放电等离子烧结制备块体非晶合金研究进展

非晶合金又称“金属玻璃”,是由于超快速冷却凝固导致无法有序排列结晶,从而得到的一种长程无序结构。这种非晶合金与存在晶界和位错的普通合金相比,具有更加优异的力学及物化性能。由于粉末状或条状非晶合金在尺寸和性能等方面的限制,因而大尺寸、优异力学性能及软磁性能卓越的块体非晶合金的制备受到了大量关注与探究。放电等离子烧结技术以温度低、效率高、时间短及冷却速率快等优点,被认为是一种具有广阔发展前景的制备方法。对Fe基、Zr基、Al基及Ti基本身的特点,以及通过放电等离子烧结技术制备不同体系块体非晶合金的物理及化学性能的研究进行了较为全面的综述。概述了放电等离子烧结技术的原理及在制备块体非晶合金方面的优势;分析了放电等离子烧结技术和制备的块体非晶合金材料存在的问题,以及采用该技术制备块体非晶合金的发展前景。重点介绍了在采用该制备不同体系的块体非晶合金时,如何通过改变放电等离子烧结参数,或通过再加工、本身粉末添加元素等方法获得大尺寸、优异性能的块体非晶合金。     

SPS烧结制备TiB2/TiC复合材料

采用金属钛粉和碳化硼为初始粉料,利用SPS放电等离子烧结技术制备了致密的纳米结构TiB2/TiC复合材料.并借助XRD、SEM考察了复合材料的相组成和显微结构,利用压痕法和小样品力学性能测试方法(MSP)测定了室温显微硬度、断裂韧性和MSP强度.研究结果表明:利用一步法直接升温至1550℃并保温6 min制备的复合材料,其晶粒尺寸大于1μm,MSP强度为833 MPa.而采用两步法升温至1550℃,然后迅速降低保温温度至1450℃,并保温6 min条件下使金属钛粉和碳化硼同步完成反应、烧结、致密化,生成晶粒细小的TiB2/TiC复合材料,晶粒尺寸大约为200 nm,并且所制备的复合材料力学性能更好,MSP强度达到1095 MPa.     

Hot Deformation Behaviour of SiC/AA6061 Composites Prepared by Spark Plasma Sintering

In this study, Si C/AA6061 composites with different Si C volume fractions(5%, 10%, 15% and 20%) were fabricated by spark plasma sintering. The deformation behaviour of the composites was studied by uniaxial compression test at temperatures from 573 K to 773 K and strain rates between 0.001 s(-)~1.and 1 s(-)~1..Results indicate that the flow stress of Si C/AA6061 composites increases with the increase of Si C volume fraction, with the decrease of deformation temperature and with the decrease of strain rate. The main deformation mechanism of the composites is dynamic recrystallisation(DRX), and the DRX degree depends on the processing parameters of deformation. Higher Si C volume fraction, higher deformation temperature and lower deformation strain rate promote the occurrence of DRX. The strain rate sensitivity and deformation activation energy of Si C/AA6061 composites are calculated. Results show that with the increase in deformation temperature and the decrease in Si C volume fraction, the strain rate sensitivity of the composites increases. From 573 K to 773 K, the average deformation activation energy of 5vol.%Si C/AA6061, 10 vol.%Si C/AA6061, 15 vol.%Si C/AA6061 and 20 vol.%Si C/AA6061 are 207.91, 230.88, 237.7 and249.87 k J mol(-)~1., respectively. The optimum hot working zone of the Si C/AA6061 composites is in the temperature range of 723 K to 773 K at strain rates from 0.1 s(-)~1.to 1 s(-)~1.     

Phase Formation and Superconductivity of Nb3Al Bulk Materials Prepared by Spark Plasma Sintering and Powder Metallurgy

Journal of Superconductivity and Novel Magnetism - Although various methods have been used to prepare Nb3Al superconducting materials to accelerate their commercialization, the preparation of Nb3Al...     

