Fe83Zr7B9Mn1非晶合金中α-Fe纳米晶化的HRTEM和结晶动力学研究

通过高分辨透射电子显微镜(HRTEM)和差示扫描量热法(DSC)研究了Fe83Zr7B9Mn1非晶合金中α-Fe纳米晶的结晶过程和非等温结晶动力学。通过HRTEM观察和X射线衍射分析,确定结晶析出相是α-Fe,在经过903K热处理之后,合金内部晶粒尺寸长大至20nm以上。对重叠放热峰进行了分峰拟合。利用Flynn-Wall-Ozawa方法确定了结晶过程的表观激活能Ea=260.3kJ/mol。进一步研究发现Fe83Zr7B9Mn1非晶合金中α-Fe纳米晶非等温结晶过程不适合用Johnson-Mehl-Avrami(JMA)模型描述,而可以利用esták-Berggren自催化模型进行描述。通过计算,α-Fe纳米晶结晶过程的指前因子以及转化函数分别为:lnA=30.6以及f(α)=α0.37(1-α)1.08。     

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.     

铁基非晶磁致低温纳米晶化的相变动力学机理研究

用低频脉冲磁场处理了非晶Fe78Si9B13合金,利用M6ssbauer谱和LDJ9600震动样品磁强计进行了微结构和磁性分析,通过DSC曲线,借助于Kis-singer公式计算了脉冲磁场处理前后样品的纳米晶化过程激活能,探讨了铁基非晶低温纳米晶化的相变动力学机理.结果表明,用脉冲磁场处理非晶Fe78Si9B13合金的晶化激活能由处理前的433.6kJ/mol降到了200kJ/mol以下,大大提高了α-Fe(Si)的形核速率,只有α-Fe(Si)的单相纳米晶体析出,析出相的晶粒尺寸约为10nm,而且脉冲磁场处理过程中,非晶Fe78Si9B13合金试样温升均<10℃,说明脉冲磁场的处理促进了非晶合金的低温纳米晶化.     

Fe74Al4Ga2P12B4Si4块体非晶合金的纳米晶化及软磁性能研究

采用铜模铸造法制备了厚2mm的Fe74Al4Ga2P12B4Si4块体非晶合金.利用X射线衍射(XRD)、差热分析(DSC)和振动样品磁强计(VSM)研究了其晶化行为和软磁性能.结果表明,非晶合金的玻璃转变温度Tg为457.35℃,晶化开始温度Tx为497.65℃.合金的过冷液相区宽度△Tx达到40.30℃,表明合金具有较大的玻璃形成能力.F74Al4Ga2P12B4Si4合金的晶化是二级晶化过程.经520℃等温退火后析出α-Fe相,其晶粒尺寸为15.9nm;而经550℃等温退火后析出α-Fe相及微量的A10.3Si0.7Fe3和Fe3B相,其中α-Fe相的晶粒尺寸为17.4nm.非晶合金的饱和磁化强度为108.816emu/g、矫顽力Hc为574.97Oe;经520℃等温退火后,纳米晶合金的饱和磁化强度为106.875emu/g、矫顽力Hc为94.16Oe.退火实验结果表明,纳米晶化对材料的饱和磁化强度没有显著影响,但会显著降低材料的矫顽力.     

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.     

机械球磨制备纳米双相Nd2Fe14B/α-Fe永磁材料及晶化行为研究

机械球磨氲气保护下的铸态Nd8Fe86B6合金,并进行晶化处理,制备了纳米双相Nd2Fe14B/α-Fe永磁材料.用XRD、TEM和DSC等手段研究了不同球磨工艺和晶化处理工艺对纳米双相Nd8Fe86B6材料组织结构影响.同时研究了非晶态Nd8Fe86B6材料的晶化行为.结果表明延长球磨时间,Nd2Fe14B相迅速细化形成非晶,α-Fe的晶粒尺寸逐渐减小,25h后趋于定值(约为7nm).球磨时间越长,所需完全晶化的温度越高,晶化后粉末的晶粒越小且越均匀.在晶化过程中,非晶态Nd8Fe86B6首先形成Nd4 4Fe77.8B17.8、Nd1.1Fe4B4、Nd2Fe14B和α-Fe四相混合物.升高温度,最后得到Nd2Fe14B相和α-Fe相,但最终产物中仍有少量未分解的Nd1.1Fe4B4相.     

