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.     

金刚石表面形成Ti3SiC2的反应机理

采用Ti、Si、TiC、金刚石磨料为原料,通过放电等离子烧结(SPS),制备了Ti3SiC2陶瓷结合剂金刚石材料.研究结果表明,Ti-Si-2TiC试样经SPS加热的过程中位移、位移率和真空度在1200℃时发生明显变化,表明试样发生了物理化学变化.XRD分析结果表明1200℃时试样发生化学反应生成了Ti3SiC2.随着温度升高,试样中Ti3SiC2含量逐渐增加.当烧结温度为1200℃、1300℃、1400℃和1500℃时,产物中Ti3SiC2含量分别为65.9%、79.97%、87.5%和90.1%.在Ti/Si/2TiC粉料中添加适量的金刚石5%和10%进行烧结,并未抑制Ti3SiC2的反应合成.SEM观察表明,金刚石与基体结合紧密,同时其表面生长着发育良好的Ti3SiC2板条状晶粒.提出了一种金刚石表面形成Ti3SiC2的机制,即金刚石表面的碳原子首先与周围的Ti反应生成TiC,然后TiC再与Ti-Si相发生化学反应,生成Ti3SiC2.     

高能球磨结合SPS技术制备Al2O3-TiC复合材料及其性能研究

以TiO2、Al、C(石墨)为原料,首先采用高能球磨引导铝热反应合成了Al2O3-TiC纳米复合粉体,然后采用放电等离子体烧结纳米复合粉体制备了Al2O3-TiC复合材料.结果表明,在氩气氛围下高能球磨3h后,原料粉末就发生了铝热反应,合成的Al2O3-TiC复合粉体粒子尺寸大约在100nm左右.采用SPS技术在1450℃保温4min烧结的试样致密度达99.6%,并且结构精细(大部分晶粒＜1μm),两相分布比较均匀,有较好的力学性能和电导性能,抗弯强度为650+21MPa,硬度为19.1±0.2GPa,断裂韧性为4.5±0.2MPa·m1/2,电导率为2.3828×105Ω-1.m-1.     

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。      

钛表面激光熔覆原位制备Ti5Si3涂层结构及摩擦学性能

利用激光熔覆技术在钛表面预置硅粉原位制备了Ti5Si3涂层.用XRD、SEM和TEM分析了涂层的组成和组织结构.在UMT摩擦磨损试验机上对Ti5Si3涂层在不同载荷和不同滑动速度下的摩擦磨损性能进行了测试.实验结果表明:涂层的物相主要是Ti5Si3相和基材Ti相,涂层的显微结构为球状和块状晶,Ti5Si3涂层具有较高的显微硬度,涂层截面的平均显微硬度约为840 HV0.2,是钛基材的4.4倍;Ti5Si3涂层可显著提高钛基材的耐磨性能;Ti5Si3涂层的磨损机理为磨粒磨损和粘着磨损.     

无压烧结Ti3SiC2/铝基复合材料组织与性能

MAX相具有独特的层状晶体结构,不但具备常用铝基复合材料外加陶瓷颗粒的性能特征,同时具有可与石墨媲美的摩擦性能.本文以Al粉、Si粉和典型MAX相Ti_3SiC_2为原料,采用冷压成型-无压烧结方法制备了Ti_3SiC_2/Al-Si复合材料,并通过金相显微镜、X射线衍射仪(XRD)、扫描电镜(SEM)、能谱仪(EDS)等分析手段,研究了烧结温度、Si元素含量对复合材料组织与性能的影响.研究表明:随着烧结温度从500℃提高到700℃,复合材料致密度先上升后下降,摩擦系数先降低后上升,硬度逐渐增大至最大值并基本保持稳定;随着Si质量分数从0增加到20.7%,复合材料的致密度逐渐降低,硬度逐渐增大,摩擦系数先降低后增大,晶粒尺寸随之下降,12.5%Si晶粒最为细小;烧结温度为650℃,Si元素质量分数为12.5%的铝基复合材料具有最低的摩擦系数0.18,相应的硬度为62 HV,致密度为92.12%.XRD物相和扫描电镜组织分析表明,复合材料的主要相组成为Al、Ti_3SiC_2,及由界面反应产生的Al_4C_3和Al的氧化产物Al_2O_3.     

