纳米聚晶金刚石的高压高温合成

利用自行研制的二级大腔体静高压装置,通过高温超高压下石墨向金刚石的直接转变,合成出了纳米聚晶金刚石块体材料.合成压力约为17GPa,温度约为2300℃.微区X射线衍射分析表明,石墨转变成了立方相的金刚石,扫描电子显微镜及X射线全谱拟合分析显示,合成出来的金刚石晶粒尺寸约16nm.压痕法测得的样品维氏硬度为100GPa以上.     

对采用三种烧结技术制备的氧化锆的致密化和性能的研究

由氨基乙酸／硝酸盐闷烧方法制备了含8％Y2O3的纳米晶钇稳定氧化锆粉末,用火花等离子体烧结（SPS）、热压（HP）和传统烧结法（CS）研究了其致密性。SPS技术比其余烧结方法优异,能在较低温度和较短烧结时间获取具有均匀形态的致密化材料（≥96％）。经SiX5、热压和传统烧结方法制备的材料,其晶粒尺寸分别是0．21、0．37和12μm。材料的总电导率与晶粒尺寸并无明确关系,但SPS烧结材料的活化能比其余两种致密化方法的稍高。由Vickers压痕法测得的硬度与晶粒尺寸无关,而断裂韧性（由压痕法测得）随晶粒尺寸增大而轻微下降。     

放电等离子烧结SiC/BN复相陶瓷的制备及力学性能

以高纯h-BN和SiC纳米粉体为原料、B_2O_3为烧结助剂,利用放电等离子烧结技术(SPS)快速烧结制备了h-BN–25%SiC复相陶瓷。用X射线衍射和扫描电子显微镜对试样的物相组成和显微结构进行分析,研究了h-BN–SiC复相陶瓷的SPS低温烧结行为及烧结温度对烧结试样的致密度、微观结构及力学性能的影响。结果表明:采用SPS烧结技术,在较低温度下即可获得致密度较高的烧结样品,烧结温度的升高,促进了h-BN晶粒的方向性排列,提高了烧结样品的相对密度。随着烧结温度的提高,晶粒尺寸增大,抗弯强度、断裂韧性和弹性模量增大,并具有相同的变化趋势。样品晶粒细小均匀,不同烧结温度样品的断裂方式相同,主要为沿晶断裂,细小SiC颗粒的钉扎效应、晶粒拔出和裂纹偏转提高了复相陶瓷的断裂强度和断裂韧性。在1 600℃烧结所得试样的综合性能较好,其抗弯强度、断裂韧性和弹性模量分别为289.2 MPa、3.45 MPa·m1/2和150.9 GPa。     

石墨烯纳米片复合氧化锆陶瓷的制备与性能研究

放电等离子体烧结(SPS)技术作为一种比较新的烧结技术已经被广泛用于制备各种材料。本文以3Y-ZrO_2粉体和石墨烯纳米片为原料,采用SPS技术制备了石墨烯纳米片复合ZrO_2陶瓷,利用扫描电镜、透射电镜和X射线衍射仪等对烧结样品的显微结构和晶相进行了表征,同时对所制备材料的密度、显微硬度和断裂韧性进行了测试。结果表明,烧结温度和石墨烯纳米片对所制备样品的显微结构和性能都有显著的影响。随着烧结温度的增加,样品的密度提高,晶粒生长明显。而石墨烯纳米片的引入则显著抑制了ZrO_2晶粒的生长,但是由于分散性问题,其显微硬度和断裂韧性反而略有降低。     

铁含量对放电等离子烧结制备Fe/辉石基复合材料性能的影响

以白云鄂博尾矿为原料,在烧结温度800℃、压力50 MPa条件下,采用放电等离子烧结(SPS)制备Fe/辉石基复合材料,并研究了不同铁含量对其物相、微观结构、密度、维氏硬度的影响。采用XRD、SEM等测试手段本别地分析了样品的物相组成和微观形貌,采用阿基米德排水法测量了样品的致密度。结果表明,铁含量对烧结体的物相、微观结构、致密度和维氏硬度等影响显著,烧结体的密度和维氏硬度随铁含量的增加而增加。     

低压烧结纳米复合WC-Co粉末的研究

对纳米复合WC-10Co粉末进行真空烧结和低压烧结,通过合金组织和性能的比较,证实了低压烧结工艺的优越性,并探讨了晶粒度对合金硬度和抗弯强度的影响.     