SPS快速烧结制备纳米结构Ti5Si3-TiC复合材料

采用金属钛和碳化硅为初始原料,采用放电等离子体快速烧结(SPS)技术制备了致密纳米结构的Ti5Si3-TiC复合材料.借助XRD、SEM和TEM考察了复合材料的相组成和显微结构,利用压痕法测定了其室温显微硬度和断裂韧性.结果表明利用SPS技术可在1260℃,保温8 min条件下使金属钛和碳化硅同步完成反应、烧结、致密化,生成Ti5Si3-TiC复合材料,并且晶粒细小,其中TiC晶粒尺寸＜200nm.     

Preparation of In2O3-Sr2RuErO6 Composite Ceramics by the Spark Plasma Sintering and Their Thermoelectric Performance

In1.94Zn0.03Ge0.03O3 and Sr2RuErO6 composite ceramics have been prepared by the spark plasma sintering (SPS) technique. Microstructure studies show that the Sr2RuErO6 phases are randomly dispersed in the In1.94Zn0.03Ge0.03O3 matrix. The results show that the Seebeck coeffcient increases with increasing the amount of Sr2RuErO6, while the thermal conductivity of the composite samples is lower than that of the In1.94Zn0.03Ge0.03O3 ceramic. The thermal conductivity of the 7 vol.% Sr2RuErO6 sample can decrease to 2.15 W·m-1·K-1 at 973 K, and the evaluated maximum ZT value is 0.23 for 3 vol.% Sr2RuErO6 samples at 973 K, which makes them promising materials for the thermoelectric devices.     

放电等离子合成Ti3AlC2-TiB2复合材料的相形成研究

采用放电等离子烧结工艺,以Ti,Al,B4C,Tic为原料制备Ti3AlC2/TiB2复合材料.通过X射线衍射分析了从600℃到1 300℃Ti3AlC2/TiB2系统反应过程的相形成规律.用扫描电镜观察了不同温度下试样的显微组织演变.结果表明,在900℃之前,主要的反应是Ti和AJ反应生成Ti-A1金属问化合物,900℃之后,Ti-Al金属问化合物与TiC逐渐生成Ti3AlC2和TiB2相,形成致密Ti3AlC2/TiB2复合材料.     

放电等离子合成Ti3AlC2/TiB2复合材料的制备及性能研究

采用放电等离子烧结方法研究了Ti3AlC2/TiB2复合材料的制备和不同TiB2含量(体积百分数)对Ti3AlC2/TiB2性能的影响.研究表明,在1 250℃,30 MPa压力和保温8 min条件下烧结,可以得到相对密度达98%以上的致密Ti3AlC2/TiB2块体材料;在Ti3AlC2中添加TiB2能大幅度提高材料的硬度;Ti3AlC2/TiB2维氏硬度达到10.39 GPa,电导率达到3.7×106 S·m-1当TiB2含量为10%时,抗弯强度为696 MPa,断裂韧性为6.6 MPa·m1/2,但当TiB2含量继续增加时,由于TiB2的团聚和TiB2抑制Ti3AlC2晶体的生长导致了材料的抗弯强度和断裂韧性的下降.     

The effect of Bi1.5Zn0.5Nb0.5Ti1.5O7 cover layer on the dielectric and tunable properties of Ba0.6Sr0.4TiO3/Bi1.5Zn0.5Nb0.5Ti1.5O7 bilayered thin films

Bi_1.5Zn_0.5Nb_0.5Ti_1.5O₇ (BZNT) thin films with different thicknesses as cover layers were deposited on the Ba_0.6Sr_0.4TiO₃ (BST) thin films on the Pt/Ti/SiO₂/Si substrates by radio frequency magnetron sputtering method. The microstructure, surface morphology, dielectric and tunable properties of BST/BZNT heterogeneous bilayered films were investigated as a function of the thickness of BZNT films and the effect of BZNT films on the asymmetric electrical properties of BST/BZNT bilayered films was discussed. It was found that BZNT cover layer significantly improved the leakage current and the dielectric loss, and the dielectric constant and tunability of BST/BZNT bilayered thin films simultaneously decreased with the increasing thickness of BZNT films. The BST/BZNT bilayered thin film with a 50 nm BZNT cover layer gave the largest figure of merit (FOM) of 33.48 with the upper tunability of 55.38%. The asymmetric electrical behavior of BST/BZNT bilayered films is probably related to an internal electric field caused by built-in voltages at Pt/BST and BZNT/Au interfaces.     

