纳米晶Sm_2Co_(17)型块体永磁的制备及磁性能

制备了两种2∶17R型Sm-Co合金:Sm2(Fe,Cu,Zr,Co)17和纯二元Sm2Co17,并利用高能球磨和放电等离子烧结(SPS)制备了致密的纳米晶块体合金,研究了其磁性能和相结构的变化。Sm2(Fe,Cu,Zr,Co)17具有较高的矫顽力,而纯二元Sm2Co17矫顽力基本为零。但高能球磨可快速降低Sm2(Fe,Cu,Zr,Co)17合金的矫顽力。利用放电等离子烧结非晶粉末制备了纳米晶块体合金,纯二元Sm2Co17合金具有较高的矫顽力,并且具有1∶7H相结构。而Sm2(Fe,Cu,Zr,Co)17合金则因为Fe-Co相及Sm2O3相的析出,具有较高的饱和磁化强度和极低的矫顽力。     

球磨诱发α-Fe粉与间苯二胺混合物的固相反应

研究了球磨α－Fe粉末与间苯二胺混合时发生的固相反应以及铁氮化物的形成机理，在球磨过程中，随着球磨时间的延长α－Fe粉末与间苯二胺混合发生的相变为α－Fe→α′－Fe(N)→ε-F2-3N,球磨250h后，可得到含有11．53％N（质量分子）的过饱和ε－Fe2-3N相，它在512℃以下是稳定的，其饱和磁化强度为814.4emu/g，剩磁为33.8emu/g，矫顽力为16.3kA/m.与固－气反应相比，用固－固反应制备ε－Fe2-3N相的效率更高。     

HDDR处理的Sm2Fe16.5Ti0.5合金的结构与氮化

采用HDDR及氮化工艺制备了Sm2Fe16.5Ti0.5Ny粉末.铸态Sm2Fe16.5Ti0.5合金存在择优取向,Sm2(Fe,Ti)17主相的214衍射峰增强.均匀化退火后,只有约0.6%的α-Fe(Ti)相与主相Sm2(Fe,Ti)17共存.经不同循环的HDDR工艺处理后,物相组成不发生变化,但α-Fe(Ti)相含量增加.HDDR工艺有助于获得细晶结构,提高磁粉的矫顽力.HDDR处理的合金的氮化由初期的Sm-Fe-Ti合金与氮快速反应阶段及后期氮在合金中的均匀化扩散阶段组成.随着氮化时间的延长,富铁相含量增加.氮化物中Sm2(Fe,Ti)17Ny主相的晶格膨胀行为由HDDR与氮化工艺共同决定.在500℃氮化2h后,796kA/m最大外场下得到的最大矫顽力为164.9kA/m,氮化12h时后得到最大剩磁45.7Am2/kg.     

机械合金化制备NdFe10.5Mo1.5Nx间隙氮化物的结构和磁性能

本论文研究了高能球磨和随后的退火工艺制备的NdFe10.5Mo1.5Nx化合物的结构和磁性.通过高能球磨单质的Nd,Fe,Mo元素粉,能获得由非晶相和纳米级的α-Fe所组成的混合物.此最终球磨粉末通过750℃退火30分钟,能形成单相性良好的1:12相.在球磨前的原始粉末中,用纳米级的Fe粉代替微米级Fe粉,所制备的NdFe10.5Mo15Nx间隙氮化物表现出了较好的磁性能.     

B掺杂对SmFe_(10)Mo_2合金的结构及磁性的影响

用电弧熔炼法制备Sm Fe10Mo2及Sm Fe10Mo1.5B0.5母合金锭,将其均匀化退火后用球磨法制备Sm Fe10Mo1.5B0.5纳米晶合金粉末,研究了B掺杂对Sm Fe10Mo2块体合金和球磨对Sm Fe10Mo1.5B0.5纳米粉末的相结构和磁性的影响。结果表明,B掺杂后合金的Th Mn12相结构不变,居里温度由270℃提高到334℃;合金成分不均匀导致热磁曲线出现两个相变点。Sm Fe10Mo1.5B0.5合金经球磨处理0.5 h后Mo大量析出,1∶12相明显减少;随着球磨时间的增加α-Fe析出并形成非磁性的Mo2Fe B2相,使内禀矫顽力明显减小,且其饱和磁化强度随着球磨时间的增加呈现先增大后减小的趋势。球磨0.5 h的纳米合金粉末永磁磁性能最佳:Ms=55Am2/kg,iHc=0.2T。     

