论了SPS方法制备氮化硅材料的烧结行为和烧结机理,分析了烧结助剂添加量和烧结温度等影响因素与材料致密度的关系,利用XRD分析了样品的物相组成,SEM观察了样品断口的显微结构,并且测试了样品的力学抗弯强度。结果表明当烧结温度为1300~1500℃,烧结助剂含量为6%~10%时,可以制备出致密度变化范围为64%~96%的α-Si3N4陶瓷材料;当烧结助剂含量为10%时,材料在1400℃即可烧结致密,致密度可达到95%以上。烧结机理为SPS低温液相烧结。材料的力学强度为50~403MPa,并且与密度关系密切。     

Effect of Sintering Temperature and Yttrium Composition on the Densification,Microstructure and Mechanical Properties of Spark Plasma Sintered Silicon Nitride Ceramics with Al2O3 and Y2O3 Additives

Silicon - Three types of silicon nitride ceramics powder blends were sintered by spark plasma sintering at different temperatures and pressures. The relative densities, microstructures, hardness...     

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.     

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。     

Y2O3添加量对Al2O3/ZrO2复合材料烧结行为和热机械性能的影响

研究了Y2O3添加量对Al2O3/ZrO2复合材料烧结行为和热机械性能(高温抗折强度和抗热震性)的影响,并研究了这些性能与物相组成和显微结构间的关系.结果表明:Y2O3在Al2O3/ZrO2复合材料中起稳定ZrO2晶型、改善烧结致密化、提高高温抗折强度和抗热震性的作用.当Y2O3添加量为1%时,试样的烧结性能和高温抗折强度较佳,体积密度、显气孔率和线收缩率分别为3.27 g/cm3、21.95%和7.43%,高温抗折强度达29 MPa;抗热震性则在Y2O3添加量为0.5%时较佳,其残余强度保持率为71%.Y2O3对Al2O3/ZrO2复合材料烧结性能和热机械性能的影响与Y2O3/ZrO2固溶体的形成、Al2O3和ZrO2晶体间的结合程度及试样中微裂纹含量密切相关.     

Effects of Current Confinement on the Spark Plasma Sintering of Silicon Carbide Ceramics

Despite numerous works have recently reported the densification of silicon carbide (SiC) ceramics using the Spark Plasma Sintering (SPS) technique, the effect of the localized electric current flow near the specimen over the liquid phase sintering process of SiC ceramics and on their microstructural features has not been completely addressed. In the present work, two different SPS setups affecting current flow are selected, one based on the ordinary die/punch setup configuration, and the other employing a BN electrically insulating coating on the inner wall of the die to force the electric current to locally flow through the inner graphite foil in contact with the ceramic compact. The effective electrical resistance and the energy consumed during the SPS runs for both setups, as well as the sintering behavior, microstructure, and mechanical properties of the SPSed materials are analyzed. The BN die coating considerably increases the effective resistance of the system, decreases the power consumption, and accelerates the SiC densification. Besides, ceramic specimens experience significantly higher real temperatures than the set values and, accordingly, coarser microstructures and tougher materials than those for the ordinary setting are produced. The thermoelectrical properties of SiC materials are proposed as fundamental in their SPS process, especially when electrical current is forced through the inner part of the SPS setting around the specimen.     

MgO–Al_2O_3–CeO_2复合烧结助剂对放电等离子烧结氮化硅陶瓷致密化和性能的影响

以MgO–Al_2O_3–CeO_2复合体系为烧结助剂,采用放电等离子烧结工艺制备氮化硅陶瓷。研究了MgO–Al_2O_3–CeO_2含量、烧结温度对氮化硅陶瓷显微结构及力学性能的影响;探讨了复合烧结助剂作用下氮化硅陶瓷的烧结机理。结果表明:当混合粉体中Si_3N_4、MgO、Al_2O_3和CeO_2的质量比为91:3:3:3、烧结温度为1600℃时,氮化硅烧结体相对密度(99.70%)、硬度(18.84GPa)和断裂韧性(8.82MPa?m1/2)达最大值,晶粒以长柱状的β相为主,α-Si_3N_4→β-Si_3N_4相转变率达93%;当混合粉体中Si_3N_4、MgO、Al2O3和CeO_2的质量比为88:4:4:4、烧结温度为1600℃时,烧结体抗弯强度(1086MPa)达到最大值。     

Influence of Spark Plasma Sintering (SPS) Conditions on Transmission of MgAl2O4 Spinel

The effects of the spark plasma sintering (SPS) parameters, such as heating rate α, temperature T and soak time t_s, and impurities on in‐line transmission T_in were examined in MgAl₂O₄ spinel. The SPS processing at T = 1300°C for t_s = 20 min with a low heating rate of α = 10°C/min is a preferable condition for attaining higher T_in. For the higher T or the longer t_s, grain coarsening enhanced the coalescence of residual pores and second phase precipitation, resulting to the limited T_in even at the slow α. Although the lower T and longer t_s attained fine and dense microstructure simultaneously, the maximum T_in was limited to about 50%. The limited transmission, particularly in the visible range, can be ascribed to the discoloration caused by the carbon contamination. The carbon contamination arose from the preexisting trace CO₃ impurities, irrespective of the SPS conditions. For the higher α, which is the primary advantage of the SPS technique, the additional carbon contamination occurred from the paper/die and remained as glassy carbon in the matrix. To attain higher T_in by the SPS technique, the lower α and T, and the shorter t_s should be utilized after removing the impurities.     

Neck Formation and Self-Adjusting Mechanism of Neck Growth of Conducting Powders in Spark Plasma Sintering

By using spherical Cu powders as the conducting sintering material, the microstructures of sintered powder particles at different stages in the process of spark plasma sintering (SPS) have been investigated. Theoretical analyses are proposed to quantify the effects of the pulsed direct current on the neck formation and the neck growth of conducting powders. It is found that there is a considerable inhomogeneous distribution of the temperature increase from the particle-contacting surface to the center of the particle when the pulsed current passes through. The temperature at the particle-contacting surface may reach the boiling point of the material, which results in neck formation at relatively low-sintering temperatures through a process of local melting and rapid solidification. The neck growth depends on the local distribution of the current intensity, which is determined by the competition between the neck cross-sectional area and the electrical resistivity increasing with the temperature. Accordingly, we propose that the coarsening of necks follows a "self-adjusting" mechanism, which is likely to be the essential reason for the homogeneous distributions of neck sizes and sizes of fine grains formed in the neck zones during the SPS process.