放电等离子快速烧结SiC晶须增强Si3N4BN层状复合材料

采用放电等离子烧结技术（SPS）快速烧结了SiC晶须增强的Si3N4/BN层状复合材料。利用SPS技术，在烧结温度为1650℃，保温15min的条件下，材料的密度可达3．18g/cm^3, 抗弯强度高达600MPa，断裂功达到3500J/m^2。研究表明；特殊的层状结构，SiC晶须的拔出与折断是材料断裂功提高的主要原因。X射线衍射及扫描电子显微镜研究表明：α-Si3N4已经在短短的烧结过程中全部转变成长柱状的β-Si3N4，并且长柱状的β-Si3N4和SiC晶须具有明显的织构。     

放电等离子烧结TiB2过程中Pa第二峰研究

放电等离子烧结TiB2过程中真空室气压Pa有二个峰值,本文对Pa第二峰进行了研究,研究结果表明：Pa第二峰是烧结过程中化学反应导致的气相沉积所致,原始粉末和烧结工艺对Pa第二峰有影响,而Pa第二峰也景响烧结材料的微观结构。     

放电等离子反应液相烧结制备CeB6阴极与性能研究

以氢直流电弧法制备CeH_x纳米粉末, 再采用放电等离子（SPS）反应液相烧结纳米CeH_x和微米B的混合粉末, 制备了高性能CeB₆多晶块体热阴极材料. 研究了SPS制备CeB₆的烧结反应式及反应液相烧结机制, 确定SPS烧结CeB₆的最佳工艺为： 压力50MPa, 烧结温度1500℃, 保温时间5min. 实验结果表明, SPS制备得到了高纯单相CeB6多晶块体, 纯度达到99.89％, 相对密度达到99.61％, 维氏硬度达到2051kg/mm², 抗弯强度达到254.2MPa. 样品在1600℃温度下拐点发射电流密度达到20.38A/cm², 功函数为2.42eV. 与传统制备法相比, SPS制备显著降低了CeB₆的烧结温度, 缩短了烧结时间, 提高了力学和发射性能.     

Comparative Study of Dense Bulk MgB2 Materials Prepared by Different Methods

We report on the results of a comparative investigation of highly dense bulk MgB₂ samples prepared by three methods: (i) hot deformation; (ii) high pressure sintering; and (iii) mechanical alloying of Mg and B powders with subsequent hot compaction. All types of samples were studied by AC susceptibility, DC magnetization, and resistivity measurements in magnetic fields up to ₀ H = 160 kOe. A small but distinct anisotropy of the upper critical field connected with some texture of MgB₂ grains was found for the hot deformed samples. The samples prepared by high pressure sintering as well as by mechanical alloying show improved superconducting properties, including high upper critical fields H _c2 (₀ H _c2 (0) 23 T), irreversibility fields H _irr which are strongly shifted towards higher values H _irr(T) 0.8 H _c2(T) and high critical current J _c (J _c = 10⁵ A/cm² at 20 K and 1 T).     

以铝为助剂结合放电等离子烧结制备Ti3SiC2

以铝为助剂结合放电等离子烧结工艺，在较低温度下快速制备出高纯致密Ti3SiC2块体材料．掺加适量铝能加快Ti3SiC2的反应合成，提高制备材料的纯度，并促进Ti3SiC2晶体的生长和材料的快速烧结致密．在升温速率为80℃／min，z轴压力为30MPa时，材料制备的最佳温度为1200-1250℃．所制备材料经XBD、SEM和EDS分析表明不含TiC和SiC等杂质相，Ti3SiC2为5-25μm的板状结晶．     

热处理温度对纳米晶Ba3(Zn0.4Co0.6)2Fe24O41晶相和X波段吸波特性的影响

采用溶胶-凝胶自蔓延法制备了Ba3(Zn0.4Co0.6)2Fe24O41铁氧体粉末,先将样品在450℃退火2h,然后将其分别在950、1100、1150、1200、1260℃下热处理5h。利用XRD和微波矢量网络分析仪对产物的晶体结构、X波段的电磁性质及其吸波性能进行了表征。实验表明,1200℃和1260℃热处理后的样品主相为六角Z相结构,并且在整个所测频段内都具有很大的磁导率虚部,后者还具有很高的磁导率实部;1mm厚的上述两样品在X波段内其反射功率损耗都在20dB以上,1200℃热处理后的样品反射功率损耗的最大值达43.112dB,上述两样品具有宽频大功率损耗特性,是X波段较为理想的微波吸收剂。     