原位合成TiB2-TiC0.8-SiC复相陶瓷的微观组织与性能研究

利用热压烧结方法原位合成了TiB2-TiC0.8-SiC复相陶瓷。通过光学显微镜(OM)、X射线衍射分析仪(XRD)和扫描电子显微镜(SEM)对材料物相组成和微观结构进行表征。研究了热压条件下烧结温度对材料物相组成、结构及力学性能的影响。结果表明:烧结温度在1700-1950℃范围内,随着温度的升高,材料的致密度、抗弯强度和断裂韧性都有显著改善。烧结温度为1900℃可得到完全致密的原位合成TiB2-TiC0.8-SiC复相陶瓷,材料的晶粒发育比较完善,条状TiB2和块状TiC0.8晶粒清晰可见。复合材料的维氏硬度、断裂韧性和弯曲强度分别达到23.6 GPa,(7.0±1.0)MPa.m1/2和470.9 MPa。当温度达到1950℃时,由于增强相TiB2晶粒长大,材料的强度降低。TiB2、TiC0.8与SiC颗粒协同,通过裂纹偏转、晶粒拔出、晶粒细化等机制对复合材料起到颗粒增强增韧的作用。     

Ti/Al2O3复合材料制备及其力学性能

利用放电等离子烧结(SPS)制备了性能优异的40%(体积分数)Ti/Al2O3复合材料,其弯曲强度、断裂韧性、显微硬度和相对密度分别为897.29MPa、17.38MPa·m1/2、17.13GPa和99.24%.SEM和HREM对复合材料的微观结构分析发现,晶粒细化、位错环强化等是材料强度提高的主要原因;裂纹的偏转和桥联是材料韧性提高的关键所在.     

激光熔敷Ti5Si3/NiTi2复合材料涂层的组织与耐磨性

以Ti-Si-Ni合金粉末为原料，利用激光熔敷技术在BT9钛合金表面制备出了以金属间化合物Ti5Si3为增强相，以NiTi2为基体的Ti5Si3/NiTi2金属间化合物快速凝固耐磨复合材料涂层，Ti5Si3/NiTi2合材料涂层的硬度高，组织均匀，致密，与基材之间为完全冶金结合，在干滑动磨损试验条件下具有很好的耐磨性。     

Ni和Ti的添加对Al2O3-Ti（C,N）复合材料性能的影响

研究了Ni和Ti的添加对真空热压烧结方法制备的Al2O3-Ti(C,N)陶瓷基复合材料的显微组织和力学性能的影响.发现添加Ni和Ti的复合材料主要由Al2O3、Ti(C,N)和Ni组成,没有发现存在金属Ti.Ti由于非常活泼,在热压烧结过程中可能与石墨模具产生的含C气氛反应生成TiC,或与高温下Ti(C,N)的少量分解产生的N2气氛反应生成TiN,这有利于减少复合材料中的气孔.适量添加Ni可通过液相烧结促进复合材料的致密化,提高复合材料的相对密度,并能通过产生裂纹偏转和裂纹桥联提高复合材料的断裂韧性.热压温度为1550℃、等摩尔比的Ni和Ti混合粉末添加量为5vol%时,Al2O3-Ti(C,N)-Ni-Ti复合材料的相对密度为99.6%,硬度为21GPa,抗弯强度为818MPa,断裂韧性为8.1 MPa.m1/2.     

Magnetic coupling in La0.67Ca0.33MnO3/La0.67Sr0.33CoO3/La0.67Ca0.33MnO3 sandwiches

La_0.67Ca_0.33MnO₃ (LCMO)/La_0.67Sr_0.33CoO₃ (LSCO)/LCMO trilayer films are fabricated on single-crystal substrates NdGaO₃ (110) and the interlayer coupling are investigated. Compared with LCMO single layer, sandwiches showed the enhanced metal-insulator transition temperature of LCMO layers. The magnetoresistance is dependent on spacer thickness and the peak value dramatically decreases when LSCO layer is thick enough because of shorting by the LSCO layer. The magnetic coercivity H_C shows a nonmonotonic behavior with changing spacer layer thickness and the waist-like hysteresis indicates that there is an indirect exchange coupling between the top and bottom LCMO layers across the spacer layer.     