高熵修饰的纳米晶合金Fe–ZrNbMoTa的成形与高温稳定性研究

目的 获得高热稳定性的铁基高熵纳米合金并研究其热稳定性机理。方法 通过高能球磨方法制备了Fe–Zr_xNb_xMo_xTa_x(x=0.1、0.2、0.5、1,原子数分数)单相纳米合金粉末,在不同的退火处理温度下对退火前后的组织演变与元素偏析行为进行表征。结果 获得了尺寸为15 nm的极细FeZr_0.2Nb_0.2Mo_0.2Ta_0.2晶粒,在900℃下退火1h后,平均晶粒尺寸增长到73nm,有第二相Fe₂Ta析出。而纳米晶Fe–Zr_1.0Nb_1.0Mo_1.0Ta_1.0合金在同样条件下退火后尺寸为55 nm,同时观察到Fe₂Ta和FeZr₂析出。结论 高熵元素的加入使该类合金具有较好的热稳定性,而新强化相的析出进一步抑制了高温下的晶粒生长,即Fe–ZrNbMoTa合金在高温...     

铜模吸铸法制备的Fe74Al4Sn2P10Si4B4C2块体非晶与块体纳米晶合金

利用铜模吸铸法制备了直径φ1.0mm和2.0mm的Fe74Al4Sn2P10Si4B4C2块体非晶合金和直径2.0mm的Fe74Al4Sn2P10Si4B4C2块体纳米晶合金圆棒.利用X射线衍射、差示扫描量热仪(DSC)和差热分析仪(DTA)对Fe74Al4Sn2P10Si4B4C2块体非晶合金的结构和热性质进行了测定.该非晶合金的超冷液相区△Tx为16.7K,约化玻璃转变温度Tg/Tm和Tg/T1分别为0.60和0.57.Fe74Al4Sn2P10Si4B4C2合金接近共晶成分,在10K/min的冷却速率下其过冷度可达86.7K.利用透射电子显微镜(TEM)观察了制备态的Fe74Al4Sn2P10Si4B4C2纳米晶合金圆棒的结构,为非晶基体上均匀分布的尺寸10～20nm的α-Fe晶粒.Fe74Al4Sn2P10Si4B4C2合金能达到较大的过冷度,具有较高的约化玻璃转变温度(接近共晶合金成分)和过冷合金熔体的二步相析出有利于块体非晶合金和块体纳米晶合金的形成.铜模吸铸法既可制备块体非晶合金,也可制备块体纳米晶合金,是一种很有吸引力的制备块体非晶合金和块体纳米晶合金的方法,并进一步证实利用快速凝固法可以直接制备块体纳米晶合金.     

机械合金化-放电等离子烧结Al2Cu颗粒增强Al基复合材料的制备

以Al粉和Cu粉为原料,采用机械合金化(MA)和放电等离子烧结(SPS)工艺,原位合成了致密的Al₂Cu/Al块体复合材料,着重研究了MA过程中粉末的形貌、尺寸和物相结构的变化以及SPS后复合材料的微观组织和力学性能。结果表明: 在MA过程中,随着MA时间延长,部分Cu原子逐渐固溶于Al原子晶格中,形成均匀过饱和的固溶体Al(Cu);在SPS过程中,Cu从过饱和固溶体中析出并与Al反应形成Al₂Cu颗粒,且弥散分布于Al基体中,形成Al₂Cu/Al复合材料;Al₂Cu/Al复合材料的致密度高达98.7%,室温下的压缩断裂强度为611.3 MPa,延伸率为9.6%,具有良好的力学性能。     

Mo-8wt%Cu纳米复合粉末的制备和烧结

采用机械合金化法制备出Mo-8wt%Cu超细复合粉末,并对由该复合粉末所制得的压坯进行了液相烧结,利用SEM、XRD等分析手段对复合粉末的特性和烧结体的组织进行了表征和观察,实验结果表明,该方法制备的Mo-8wt%Cu超细复合粉末颗粒细小,平均粒径在300nm左右,高能球磨后的复合粉末由Mo-Cu过饱和固溶体相和Cu相组成,而且两相的晶粒度达到纳米级,其中Mo-Cu过饱和固溶体相的晶粒约为106nm,复合粉末具有很高的烧结特性,经高温烧结后合金致密度达到98.5%以上,而且金相组织分布均匀。     

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.     

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.     

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.