Structure and microwave dielectric properties of Bi1.5Zn1.0Nb1.5O7 thin films deposited on alumina substrates by pulsed laser deposition

Bi_1.5Zn_1.0Nb_1.5O₇ (BZN) thin films were deposited on polycrystalline alumina substrates by pulsed laser deposition at different substrate temperatures. The phase structure and surface morphology were characterized using X-ray diffractometer (XRD) and atomic force microscopy. Microwave dielectric properties were performed using split-post dielectric resonator method at spot frequencies of 10, 15 and 19 GHz, respectively. The XRD results indicate that the as-deposited Bi_1.5Zn_1.0Nb_1.5O₇ thin films deposited at 650 °C are amorphous in nature. The dielectric permittivity and loss tangent of the amorphous BZN thin films are 75.5 and 0.013 at 10 GHz, respectively. As the measure frequency increased to 19 GHz, the dielectric permittivity slightly decreases and loss tangent slightly increases. BZN thin films were crystallized after the post-annealing by a rapid thermal annealing in air for 30 min. The crystallized BZN thin films exhibit the excellent dielectric properties and frequency responses. The dielectric permittivity and loss tangent of the crystallized BZN thin films are 154 and 0.038 at 10 GHz, respectively.     

硼砂对自蔓延高温合成ZrB2粉体的影响

以ZrO_2、Mg、B_2O_3及Na_2B4O_7为原料,采用自蔓延高温合成技术制备ZrB2粉体。通过FactSage7.0软件计算,从热力学角度研究了该反应体系发生自蔓延反应的可能性。采用X射线粉末衍射物相分析仪、场发射电子扫描电镜-能谱分析对最终产物的物相组成及显微形貌进行检测。分析结果显示,过量的Mg、B_2O_3可有效提高产物中ZrB_2的含量,Mg和B_2O_3分别过量40%(质量分数)、30%(质量分数)为Mg-ZrO_2-B_2O_3体系的较佳配比。基于上述优化配比,研究了用无水硼砂(Na_2B_4O_7)替换原料中B_2O_3对产物ZrB_2含量及晶粒尺寸的影响,当替换量达到15%(质量分数)时,ZrB_2的含量最高,并且随着Na_2B_4O_7替换量的增加,产物的晶粒尺寸由2μm减小至不足0.5μm。     

Synthesis and characterization of the colossal magnetoresistance manganite La1.2(Sr1.4Ca0.4)Mn2O7 by citrate gel

Single-phase La_1.2(Sr_1.4Ca_0.4)Mn₂O₇ has been synthesized from the aqueous solution of metal nitrates and citric acid by the sol-gel technique. Small particle size with high homogeneity of the powder was obtained. The valence of Mn is determined to be 3.45±0.05 by chemical titration. The MR ratio [ρ−ρ(H)]/ρ(H), is 115% (102 K, 1.5 T) for the composition prepared by the citrate route, and is nearly three times larger than that of the sample prepared by solid state reaction.     

Enhanced tunable dielectric properties of Ba0.5Sr0.5TiO3/Bi1.5Zn1.0Nb1.5O7 multilayer thin films by a sol-gel process

Ba_0.5Sr_0.5TiO₃(BST)/Bi_1.5Zn_1.0Nb_1.5O₇(BZN) multilayer thin films were prepared on Pt/Ti/SiO₂/Si substrates by a sol-gel method. The structures and morphologies of BST/BZN multilayer thin films were analyzed by X-ray diffraction (XRD) and field-emission scanning electron microscope. The XRD results showed that the perovskite BST and the cubic pyrochlore BZN phases can be observed in the multilayer thin films annealed at 700 °C and 750 °C. The surface of the multilayer thin films annealed at 750 °C was smooth and crack-free. The BST/BZN multilayer thin films annealed at 750 °C exhibited a medium dielectric constant of around 147, a low loss tangent of 0.0034, and a relative tunability of 12% measured with dc bias field of 580 kV/cm at 10 kHz.