分散的Sm-Co永磁纳米颗粒的机械化学合成及磁性能

通过机械化学合成方法制备了矫顽力分别为2.95×106、2.83×106和8.60×105A/m的分散的单晶纳米Sm2Co7、SmCo5和Sm2Co17硬磁颗粒。研究了球磨时间、原料配比和退火工艺等对所制备的纳米永磁颗粒的微观组织、结构和磁性能的影响。结果表明,机械化学球磨时间至少是4h或更长时才能获得Sm-Co硬磁合金粉末。原料经过高能球磨后、未退火时,由于大部分颗粒为非晶结构,矫顽力较低,随着退火温度的上升,矫顽力增大,当退火温度为600℃时,达到最大值为2.83×106A/m,然后,随着退火温度的进一步升高,矫顽力减小。Sm-Co纳米颗粒的粒径随着退火温度的降低而明显减小。     

Sm3(Fe,Ti)29Nx/α-Fe双相纳米磁性材料的微结构与磁性能

研究了熔体快淬工艺及添加元素Ti对Sm-Fe合金相的形成及结构的影响,成功制备了Sm3(Fe,Ti)29Nx/α-Fe双相纳米耦合永磁材料.研究发现,快淬薄带由Sm3(Fe,Ti)29和α-Fe两相组成,晶化前在纳米晶周围存在部分非晶相,晶化后的晶粒间晶界平直光滑、且晶粒间结合紧密没有界面相,为晶粒间直接接触耦合.对甩带后的样品采用750℃保温10min的晶化退火得到的颗粒比较细小且均匀.氮化磁粉磁滞回线的第二象限没有出现明显的台阶,表现为单相永磁材料的特点,说明硬磁相Sm3(Fe,Ti)29Nx与软磁相α-Fe晶粒之间的交换耦合作用已形成.     

分散的Sm-Co永磁纳米颗粒的机械化学合成及磁性能

通过机械化学合成方法制备了矫顽力分别为2.95×106、2.83×106和8.60×105 A/m的分散的单晶纳米Sm2Co7、SmCo5和Sm2Co17硬磁颗粒。研究了球磨时间、原料配比和退火工艺等对所制备的纳米永磁颗粒的微观组织、结构和磁性能的影响。结果表明,机械化学球磨时间至少是4h或更长时间才能获得Sm-Co硬磁合金粉末。原料经过高能球磨后、未退火时,由于大部分颗粒为非晶结构,矫顽力较低,随着退火温度的上升,矫顽力增大,当退火温度为600℃时,达到最大值为2.83×106 A/m,然后,随着退火温度的进一步升高,矫顽力减小。Sm-Co纳米颗粒的粒径随着退火温度的降低而明显减小。     

Sm3（Fe，Ti）29Nx／α-Fe双相纳米磁性材料的微结构与磁性能

研究了熔体快淬工艺及添加元素Ti对Sm-Fe合金相的形成及结构的影响．成功制备了Sm3（Fe，Ti）29Nx／α-Fe双相纳米耦合永磁材料。研究发现．快淬薄带由Sm3（Fe，Ti）29和α-Fe两相组成，晶化前在纳米晶周围存在部分非晶相．晶化后的晶粒间晶界平直光滑、且晶粒间结合紧密没有界面相．为晶粒间直接接触耦合。对甩带后的样品采用750℃保温10min的晶化退火得到的颗粒比较细小且均匀。氮化磁粉磁滞回线的第二象限没有出现明显的台阶，表现为单相永磁材料的特点，说明硬磁相Sm3（Fe，Ti）29Nx与软磁相α-Fe晶粒之间的交换耦合作用已形成。     

PM法制备Sm2Fe17Nx永磁材料最佳工艺的研究

采用粉末冶金工艺制备了各向异性Sm2Fe17Nx永磁粉末.重点考查了工艺参数对Sm2Fe17合金的显微组织及Sm2Fe17Nx粉末磁特性的影响.结果表明,铸态合金的均匀化、粉末的氮化以及粉碎过程是获得高性能磁粉的关键因素.采用优化工艺条件制备的磁粉的磁特性为Jr=1.24T,iHc=756kA/m,(BH)max=220kJ/m3.     

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.     

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.     

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.     

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.     

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.     

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.     

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.