高温氧化对钛合金微弧氧化陶瓷膜组成与结构的影响

针对钛合金不耐高温氧化的问题,在铝酸钠电解液体系中,利用双相脉冲直流微弧氧化技术,在TC4钛合金表面原位生长以Al2TiO5为主晶相的复合氧化物陶瓷膜,研究了1000℃高温氧化对陶瓷膜试样的相组成、结构的影响及膜层增重特点.研究表明,陶瓷膜层试样的高温氧化过程包括Al2TiO5分解、基体氧化和膜层表面形貌变化3个方面.高温氧化后,膜层的主晶相由Al2TiO5变为α-Al2O3和金红石型TiO2,同时,膜层的表面形貌发生显著的变化;由于膜层和基体的热膨胀系数不同和基体钛的氧化,使得高温氧化后膜层在冷却过程中表面出现裂纹和脱壳.陶瓷膜层极大地减少了TC4钛合金在1000℃高温氧化时的增重,因此,陶瓷膜层可用于TC4钛合金的恒温氧化防护.     

多孔γ-Al2O3过渡膜的结构与性能研究

采用溶胶-凝胶技术,在多孔Al2O3载体上制备了一层适合于涂覆分离膜的γ-Al2O3多孔过渡膜.通过XRD与DTA-TG等测试手段研究了γ-Al2O3凝胶膜在热处理过程中的物理化学变化;通过TEM、SEM分析与泡点法研究了多孔膜的微观结构.实验结果表明:实验中制备的γ-Al2O3膜具有择优取向的特点;γ-Al2O3过渡膜的最可几孔径为0.38μm左右,厚度为4μm.薄膜的渗透性能测试结果表明,材料对H2与N2气的最大分离系数α=3.30.     

Al 2O 3/ Al 复合材料的界面结构特征

利用高分辩透射电子显微镜研究挤压铸造法制备的亚微米 Al 2O 3颗粒增强 Al 基复合材料的界面微观结构。结果表明 : Al基体的 (200) 和 (111) 面优先沿 Al 2O 3颗粒表面生长 , 在复合材料界面处 Al 基体与 Al 2O 3颗粒具有 Al (200) ∥Al 2O 3 (101 2) 、Al [011 ] ∥Al 2O 3 [0221 ] 的晶体学位向关系并形成半共格界面 , 且界面存在 Al (111) / / Al 2O 3 ( 1120) 的共格关系。界面干净无任何反应物。接近界面的 Al 基体中出现了柏氏矢量为 b= 1/ 3 [ 111 ] 弗兰克不全刃位错 , 该刃位错引起界面附近基体中明显的晶格应变场 , 位错周围晶格变形场的范围约为 20～30 层原子面宽度 , 而在 Al 2O 3颗粒靠近界面的区域中未观察到位错等缺陷。并从晶体学角度对界面的形成机制进行了分析。     

微弧氧化时间对铝合金陶瓷涂层结构和耐磨性的影响

铝合金微弧氧化陶瓷涂层结构致密,与基体结合牢固,具有良好的耐磨、耐蚀和电绝缘性能,应用前景广阔.采用微弧氧化工艺在6063铝合金表面沉积了Al2O3陶瓷涂层,考察了不同微弧氧化时间对涂层的微观结构、显微硬度、结合力及摩擦磨损性能的影响.结果表明:在电流密度一定的条件下,处理时间对涂层组织结构和性能有着较大的影响,随着微弧氧化时间的延长,涂层中α-Al2O3与γ-Al2O3相的衍射峰明显增强,制备的涂层表面更加致密,孔隙减少,同时所制备的涂层具有高的显微硬度(平均1180 HV)和好的抗耐磨性能,涂层与基体间的临界载荷约为85N,即涂层与基体间有强的结合力.     

DLC膜厚度对镁基表面DLC/MAO复合膜层性能的影响

采用线性离子束沉积技术于AZ80镁合金微弧氧化(MAO)陶瓷层表面沉积不同厚度的类金刚石碳(DLC)膜,形成DLC/MAO复合膜层。对比研究4种膜基系统的表面结构特征、力学性能以及摩擦学性能差异。结果表明:随DLC膜厚度增加,复合膜层表面微孔数量减少,孔径减小,但凹凸不平趋势增加,且DLC膜表面颗粒特征更加明显,表现为DLC-80min/MAO/AZ80膜基系统具有最小的表面粗糙度,最大的硬度H、弹性模量E及H/E值;不同厚度DLC/MAO/AZ80膜基系统平均摩擦因数较MAO/AZ80显著降低;DLC膜厚度增加导致3种复合膜基系统的表面微观结构改变,使得摩擦因数与磨痕形貌存在差异;各膜基系统表面磨痕处均形成了Fe的转移层,由于表层DLC膜"裸露"的大量C对磨损界面具有很好的润滑作用,而使得镁合金基体获得有效保护。     

