放电等离子超快速烧结 SiC-Al2O3纳米复相陶瓷

本文介绍用非均相沉淀法制备的纳米SiC-Al     

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.     

放电等离子烧结中颈部形成机理探讨

放电等离子烧结(Spark Plasma Sintering,简称SPS)是一种新的固体压缩烧结技术,它具有升温速度快、烧结时间短、冷却速度快、外加压力和烧结气氛可控、节能环保等鲜明特点,成为材料发展和组织优化的有力工具.SPS在材料制备中的应用越来越广泛,但现阶段对SPS烧结过程的认识远未形成统一观点.SPS过程中颈部的形成是一个关键的阶段,影响到整个烧结过程.本文针对火花等离子烧结颈部的形成机理进行分析认为(1)在SPS烧结非金属材料过程中颈部的形成机理可能是塑性变形和蠕变;(2)导电材料烧结颈部形成过程中可能有火花放电现象发生,其主要机理可能是熔化和凝固、塑性变形、蠕变.同时,本文以纯铜为例,对其SPS烧结过程和结果进行了分析,对烧结过程中颈部的形成情况进行观察,并给出了解释.     

放电等离子烧结法制备牙科陶瓷的研究

采用放电等离子烧结(SPS)法制备长石类牙科陶瓷,研究了烧结工艺对其性能的影响。结果表明,在压力30MPa,烧结升温速度100℃/min,烧结温度1120-1300℃下,SPS能够实现长石瓷的高密度烧结,断裂韧性达到1.4MPa·m1/2以上。     

Ti-Al-Al2O3纳米粉体的机械活化-放电等离子烧结

TiAl基合金是很有发展潜力的高温结构材料,为实现快速高效制备此材料,采用新型的机械活化-放电等离子烧结(MA-SPS)制备纳米材料的有效方法,原位制备Ti-Al金属间化合物Ti-47%Al-10%Al2O3(Al为原子分数,Al2O3为质量分数)材料.介绍了放电等离子烧结这种新兴的纳米固体材料制备技术的特点,结合Ti-Al基合金的具体制备工艺,对MA-SPS的特征予以详细分析研究.通过X射线衍射、扫描电镜、透射电镜等分析,经机械球磨活化后,得到晶粒度小于24 nm的纳米单质元素粉体,为后续原位烧结提供合适的烧结原料.其中添加的Al2O3起到细化晶粒、促进纳米化和机械活化、提高出粉率等作用.纳米粉体在合适的参数下经放电等离子烧结后,可得到致密度达98.7%的(TiAl Ti3Al)理想双相组织,其成分的晶粒度小于91 nm,成为纳米固体材料.     

Si 含量对放电等离子烧结原位Nb/ Nb5Si3复合材料显微结构的影响

Nb/ Nb₅Si₃ 是一种新型的高温结构复合材料, 为了降低该材料的制备成本并有效控制材料的显微结构, 本文作者以Nb、Si 粉末为原料, 采用放电等离子烧结(SPS) 技术原位合成了近理论密度的Nb/ Nb₅Si₃ 复合材料, 着重研究了Si 含量对Nb/ Nb₅Si₃ 复合材料显微结构的影响。结果表明: 制备的复合材料由合成的Nb₅Si₃和均匀分布的Nb 颗粒组成; 在原子分数为6 %～20 %Si 范围内, 随着Si 含量增加, 复合材料中Nb₅Si₃ 数量增加, Nb 颗粒尺寸减小, 复合材料的致密性和硬度提高。      

放电等离子超快速烧结 SiC-Al2O3纳米复相陶瓷

本文介绍用非均相沉淀法制备的纳米SiC-Al2O3复合粉体经放电等离子超快速烧结得到晶内型的纳米复相陶瓷,超快速烧结的升温速率为600℃/min,在烧结温度不保温,迅即在3min内冷却至600℃以下.与热压烧结相比,可降低烧结温度200℃以上.力学性能研究结果表明,在1450℃超快速烧结得到的纳米复相陶瓷的抗弯强度高达1000MPa,维氏硬度为 19GPa,断裂韧性也比Al2O3有所提高.TEM像显示纳米SiC颗粒大多分布在Al2O3母体晶粒内,而断裂表面的SEM像表明,穿晶断裂是其主要的断裂模式,这是所制备的纳米复相陶瓷力学性能大幅提高的主要原因.     

