La2Fe14B和Ce2Fe14B合金在快淬和热处理过程中相析出行为的比较

研究了溶体快淬三元La_2Fe_(14)B和Ce_2Fe_(14)B合金的相析出行为和磁性能,对不同快淬速度(10~50 m/s)和不同热处理温度下制备的样品进行了系统分析。结果表明,通过直接快淬,La_2Fe_(14)B合金中不能形成2∶14∶1硬磁相,而Ce_2Fe_(14)B合金可以获得2∶14∶1相。La_2Fe_(14)B合金在10m/s快淬时主要由La和α-Fe相组成,而Ce_2Fe_(14)B合金中2∶14∶1硬磁相在10m/s和20m/s快淬时析出。随着辊速的增加,非晶相逐渐增多并成为主相。在热处理过程中,La_2Fe_(14)B合金析出相以α-Fe和La相为主,并且高温下液态的富La相和α-Fe相可以共存;而Ce_2Fe_(14)B合金中先析出α-Fe,后析出2∶14∶1硬磁相,随后析出相长大。结果还表明,La_2Fe_(14)B比Ce_2Fe_(14)B有更高的非晶居里温度和更低的α-Fe相析出温度。由于硬磁相的析出,Ce_2Fe_(14)B合金可以获得较好的硬磁性能,包括一定的矫顽力。此研究对含La、Ce稀土永磁材料的生产具有一定的指导作用。     

Fe86Zr5.5 Nb5.5 B3非晶合金的超高压烧结成型

为了获得致密的块状Fe86Zr55Nb55B3纳米晶合金,研究了高压快速烧结工艺参数对样品致密度和α-Fe相晶粒尺寸的影响.结果表明:快淬球磨破碎非晶粉末在5.5 GPa/3min烧结条件下,当Pw=1150 W后,可获得相对密度为98.3%、单相α-Fe纳米晶(16.3 nm)块体合金,且随着Pw和t的增加,样品相对密度和α-Fe相晶粒尺寸均略有增加,样品典型的比饱和磁化强度σs和矫顽力Hc分别为119.6 emu/g,63.8 Oe.     

Fe77Co2Zr9B10Cu2合金的制备及其磁性能

采用单辊快淬法制备了Fe77Co2Zr9B10Cu2合金,在530～750℃等温退火40 min,利用X射线衍射和振动样品磁强计研究了Fe77 Co2 Zr9 B10 Cu2合金的微观结构和磁性能。结果表明:淬态Fe77Co2Zr9B10Cu2合金为非晶、纳米晶双相结构。随着退火温度的升高,α-Fe晶体相从非晶、基体中析出,晶粒尺寸长大,晶化体积分数增加,矫顽力先减小后增大,比饱和磁化强度逐渐增大。实验结果表明,530℃退火后合金的矫顽力最小,在670℃时迅速增大。样品的磁性与其微观结构、晶粒尺寸、晶化体积分数等因素有关.     

Fe78Co2Zr8Nb2B10-xGex（x=1,2,3）合金的晶化过程和磁性能研究

采用单辊快淬法制备Fe78Co2Zr8Nb2B10-xGex(x=1,2,3)系非晶合金,在不同热处理条件下对两种合金进行热处理。利用X射线衍射仪(XRD)、透射电镜(TEM)和振动样品磁强计(VSM)等测试手段对合金的微观结构和磁性能进行研究。研究结果表明,3种合金的晶化过程相似:非晶→非晶+α-Fe(Co)→α-Fe(Co)+Fe3Zr+Fe2B。3种合金的比饱和磁化强度(Ms)大体上随退火温度的升高而增大;3种合金的矫顽力(Hc)随退火温度的升高均呈现先增加、后降低、再增加的复杂变化趋势。     

单晶多孔α-Fe2O3纳米棒的制备及其催化性能

以Fe(NO)3·9H2O和KOH为原料,在100℃下水热反应6h制备了α-FeOOH纳米棒,并在不同温度下对其进行热处理,得到具有一维纳米孔结构的α-Fe2O3单晶.用XRD和TEM对α-FeOOH和热处理产物a-Fe2O3的物相、形貌进行表征,并结合TGA和FT-IR研究了α-FeOOH的热处理过程.结果表明,α-FeOOH在239～295℃温度区间发生脱水相变a-FeOOH→α-Fe2O3.纳米α-Fe2O3很好地保持棒状,但在其表面出现了孔洞,随着温度的升高孔洞趋于愈合.采用DTA考察了α-Fe2O3纳米棒对高氯酸铵(AP)的催化作用.不同温度下热处理得到的α-Fe2O3均使AP的高温分解温度显著降低,其中350℃热处理得到的α-Fe2O3纳米棒使AP高温分解温度最大降幅达71.4℃.     

低温烧结(Zr0.8Sn0.2)TiO4陶瓷的晶相组成与微波介电性能

讨论了低温烧结(Zr0.8Sn0.2)TiO4微波介质陶瓷的晶相组成与制备工艺、掺杂离子的关系,结果表明粉体的合成温度对烧结体的晶相构成有很大的影响,进而影响材料的谐振频率温度系数τf,稍高的合成温度有利于提高α-PbO型ZST相的稳定性,使谐振频率温度系数τf由107 ppm/℃降至20.88 ppm/℃.采用Nb5+离子掺杂能更有效地抑制烧结过程中游离氧化物相的析出,当Nb5+达到0.15mol%时,920℃烧结样品的介电常数为25,谐振频率温度系数τf为-2.44 ppm/℃,品质因数Q·f达4868GHz(5GHz).     