添加剂对喷射电沉积纳米晶Co-Ni合金的影响

在氯化镍-硫酸钴体系电解液中采用添加剂喷射电沉积纳米晶Co-Ni合金,测定了其阴极极化曲线.研究了添加剂对阴极过电位、电流效率、镀层中Co含量、镀层的相结构、晶粒尺寸、表面形貌及显微硬度、软磁性能等影响.结果表明:添加剂增加了极化作用,影响了Co、Ni电沉积的动力学过程.当添加剂为2.5g/L时,与未加添加剂相比较,阴极过电位从3.594V增大到4.755 V,电流效率和沉积层中Co含量变化不大,但沉积层晶粒尺寸从12.8 nm明显降低到5.5 nm,维氏硬度从423升高到511,同时Co-Ni合金的软磁性能得以提高.     

ZrO2-TiO2复合粉末的纳米结构及发光性质

采用溶胶-凝胶方法制备了ZrO2-TiO2纳米复合粉末,通过对干凝胶粉的DTA/TG热分析以及粉末样品的X射线衍射(XRD)和透射电镜(TEM)结构表征发现,随着ZrO2含量的增强,550℃热处理的粉末样品晶粒尺寸由14nm左右减小为2～4nm,主晶相由锐钛矿相转化为ZrTiO4相;并且在650℃较低温度下即可获得ZrTiO4纳米晶.粉末的发光性质研究表明,与纯TiO2相比,引入Zr4+的复合粉末其发射光谱发生了8nm的红移;其中0.4ZrO2-O.6TiO2样品发光强度最大,约为纯TiO2粉末的2.4倍.     

纳米金刚石-立方相氮化硅烧结体的高温高压制备与表征

采用直接相变的方法制备出了纳米金刚石一立方相氮化硅的烧结体.将石墨与六方相氮化硅的混合粉末经氮气保护球磨26小时后,在约18 GPa、2000℃的压力／温度条件下进行烧结.对烧结产物的X射线衍射分析和扫描电镜分析表明,烧结体中的石墨和六方相氮化硅全部转变成纳米金刚石和纳米立方相氮化硅.烧结体的硬度测试结果显示其平均维氏硬度约为39 GPa.     

WO_3-SiO_2复合薄膜的烧结温度–相组成–气敏特性关系

以钨酸和正硅酸乙酯(tetraethyl orthosilicate,TEOS)为原料,采用改进的溶胶–凝胶工艺,在Al2O3基底上制备WO3–SiO2复合薄膜,重点考查复合薄膜的烧结温度、物相组成及气敏性三者之间关系。用X射线粉末衍射仪和场发射扫描电子显微镜表征复合薄膜的微观结构,结果表明:在烧结温度为500℃与650℃时,复合薄膜为立方相和正交相混合相,复合薄膜的晶粒尺寸为25～30nm,分布均匀。650℃烧结时,对还原性挥发性有机化合物(volatileorganiccompounds,VOCs)气体中丙酮具有较好的敏感性。750℃烧结时,复合薄膜只有单一的正交相,晶粒尺寸在30nm左右,此时复合薄膜对氧化性气体NO2具有很好的敏感性与选择性,最低响应浓度(体积)为10–7,响应时间为2s,恢复时间约为10s。     

Spark plasma sintering of cobalt ferrite nanopowders prepared by coprecipitation and hydrothermal synthesis

Cobalt ferrite exhibits a high coercivity at room temperature and a strong magnetic anisotropy compared to the other spinel ferrites and, consequently appears as an interesting material for permanent magnets and high-density recording. The magnetic properties depend also on the crystallite size. In order to keep the powder properties in a bulk material, dense nanostructured cobalt ferrite has to be sintered. A field activated sintering process like spark plasma sintering (SPS) may be promising for such challenge. The present paper deals with: (i) the preparation of cobalt ferrite by two methods: coprecipitation and hydrothermal synthesis in supercritical water; (ii) the SPS sintering of the cobalt ferrite nanopowder prepared by coprecipitation. The sintering of the as-processed powder and that obtained after a thermal treatment resulting in the spinel phase has been investigated. The influence of the starting powder and the sintering parameters such as the temperature, the duration of the SPS stage on the grain growth and the densification degree of bulk materials will be presented.     