离子束辅助沉积Al2O3薄膜的微观状态及其物理特性研究

本文利用透射电子显微镜、原子力显微镜、X光电子能谱等微观分析手段 ,系统研究了氧离子束辅助离子束沉积方法制备的Al2 O3 薄膜的化学成分、微观结构、表面形貌及其随退火温度的变化 ,并对Al2 O3 薄膜折射率、显微硬度和膜基结合强度等物理特性及其随沉积温度的变化进行了详细研究。研究发现 :用离子束辅助沉积制备的薄膜基本满足Al2 O3 的标准成分配比 ;在沉积温度低于 5 0 0℃制备的Al2 O3 薄膜以非晶Al2 O3 相a Al2 O3 为主 ;Al2 O3 薄膜的表面粗糙度、折射率、显微硬度随沉积温度的增加而增加 ;当沉积温度高于 2 0 0℃时 ,薄膜与基体间的膜基结合强度将随沉积温度的增加而下降。分析表明 :薄膜表面形貌与晶体内部的结构相变有关 ,薄膜的退火相变途径为a Al2 O380 0℃ γ Al2 O310 0 0℃ γ Al2 O3 +α Al2 O312 0 0℃ α Al2 O3 。     

多孔γ-Al2O3过渡膜的结构与性能研究

采用溶胶－凝胶技术，在多孔Al2O3载体上制备了一层适合于涂覆分离膜的γ-Al2O3多孔过渡膜。通过XRD与DTA－TG等测试手段研究了γ-Al2O3凝胶膜在热处理过程中的物理化学变化；通过TEM、SEM分析与泡点法研究了多孔膜的微观结构。实验结果表明：实验中制备的γ-Al2O3膜具有择优取向的特点；γ-Al2O3过渡膜的最可几孔径为0．38μm左右，厚度为4μm，薄膜的渗透性能测试结果表明，材料对H2与N2气的最大分离系数α＝3．30。     

电压对镁合金微弧氧化膜组织及耐蚀性的影响

由于镁合金耐蚀性差,其应用受到了限制.采用 SEM-EDS,XRD等表面分析技术研究了不同电压对MB5镁合金微弧氧化膜表面形貌、相结构与成分的影响,并用电化学测试方法考察了氧化膜层的耐腐蚀性能.结果表明:处理电压对微弧氧化膜层的微观组织结构、成分有显著影响,而微弧氧化膜层的微观组织结构与成分又直接影响其耐蚀性.在120～200 V下进行微弧氧化,160 V时试样耐蚀性最好.镁合金微弧氧化膜由α-MgF2,MgO,Mg2SiO4和MgAl2O4等含硅或铝的尖晶石型氧化物组成,随着氧化处理电压的增加,MgO的含量明显增加.微弧氧化时出现氧化膜微区熔化,溶液离子与基体合金都参与了微弧区物理化学反应.     

铍铝合金微弧氧化膜的微观结构、成分及性能

目前国内尚未开展铍铝合金的微弧氧化技术研究。采用微弧氧化技术在粉末冶金铍铝合金材料表面原位生长出一层氧化膜;采用扫描电子显微镜(SEM)、能谱仪(EDS)、X射线衍射仪(XRD)对氧化膜层的结构、形貌和成分组成进行表征分析。结果表明:氧化膜层平滑、致密,表面分布着Be、O、Al等元素。在微弧放电的高温下,氧化膜层的形成是各个反应过程的综合结果。所得氧化膜层的厚度均值为11.221μm,从氧化膜表层到基体方向,O、Si、P元素的含量有明显减少的趋势,而Al元素和Be元素含量的变化趋势则刚好相反。膜层有一定的结合强度、硬度和较小的表面粗糙度,并且能耐114 h的盐雾试验,击穿电压高于1 000 V。     

离子束辅助沉积A12O3薄膜的微观状态及其物理特性研究

本利用透射电子显微镜、原子力显微镜、X光电子能谱等微观分析手段，系统研究了氧离子束辅助离子束沉积方法制备的Al2O3薄膜的化学成分、微观结构、表面形貌及其随退火温度的变化，并对Al2O3薄膜折射率、显微硬度和膜基结合强度等物理特性及其随沉积温度的变化进行了详细研究。研究发现：用离子束辅助沉积制备的薄膜基本满足Al2O3的标准成分配比；在沉积温度低于500℃制备的Al2O3薄膜以非晶Al2O3相a—Al2O3为主；Al2O3薄膜的表面粗糙度、折射率、显微硬度随沉积温度的增加而增加；当沉积温度高于200℃时，薄膜与基体间的膜基结合强度将随沉积温度的增加而下降。分析表明：薄膜表面形貌与晶体内部的结构相变有关，薄膜的退火相变途径为a—Al2O3800℃→γ-Al2O31000℃→γ-Al2O3 α-Al2O31200℃→α-Al2O3。     

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.     

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.     

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.     

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.     

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.     

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.     

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.     

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。     

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。