Varistor properties of ZnO-Pr6O11-CoO-Cr2O3-Y2O3-In2O3 ceramics

The varistor properties of the ZnO-Pr₆O₁₁-CoO-Cr₂O₃-Y₂O₃-In₂O₃ ceramics were investigated for different concentrations of In₂O₃. The increase of In₂O₃ concentration slightly increased the sintered density (5.60-5.63 g/cm³) and slightly decreased the average grain size (3.4-2.9 μm). The breakdown field increased from 6023 to 14822 V/cm with increasing concentration of In₂O₃. The nonlinear coefficient increased from 17.6 to 44.6 for up to 0.005 mol%, whereas the further doping caused it to decrease to 36.8. In₂O₃ acted as an acceptor due to the donor concentration, which decreases in the range of 1.02 × 10¹⁷ to 0.24 × 10¹⁷/cm³ with increasing concentration of In₂O₃.     

Microstructures of YBa2Cu3O7/La0.7Ca0.3MnO3 and La0.7Ca0.3MnO3/YBa2Cu3O7 bi-layers grown on (001)LaAlO3

Epitaxial YBa₂Cu₃O₇/La_0.7Ca_0.3MnO₃ (YBCO/LCMO) bi-layers and La_0.7Ca_0.3MnO₃/YBa₂Cu₃O₇ (LCMO/YBCO) bi-layers were grown on (001)LaAlO₃ by pulsed laser deposition, and their microstructures were compared by transmission electron microscopy investigation. In the YBCO(100 nm)/LCMO(150 nm) bi-layers, the LCMO layer consists of columnar grains of ~ 17 nm in diameter and contains mixed orientation domains of [100]_c, [010]_c and [001]_c. The YBCO layer is totally c-axis oriented and the YBCO lattices are tilted − 2.5° to + 2.5° as they grew on the rough surfaces of LCMO columnar grains. For the LCMO(140 nm)/YBCO(140 nm) bi-layers, the LCMO/YBCO interface is sharp and flat. The initial 12-nm thickness of the YBCO layer is composed of c-axis oriented domains, and the upper part of YBCO layer is [100] oriented. The LCMO layer was predominantly [001]_c oriented while [100]_c-oriented domains were occasionally observed.     

Syntheses of hollandite type Rb2Cr8O16, K2Cr2V6O16 and K2V8O16

Hollandite-type compounds, Rb₂Cr₈O₁₆, K₂Cr₂V₆O₁₆ and K₂V₈O₁₆, were synthesized under high P-T conditions up to 1200°C and 7GPa. The structural refinement using a single crystal of Rb₂Cr₈O₁₆ confirms that the structure is similar to that of K₂Cr₈O₁₆. Magnetic measurements indicate that Rb₂Cr₈O₁₆ is ferromagnetic below 295K, K₂Cr₂V₆O₁₆ paramagnetic down to 77K and K₂V₈O₁₆ has susceptibility anomaly at 175K. These compounds are all semiconductive and show discontinuities in temperature-resistivity curves at points corresponding to magnetic anomalies.     

PbSbBiS4-Sb2S3 and PbSbBiS4-Bi2S3 joins in the PbS-Sb2S3-Bi2S3 system

Phase equilibria along the PbSbBiS₄-Sb₂S₃ and PbSbBiS₄-Bi₂S₃ joins of the PbS-Sb₂S₃-Bi₂S₃ system have been studied for the first time using differential thermal analysis, X-ray diffraction, microstructural analysis, microhardness tests, and density measurements, and the phase diagrams of the joins have been mapped out. The joins are shown to be pseudobinary with limited series of terminal solid solutions. The solid solutions are p-type semiconductors.     

Structural study of Sr0.3Ba0.7Nb2O6 and La0.030Sr0.255Ba0.700Nb2O6 ceramic systems

Sr_0.3Ba_0.7Nb₂O₆ (SBN) and La_0.030Sr_0.255Ba_0.700Nb₂O₆ (LSBN) ceramic compounds have been prepared using the traditional ceramic method at two different calcination temperatures (900 and 1000 °C) and later sintered both at 1400 °C. A study of the effects of the calcination temperatures and La substitution on the morphological, compositional, and structural properties of SBN and LSBN is presented using scanning electronic microscopy (SEM), energy dispersive spectroscopy (EDS), and X-ray diffraction (XRD) analysis. From Rietveld refinement processes, the XRD patterns were interpreted to evaluate such effects in the structural parameters and the site occupation factors of the heavy metals and oxygen atoms. The effect of the incorporation of La resulted in a 0.25% cell contraction and turned out to be higher than the 0.08% dilation effect produced by the increase of calcination temperature. The La ion with similar effective ionic radius and higher electronegativity is incorporated into the structure occupying the A₁ site just like the Sr ions in the SBN compound. Differences in the site occupation factors between the SBN and LSBN samples lead to substantial changes in the physical properties such as temperature of relative dielectric constant maximum, relative dielectric constant, and dielectric loss, correlated with the distortion and the relative orientation of the oxygen octahedra.     