Densification and properties of zirconia prepared by three different sintering techniques

Densification of nanocrystalline yttria stabilized zirconia (YSZ) powder with 8 mol% Y₂O₃, prepared by a glycine/nitrate smoldering combustion method, was investigated by spark plasma sintering, hot pressing and conventional sintering. The spark plasma sintering technique was shown to be superior to the other methods giving dense materials (≥96%) with uniform morphology at lower temperatures and shorter sintering time. The grain size of the materials was 0.21, 0.37 and 12 μm after spark plasma sintering, hot pressing and conventional sintering, respectively. Total electrical conductivity of the materials showed no clear correlation with the grain size, but the activation energy for spark plasma sintered materials was slightly higher than for materials prepared by the two other densification methods. The hardness, measured by the Vickers indentation method, was found to be independent on grain size while fracture toughness, derived by the indentation method, was slightly decreasing with increasing grain size.     

Transparent YAG obtained by spark plasma sintering of co-precipitated powder. Influence of dispersion route and sintering parameters on optical and microstructural characteristics

A fine-grained (330 nm) yttrium aluminium garnet (YAG) ceramic, presenting a non-negligible transparency (66% RIT at 600 nm), was obtained by spark plasma sintering. The YAG powder was manufactured by co-precipitation, starting from a yttrium and aluminium chlorides solution. A soft precursor was obtained, whose phase evolution was studied by X-ray diffraction. Calcined powders were dispersed by either ball milling or by ultrasonication and then subjected to spark plasma sintering at several temperatures (1200–1400 °C) and for a reduced time (15 min). It is shown that the dispersion method plays a key role in enhancing the optical characteristics of YAG ceramics, in order to obtain a material with a small grain size, transparent in both the visible and the infrared range.     

放电等离子烧结La0.67Sr0.33MnO3-δ粉体的输运性质

用自蔓延高温合成技术合成La0.67Sr0.33MnO3-δ粉体.探讨了放电等离子烧结的烧结温度对合成粉体的显微结构和输运性质的影响.扫描电镜和密度测试结果表明:放电等离子烧结后的晶粒大小均匀,烧结体致密度高.随着烧结温度的升高,样品的电阻率明显下降.由于氧缺位的存在,金属-绝缘相转变温度随着烧结温度的升高而降低.相对于传统的固相烧结,放电等离子工艺制得的样品的致密度较高导致颗粒间的巨磁电阻有所提高.     

Formation of Grain Boundaries in Liquid-Phase-Sintered WC–Co Alloys

The origin of WC/WC grain boundaries in liquid-phase-sintered WC–Co alloys has been investigated in a WC–Mo₂C–Co model system using coarse WC polygrain powder. The evolution of grain shape during liquid phase sintering was able to be identified by observing a growth layer that contained Mo. During liquid phase sintering, most of the grain boundaries in the powder were penetrated by a Co liquid but some of them were not. Electron backscattered diffraction analysis confirmed that some boundaries in the powder, in particular, Σ2 twist boundaries and Σ97 special boundaries, remained intact during liquid phase sintering. These experimental results confirm that the grain boundaries of WC grains in liquid-phase-sintered WC–Co alloys originated from those present in the starting powder.     

Characteristics and machinability of lead-free P/M Cu60-Zn40 brass alloys dispersed with graphite

The aim of this paper was to produce a lead-free machinable brass dispersed with graphite particles by powder metallurgy process.The weight of brass powder decreased with increasing the heat treatment temperature over 873 K by vaporized zinc. The voids were also observed according to Kirkendall effect by the difference of diffusion velocity between Cu and Zn at the brass powder surface. In the case of spark plasma sintering, however, zinc vaporization has not occurred because of sealing pressurization and pressure forming. A specimen of brass without graphite particle, sintered at 1053 K by SPS, had a large elongation similar to that of the cast brass alloy.Using the blended brass powder with graphite particles, graphite particles were dispersed in extruded material by applying the SPSed billet. P/M extruded brass alloys with 1 mass% graphite particle was significantly effective to improve their machinability as well as the conventional brass alloys with lead.     

