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.     

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。     

Fe85Hf7B7Cu1非晶合金的非等温晶化动力学

利用非等温方法研究了Fe15Hf7B4Cu1非晶合金的晶化过程,晶化过程分两步进行,并利用修正的Kissinger方程计算了晶化动力学参数.第一个晶化过程是±-Fe的形成过程,其激活能为299±10kJ/tool,Avrami指数为1.3,是以预先形核的核心为基础的三维扩散控制生长方式为主;第二个晶化过程为残余非晶中Fe3B的形成过程,其激活能为423±12kJ/mol,Avrami指数为3.1,是以形核率逐渐减小的界面控制生长方式为主.     

Fe85Hf787Cu1非晶合金的非等温晶化动力学

利用非等温方法研究了Fe15Hf7B4Cu1非晶合金的晶化过程,晶化过程分两步进行,并利用修正的Kissinger方程计算了晶化动力学参数.第一个晶化过程是±-Fe的形成过程,其激活能为299±10kJ/tool,Avrami指数为1.3,是以预先形核的核心为基础的三维扩散控制生长方式为主;第二个晶化过程为残余非晶中Fe3B的形成过程,其激活能为423±12kJ/mol,Avrami指数为3.1,是以形核率逐渐减小的界面控制生长方式为主.     

低频脉冲磁场处理非晶Fe78Si9B13合金纳米晶化的DSC研究

用低频脉冲磁场处理非晶Fe78Si9B13合金,采用差示扫描热分析(DSC)的方法测定了不同升温速率下非晶Fe78Si9B13合金的DSC曲线,利用Kissinger方程计算出了晶化过程的激活能.结果表明,晶化激活能由处理前的433.6kJ/mol降到200kJ/mol以下,提高了晶核形核速率,抑制了晶核长大速率,从而实现了非晶合金的低温纳米晶化.     

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.     

α-Fe/Nd2Fe14B复合纳米晶的织构形成研究

采用X射线衍射分析(XRD)技术,研究了NdprFeCoB熔体快淬所制备的α-Fee/Nd2Fe14B纳米晶的织构形成过程.结果表明,Nd2Fe14B纳米晶具有较强的(001)织构,而α-Fe纳米晶具有(110)织构,这些织构垂直于薄带表面,且从自由面到激冷面逐渐减弱.从自由面到激冷面,Nd2Fe14B相在(001)晶面法线方向的尺寸和α-Fe相在(220)晶面法线方向的尺寸逐渐减小.在激冷面各晶面法线方向的尺寸相近,表明纳米晶的形状近似于等轴晶.α-Fe/Nd2Fei4B纳米晶织构的形成和生长受合金薄带在凝固过程中热流梯度的控制.     

Fe_(63)Ni_1Al_5Ga_2P_(9.65)B_(4.6)Si_3C_(6.75)Co_5非晶合金的晶化行为研究

采用XRD、DSC检测技术,采用连续升温晶化和等温退火晶化方法,研究分析了Fe63Ni1Al5-Ga2P9.65B4.6Si3C6.75Co5非晶薄带的晶化动力学行为和晶化过程中晶化相的析出过程。结果表明,该非晶合金的玻璃转变和晶化行为均具有显著的动力学特征。Kissinger法计算得到的Eg、Ex、Ep1、Ep2分别为750、340、432、689kJ/mol,Eg Ex,表明合金具有较好的热稳定性。合金晶化过程为:非晶→非晶+α-Fe→非晶+α-Fe+Fe2P+Fe3P→α-Fe+Fe2P+Fe3P+Fe3C(Al,Si)+Fe5PB2+SiC。合金的晶化类型为初晶型和随后的共晶型反应。     

FeCoNbSiBCu大块非晶合金的热稳定性与晶化过程研究

用差示扫描量热分析和原位高温X射线衍射研究了(Fe36Co36Nb4Si4.8B19.2)100-xCux(x=0, 0.5, 0.6, 0.7)大块非晶合金的热稳定性及其晶化过程.结果表明,微量Cu显著改变了Fe36Co36Nb4Si4.8B19.2大块非晶合金的晶化过程,无铜合金表现出单一尖锐晶化峰,而含铜量原子分数为0.5%,0.6%和0.7%的晶化过程分为四个阶段,Cu的加入提高了非晶合金纳米析出相的热稳定性.原位X射线衍射研究表明,FeCoNbSiBCu大块非晶合金初始晶化相为bcc-FeCo并于930K转变为bcc-Co7Fe3相.Cu添加后bcc-Co7Fe3的晶化表观激活能由460.41kJ/mol升高至545.69kJ/mol.用谢乐公式计算样品在840K保温17.5min的平均晶粒尺寸为22.3nm.     

α-Fe/Nd2Fe14B复合纳米晶合金的X射线定量相分析

采用联立方程组确立了α-Fe/Nd2Fe14B复合纳米晶合金中相含量的计算方法.该方法运用最小二乘回归法和抛弃平均法消除病态方程组.将其应用于α-Fe/Nd2Fe14B复合纳米晶合金的相含量计算,所得结果与直接对比法一致.     

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.     

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.     

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.     

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.     

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.     

MoO3-V2O5-P2O5-Fe2O3玻璃的制备及性能研究

制备了MoO3-V2O5-P2O5-Fe2O3系磷酸盐玻璃,研究了玻璃形成能力、热膨胀系数和抗潮解等性能.结果表明,MoO3-V2O5-P2O5-Fe2O3系统具有较宽的玻璃形成区和较强的玻璃形成能力,当MoO3/V2O5≈1.5时,玻璃形成能力最强.MoO3-V2O5-P2O5-Fe2O3玻璃的热膨胀系数约为60～110×10-7/℃,并且随着Fe2O3含量的增加而逐渐增大.加入适量的Fe2O3能够显著改善MoO3-V2O5-P2O5玻璃的抗潮解性能,在90℃的去离子水中的溶解速率达到8.0×10-9g·cm-2·min-1.     

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.     

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.     

MgO-Al2O3-SiO2-TiO2-Y2O3玻璃的弹性模量

根据硬盘基板用材料的要求，制备了MgO-Al2O3-SiO2-TiO2-Y2O3高弹性模量玻璃（120GPa)，玻璃的弹性模量随组成的变化服从Makishima-Mackenzie理论，MgO,Al2O3,TiO2,Y2O3等具有较高单位体积离解能的氧化物有利于提高玻璃的弹性模量，但玻璃弹性模量的理论计算值低于测试值，这是因为Makishima-Mackenzie理论没有考虑玻璃内阳离子的具体配位，对MgO,Y2O3堆积密度因子的堆导存在误差，因此利用Makishima-Mackenzie理论发展高弹性模量玻璃时应对MgO,Y2O3等氧化物的计算进行修正。