Fe基非晶/纳米晶粉末的放电等离子烧结及磁性能

研究了SPS温度对球磨熔体快淬Fe₇₀Cr₈Mo₂Si₅B₁₅粉末以及MA Fe_73.5Cu₁Nb₃Si_{13 5}B₉ 和Fe₈₀C_o4Nb₇B₉纳米晶粉末的烧结块体合金组织结构与磁性能的影响.结果表明: (1)在30MPa/5min条件下,块体合金相对密度随着烧结温度的升高而增加,当烧结温度为1000℃时,Fe₇₀Cr₈Mo₂Si₅B₁5合金相对密度已达99%以上,当烧结温度进一步升高至1050℃后, Fe_73.5Cu1Nb₃Si1_3.5B₉和Fe₈₀Co₄Nb₇B₉合金相对密度也达到99%;(2)烧结块体合金的主要组成相为α-Fe相,尚存在少量的第二相金属间化合物,这些块体合金α—Fe相的晶粒尺寸均处于纳米级范围内,以Fe₇₀Cr₈Mo₂Si₅B₁₅块体合金的晶粒尺寸为最小,其平均晶粒尺寸约50nm; (3)随着烧结温度的升高,这些块体合金的饱和磁感应强度B_s增大,矫顽力H_c随之降低,以Fe₇₀Cr₈Mo₂Si₅B₁₅块体合金的矫顽力H_c(4.1kA·m^-1)最低.     

纳米复合Pr2Fe14B/α-Fe永磁材料晶化行为和磁性能的研究

利用熔体快淬和晶化处理方法制备了Pr2Fe14B/α-Fe纳米复合永磁材料.采用X射线衍射分析(XRD)、差热分析(DTA)、磁性测量(VSM)等方法对合金的晶化行为和磁性能进行研究.结果发现对于Pr2Fe14B/α-Fe熔体快淬永磁粉末,α-Fe相析出温度对材料升温速率敏感,可通过提高升温速率尽量使α-Fe和Pr2Fe14B两相的析出温度接近,但难以找到一个温度使两相同时大量析出.(Pr8.2Fe86.1B5.7)0.99Zr1淬态合金在963K时,会生成亚稳相Pr2Fe23B3,使磁性能恶化,延长晶化热处理时间或增高晶化热处理温度均可使亚稳相分解.合金在合适的条件下热处理后,材料磁性能较淬态样品有明显提高.     

烧结工艺对贮氢合金La0.67Mg0.33Ni2.5Co0.5的微观组织结构及电化学性能影响的研究

系统研究了固相反应烧结方法制备La0.67Mg0.33Ni2.5Co0.5贮氢合金的烧结工艺对该合金的微观组织结构及电化学性能的影响规律.分析和研究了合金的微观组织结构、电化学放电性能及Mg含量的挥发损失问题.XRD和SEM及EPMA分析结果表明,在不同烧结条件下合金均由不合Mg的LaNi5相、富Mg的LaNi3相及一个贫Mg的LaNix(x=3.0～3.8)相三相组成.当烧结温度不超过1203k时合金主相为LaNi3相,当烧结温度超过1203K,LaNi5相逐步成为主相.原子吸收光谱分析结果表明,烧结温度不超过1203K,Mg元素没有明显损失;当烧结温度超过1203K,会引起Mg的大量挥发损失.电化学性能分析结果表明,烧结温度不超过1203K,合金放电能力主要受合金组织形成与均匀性影响;而烧结温度超过1203K,Mg元素挥发损失成为影响合金放电能力的决定因素.烧结条件为873～1123k保持24h、1203k保持2h,是制备La0.67Mg0.33Ni2 5Co0.5贮氢合金的适宜工艺.用该工艺制备的La0 67Mg0.33Ni2.5Co0.5贮氢合金Mg含量稳定(2.92%质量分数)、微观组织均匀、放电容量高(395mAh/g)、活化性能好(2个循环).     

Nd2Fe14B/α-Fe纳米复相永磁合金微结构的形成

研究了使用不同快淬速度制备的Nd3 6Pr5 4Fe83Co3B5合金中Nd2Fe14B/α-Fe复合纳米晶结构的形成.采用X射线(XRD)、透射显微(TEM)分析技术和振动样品磁强计(VSM)观测和测量了材料的微结构和磁性.结果表明,使用最佳淬速(20m/s)形成的Nd2Fe14B/α-Fe复合纳米晶结构晶粒细小,晶粒尺寸均匀Nd2Fe14B相和α-Fe相的平均晶粒尺寸分别为14nm、16nm.合金中α-Fe相的体积分数为48.6%.纳米晶合金的磁性能为Jr=1.108T,Hc=446.5kA/m,(BH)max=193.6kJ/m3,剩磁比Jr/Js=0.736.     

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.     

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.     

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.     

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.     

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.     

Characterization of YBa2Cu3O7/PrBa2Cu3O7 superlattices

We investigated the structural and superconducting properties ofc-axis oriented (YBa₂Cu₃O₇) _nY /(PrBa₂Cu₃O₇) _npr superlattices with thicknesses of the individual layers down to one unit cell (10nY1; 18>nPr 1). By transmission electron microscopy and X-ray diffraction we find an excellent structural quality of the samples, though the quantitative analysis shows the existence of defects. In superlattices with decoupled YBa₂Cu₃O₇ layers of two unit cell thickness we find a highT _c value of 75 K. We probed the flux line structure in the superlattices by measurements of the critical current density in magnetic fields. The experiments show that the flux-line dynamics is dominated by the movement of pancake vortices.     

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.     

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.