放电等离子烧结技术制备Fe78Si13B9块体非晶纳米晶磁性材料

通过高能球磨技术制备了Fe₇₈Si₁₃B₉磁性非晶合金粉体,采用XRD和DSC分析了Fe₇₈Si₁₃B₉非晶合金粉体的相组成、玻璃转变温度T_g、开始晶化温度 T_x 和晶化峰温度T_p;利用放电等离子烧结（SPS）技术在不同烧结温度下制备了块体磁性非晶纳米晶合金试样,利用XRD、SEM、Gleeble3500、VSM等分析了不同烧结温度下烧结块体试样的相转变特性、微观形貌、力学性能和磁学性能。结果表明,在500 MPa的烧结压力下,随着烧结温度的升高,烧结试样中的非晶相开始逐渐晶化,烧结试样的致密度、抗压强度、微观硬度、饱和磁化强度均显著提高;在500 MPa的烧结压力和823.15 K的烧结温度下,获得了密度为6.6 g/cm³,抗压强度为1500 MPa,饱和磁化强度为1.3864 T的非晶纳米晶磁性材料。     

放电等离子烧结技术与新材料研究

详细介绍了放电等离子烧结(spark plasma sintering，SPS)技术的工艺特点、特殊的烧结机理以及设备发展概况。重点阐述了SPS新材料研究开发的国内外发展状况，包括剃度材料、综合性能优异的稀土永磁Nd-Fe-Co材料、热电能源转换材料(CoSb3系列)、纳米WC-Co硬质材料等。最后展望了SPS新材料在中国的发展前景及应该采取的对策。     

放电等离子烧结制备块状纳米晶SmCo5烧结磁体

采用放电等离子烧结（SPS）技术制备了致密纳米晶SmCo5烧结磁体，研究了磁体的结构和磁性能。X衍射结果表明，烧结磁体具有CaCu5结构，说明SPS过程可以获得稳定的1：5相。TEM观察显示，磁体由平均晶粒尺寸约为30nm的1：5相构成。室温时磁体的矫顽力高达2208kA/m，而剩磁比高达0，7，说明在纳米晶之间存在强烈的晶间交换耦合作用。烧结磁体具有良好的高温性能，773K时的矫顽力为456kA/m，矫顽力温度系数β为-0．212％/K。     

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.     

Investigation of the growth of In2O3 on Y-stabilized ZrO2(100) by oxygen plasma assisted molecular beam epitaxy

Thin films of In₂O₃ have been grown on Y-stabilised ZrO₂(100) substrates by oxygen plasma assisted molecular beam epitaxy over a range of substrate temperatures between 650 °C and 900 °C. Growth at 650 °C leads to continuous but granular films and complete extinction of substrate core level structure in X-ray photoelectron spectroscopy. However with increasing substrate temperature the films break up into a series of discrete micrometer sized islands. Both the continuous and the island films have excellent epitaxial relationship with the substrate as gauged by X-ray diffraction and selected area electron diffraction and lattice imaging in high resolution transmission electron microscopy.     

热压与放电等离子体烧结两种工艺制备Al2O3/Cu复合材料

由机械合金化法(MA)制得纳米级Al₂O₃颗粒弥散镶嵌于微米级Cu颗粒表面的复合粉末, 利用球形化工艺改善所制得复合粉的形貌及粒度范围, 分别采用热压法(HP)和放电等离子体烧结(SPS)法制备Al₂O₃/Cu复合材料。通过测试密度、 电导率、 抗弯强度及SEM复合粉形貌和烧结体断口分析、 微区成分分析, 对比研究了Al₂O₃质量分数分别为0%、 0.5%、 1.0%、 1.5%时Al₂O₃/Cu复合材料的物理、 力学和电学性能。结果表明: 不同制备工艺下随着Al₂O₃含量增加, 材料的抗弯强度先增后降, 电导率除受杂质影响外, 还受材料缺陷的影响, 故变化规律不明显, 对于Al₂O₃含量相同的Al₂O₃/Cu复合材料, 采用SPS法制备的复合材料的致密度、 抗弯强度及电导率均高于HP法; 在弯曲应力下两种制备方法所得复合材料均发生延性断裂。      

Synthesis of Mg[Ti2]O4 by spark plasma sintering

We have successfully prepared magnetic frustrated compound Mg[Ti₂]O₄ by a novel technique of spark plasma sintering. X-ray diffraction confirms that the sample is single phase and the spinel parameter a = 8.504(7) Å at the room temperature. The magnetic susceptibility shows that an abnormal drop is exhibited at about 254 K, indicating a magnetic single formation, and that a paramagnetic susceptibility increase which obeys the Curie Law appears below about 150 K, revealing that the number of Ti³⁺ ions which don't take part in spin dimer is about 2.6%. The resistivity shows a jump at the temperature of 254 K, in agreement with the transition temperature of measurement of the susceptibility.     

Microwave sintering of Si3N4 with LiYO2 and ZrO2 as sintering additives

Phase transformation, microstructure development and mechanical properties of 2.45 GHz microwave-sintered silicon nitride (Si₃N₄) with lithium yttrium oxide (LiYO₂) and zirconia (ZrO₂) sintering additives were investigated. It was found that α to β phase transformation completed at a lower temperature of 1500 °C. Scanning electron microscopy (SEM) micrographs revealed a bimodal microstructure with a large number of elongated β-Si₃N₄ grains in addition to smaller grains. Surface residual porosity was observed in all sintered samples due to selective localized over heating of grain-boundary glassy phase. The high aspect-ratio of β-Si₃N₄ grains exhibited significant crack deflection, debonding and pull-out. It was observed that Vickers hardness and indentation fracture toughness increased with increasing sintering temperature.     