Highly dense spinel ceramics with completely suppressed grain growth prepared via SPS with NaF as a sintering additive

For the preparation of transparent spinel ceramics it is common practice to use LiF as a sintering additive to achieve transparency. However, it is well known that in this case the grain size exhibits a significant increase compared to pure spinel ceramics, which can lead to a deterioration in mechanical properties. The findings of this paper indicate that when NaF is used as a sintering additive for the preparation of spinel ceramics via spark plasma sintering (SPS) translucent materials with a high level of densification can be obtained without observable grain growth. It is shown that the grain size after SPS at 1500 °C with 1 h dwell is essentially the same as the primary particle size of the spinel powder, whereas pure spinel ceramics prepared via SPS under the same conditions exhibit grain growth by approximately a factor 5.     

Spark plasma sintering of lead phosphovanadate Pb3(VO4)1.6(PO4)0.4

Lead phosphovanadates can be used as reactants for the synthesis of iodoapatite. Because of its high chemical durability, iodoapatite has considerable potential interest for immobilizing radioactive iodine. Iodine-bearing compounds must be synthesized and consolidated at low temperatures to avoid iodine volatilization. Spark plasma sintering (SPS) thus appears to be a suitable sintering process because of its short processing time. This paper deals with spark plasma sintering of lead phosphovanadate powder prepared mechanically by attrition and planetary ball milling. The influence of sintering parameters such as the heating rate, temperature, and holding time on the degree of densification and the microstructure of bulk materials is discussed. The bulk characteristics were directly correlated with the shrinkage curves. The powder characteristics were determined (grain size and size distribution, specific area, crystallite size, etc.) to explain the singular sintering behavior of the attrited powder; we also investigated whether the latter exhibited the same singular behavior during conventional sintering and hot pressing.     

Effect of β to α phase transformation on microstructure and thermal conductivity of SiC ceramic densified with Y2O3-MgO additives in argon

SiC ceramic was fabricated by spark plasma sintering of β-SiC powder and Y₂O₃-MgO additives in argon. The effects of β→α phase transformation of SiC on microstructure and thermal conductivity of densified bulks were systematically investigated, in comparison to the counterparts using α-SiC as starting powder. The β→α phase transformation led to a “unimodal to bimodal” transition in grain size distribution. After sintering at 1850 ^oC, the incomplete β→α phase transformation induced the appearance of β/α heterophase boundary with strong effect of phonon-scattering. After sintering at 2050 ^oC, the completion of β→α phase transformation resulted in enlarged grains and disappearance of β/α heterophase boundary in SiC ceramic. The lattice oxygen content was decreased primarily by enhanced grain growth and oxygen picking-up of sintering additives, and possibly some contribution from β→α phase transformation. The optimized microstructure enabled SiC ceramic to obtain a remarkable increase in thermal conductivity from 126 to 204 W/mK after the replacement of α-SiC by β-SiC as starting powder and the accomplishment of β→α phase transformation.     

纳米介电陶瓷的晶粒尺寸效应及低温烧结技术

微电子技术对纳米陶瓷材料的需求催生了各种新型纳米陶瓷材料制备与烧结技术的开发与研究。结合纳米晶介电陶瓷的晶粒尺寸效应（即晶粒尺寸与陶瓷介电特性、烧结特性之间的依赖关系）,系统介绍了制备纳米晶介电陶瓷材料的低温烧结技术,包括液相烧结、两步烧结、水热压烧结和放电等离子体烧结,重点阐述了各种低温烧结技术的基本原理、使用设备、实验参数,比较了其优、缺点和应用领域,综述了近年来国内外相关领域的研究进展,并对这些技术目前存在的问题和今后的研究方向进行了分析和展望。