Nanocrystallization of SrBi2Nb2O9 from glasses in the system Li2B4O7---SrO---Bi2O3---Nb2O5

Transparent glasses in the system (100−x)Li₂B₄O₇–x(SrO---Bi₂O₃---Nb₂O₅) (10≤x≤60) (in molar ratio) were fabricated by a conventional melt-quenching technique. Amorphous and glassy characteristics of the as-quenched samples were established via X-ray powder diffraction (XRD) and differential thermal analyses (DTA) respectively. Glass–ceramics embedded with strontium bismuth niobate, SrBi₂Nb₂O₉ (SBN) nanocrystals were produced by heat-treating the as-quenched glasses at temperatures higher than 500 °C. Perovskite SBN phase formation through an intermediate fluorite phase in the glass matrix was confirmed by XRD and transmission electron microscopy (TEM). Infrared and Raman spectroscopic studies corroborate the observation of fluorite phase formation. The dielectric constant (_r) and the loss factor (D) for the lithium borate, Li₂B₄O₇ (LBO) glass comprising randomly oriented SBN nanocrystals were determined and compared with those predicted based on the various dielectric mixture rule formalism. The dielectric constant was found to increase with increasing SBN content in LBO glass matrix.     

静电纺丝法制备的Co0.6Ni0.3Cu0.1Fe2O4和Co0.6Ni0.3Zn0.1Fe2O4纳米纤维的结构及磁性能

采用静电纺丝技术制备出表面光滑、直径均匀的Co_(0.6)Ni_(0.3)Cu_(0.1)Fe_2O_4/PVP和Co_(0.6)Ni_(0.3)Zn_(0.1)Fe_2O_4/PVP纳米纤维前驱丝,经500~900℃煅烧后得到Co_(0.6)Ni_(0.3)Cu_(0.1)Fe_2O_4和Co_(0.6)Ni_(0.3)Zn_(0.1)Fe_2O_4纳米纤维。用TG-DSC、XRD、SEM及VSM现代测试分析手段对Co_(0.6)Ni_(0.3)Cu_(0.1)Fe_2O_4和Co_(0.6)Ni_(0.3)Zn_(0.1)Fe_2O_4纳米纤维的结构、形貌及磁学性能进行测试表征。结果表明:在空气气氛中经500~900℃煅烧后可得到纯尖晶石相、结晶度良好的纳米纤维或短纤维;当温度为700℃时,Co_(0.6)Ni_(0.3)Cu_(0.1)Fe_2O_4和Co_(0.6)Ni_(0.3)Zn_(0.1)Fe_2O_4纳米纤维的形貌细长而光滑且直径相对均匀,大约为80nm;此时Co_(0.6)Ni_(0.3)Cu_(0.1)Fe_2O_4纳米纤维则保有较高的剩磁比(M_r/M_s)及矫顽力,分别为0.56和1 088.87Oe。在500℃、600℃、700℃、800℃、900℃煅烧后,Co_(0.6)Ni_(0.3)Zn_(0.1)Fe_2O_4纳米纤维的饱和磁化强度分别比Co_(0.6)Ni_(0.3)Cu_(0.1)Fe_2O_4纳米纤维增大了14.5%、7%、16%、10.7%、8%,而矫顽力则分别降低了38%、51%、50%、46%、46.7%。两种纳米纤维的饱和磁化强度及矫顽力存在差异,为CoNi铁氧体在电磁方面的应用提供了很好的参考。     

Vapour-liquid equilibria in the ternary mixtures N2---CH4---C2H6 and N2---C2H6---C3H8

A systematic study was performed with mixtures consisting of N₂, CH₄, C₂H₆ and C₃H₈, to investigate experimentally phase equilibria and caloric properties and to test the accuracy of thermodynamic correlations. The first part of this Paper reports results of T---p---x---y measurements on ternary systems in the range 20 < p < 120 bar and 140 < T < 220 K. The results are compared with data calculated by generalized equations of state.     

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.