Fabrication and mechanical properties of monolithic MoSi2 by spark plasma sintering

Fine MoSi₂ powders containing a small amount of Mo₅Si₃ have been prepared by self-propagating high-temperature synthesis (SHS), followed by spark plasma sintering (SPS) for 10 min at 1200-1500°C and 30 MPa. Dense MoSi₂ materials, in which the grain size is ∼7.5 μm, have been fabricated at 1300°C. They exhibit excellent mechanical properties: Vicker’s hardness H_v (10.6 GPa), fracture toughness K_IC (4.5 MPa m^1/2), and bending strength σ_b (560 MPa). The strength of 325 MPa can be retained up to 1000°C.     

机械合金化和SPS工艺制备9CrWTi-Y2O3/铁素体-马氏体钢

采用机械合金化(MA)和放电等离子体烧结(SPS)工艺制备了9CrWTi-0.35%Y₂O₃氧化物弥散强化铁素体-马氏体钢(9CrWTi-0.35%Y₂O₃/FMs)。利用SPS温度和位移测量装置、 OM、 FE-SEM、 TEM、 EDX表征了材料烧结收缩曲线及热处理前后的显微组织和成分, 并采用电子拉伸试验机测试了室温拉伸性能。结果表明: 9CrWTi/FMs和9CrWTi-0.35%Y₂O₃/FMs在烧结过程出现液相烧结特征。提高烧结温度和压力, 9CrWTi-0.35%Y₂O₃/FMs孔隙度减小, 密度提高, 晶粒变细, 抗拉强度增加, 但延伸率仅为2%左右。富集Y-Ti-O的弥散相颗粒大小为5～20 nm, 较均匀地分布在基体上。9CrWTi-0.35%Y₂O₃/FMs烧结态、 10%盐水淬火态及750 ℃高温回火态的显微组织分别为等轴铁素体、 细长板条马氏体及等轴和残余铁素体。9CrWTi-0.35%Y₂O₃/FMs烧结体经盐水淬火、 回火后, 抗拉强度、 屈服强度和总延伸率由1554 MPa、 1430 MPa、 1.8%变为1198 MPa、 1006 MPa和12.8%。     

Bulk nanocrystalline Al85Ni10La5 alloy fabricated by spark plasma sintering of atomized amorphous powders

Amorphous Al₈₅Ni₁₀La₅ powders were consolidated to cylindrical samples by spark plasma sintering (SPS), and their microstructures and mechanical properties were investigated. When the powders were consolidated below the crystallization temperature, an amorphous phase was retained in the consolidated sample. Sintering above the crystallization temperature caused full crystallization. The Vickers hardness of the amorphous-containing sample was about 350 HV in the as-sintered state and increased up to 450 HV by a subsequent heat treatment just below the crystallization temperature. The highest hardness was achieved in a nanocrystalline microstructure. Compression tests revealed the brittle nature of the consolidated samples although the fracture and yield strength was higher than 1 GPa. The brittleness is due to the low relative density of the amorphous-containing samples and the presence of a large amount of intermetallic compounds in the fully crystallized sample.     

Directionally solidified ZrO2-Ta and ZrO2(Y2O3)-Ta composites

Aligned eutectic composites of unstabilized ZrO₂-Ta and Y₂O₃-stabilized ZrO₂-Ta were grown by direct internal zone melting. Samples with unstabilized ZrO₂ were almost completely crack-free even though the matrix had transformed from the tetragonal to the monoclinic lattice. Stabilized ZrO₂-Ta composites were heavily cracked and exhibited less homogeneous fiber growth. The Ta fiber diameter in unstabilized eutectics decreased from 0.45 to 0.20 μm, as growth rates increased from 4.4 to 27 cm/h. The fracture of the composites always took place in a controlled manner. The reason is plastic deformation of the fibers and subsidiary crack formation within the twinned ZrO₂ matrix. The Ta fiber ductility is caused by solute Zr which reduces the oxygen solubility of Ta considerably.     

Densification and polymorphic transition of multiphase Y2O3 nanoparticles during spark plasma sintering

Multiphase (MP) monoclinic and cubic Y₂O₃ nanoparticles, 40 nm in diameter, were densified by spark plasma sintering for 5-15 min and100 MPa at 1000 °C, 1100 °C, and 1500 °C. Densification started with pressure increase at room temperature. Densification stagnated during heating compared to the high shrinkage rate in cubic single-phase reference nanopowder. The limited densification of the MP nanopowder originated from the vermicular structure (skeleton) formed during the heating. Interface controlled monoclinic to cubic polymorphic transformation above 980 °C led to the formation of large spherical cubic grains within the vermicular matrix. This resulted in the loss of the nanocrystalline character and low final density.