Ba0.5Sr0.5TiO3铁电薄膜的微弧氧化制备工艺

用分析纯Ba(OH)2·8H2O和Sr(OH)2·8H2O配制电解液(浓度各为0.2 mol/L),采用微弧氧化技术在工业纯钛板(99.5％)表面原位生成BaxSr(1-x)TiO3铁电薄膜.对不同电流密度、电流频率和反应时间条件下获得的薄膜进行表征,研究了各因素对薄膜物相构成、表面形貌和表面粗糙度的影响.结果表明:所得薄膜均主要由四方相Ba0.5Sr0.5TiO3构成;电流密度为20 A/dm2、电流频率为100 Hz、反应时间为10 min时,所得薄膜最平整、致密、表面粗糙度值最小,且微弧氧化孔洞分布最均匀,测得该薄膜在1 kHz条件下的介电常数为411.3.     

薄膜厚度对Y掺杂Ba0.6Sr0.4TiO3薄膜结构及介电性能的影响

采用溶胶-凝胶法(Sol-gel)在Si/SiO2/Ti/Pt基片上制备了不同厚度(正比于薄膜层数)的钇(Y)掺杂Ba0.6Sr0.4TiO3(BST)薄膜,研究了膜厚度对薄膜结构和介电性能的影响。原子力显微镜(AFM)表明,Y掺杂BST薄膜可显著改善表面形貌,且强烈依赖于薄膜厚度。当薄膜厚度适中(即当层数为8)时,表面晶粒细小、致密、均匀,晶界分明。X射线衍射(XRD)表明,Y掺杂BST薄膜显示钙钛矿结构,主要沿(110)晶面生长。随着薄膜厚度的增加,BST(110)峰的衍射强度先增后减,表明薄膜的相结构与薄膜厚度直接相关。Y掺杂BST薄膜显示优异的综合介电性能,且随着膜厚的增加,电容或介电常数减小。8层薄膜的综合介电性能最优,零偏压时的电容为17.8pF(介电常数130)、介电损耗为0.0057,调谐率为32%,优值因子为56,可满足微波调谐器件的需要。同时,就有关机理进行了分析。     

Y掺杂(Ba0.6Sr0.4)0.8TiO3薄膜的结构及介电性能

通过钇(Y)掺杂、适当增加钛(Ti)含量和调节薄膜厚度等优化设计,用改善的溶胶-凝胶(Sol-Gel)法制备了光滑致密的Y掺杂多层钛酸锶钡(Ba0.6Sr0.4)0.8TiO3,BST)薄膜,研究了该薄膜的结构及介电性能。X射线衍射(XRD)表明,该薄膜为钙钛矿结构,但其衍射峰强度很弱,主要与Y掺杂和微过量Ti有效减弱其铁电性有关。原子力显微镜(AFM)表明,该薄膜晶化较弱,且随厚度的增加晶化减弱,和XRD结果一致。该薄膜比Y掺杂的Ba0.6Sr0.4TiO3薄膜显示更优异的综合介电性能,但与薄膜的厚度有关。随膜厚的增加,薄膜的电容和调谐率减小,但介电损耗大幅减小,其中,4层薄膜零偏压的介电常数为161、电损耗约为0.006,40V的调谐率为45.5%、优质因子大于75,可满足微波调谐器件的需要。     

微弧氧化SrTiO_3铁电薄膜的微观结构及性能

以0.2 mol/L Sr(OH)2+0.2 mol/L NaOH溶液为电解液,工艺参数分别设置为电流密度2 A/cm2、电流频率100 Hz、反应时间30 min及占空比85%,采用微弧氧化法在工业纯Ti板(99.5%)表面原位生长SrTiO3薄膜,并对薄膜的物相组成,元素分布情况及薄膜介电、铁电性能进行表征。结果表明:所得薄膜主要由四方相SrTiO3构成。薄膜介电常数随频率升高而降低,其在1 kHz条件下的介电常数为317。薄膜中除Sr、Ti、O元素外,还存在Na元素,且Na元素在薄膜与基体结合处出现富集,元素分布的微小波动可能是由微弧氧化孔洞造成。     

微弧氧化沉积BaTiO3介电薄膜的截面结构研究

采用微弧氧化技术在工业纯Ti板表面沉积了BaTiO3薄膜,利用XRD、SEM、EPMA表征了薄膜表面及截面的物相组成、截面结构以及截面元素分布情况,并利用电容探测仪检测了薄膜的介电性能。结果表明:薄膜表面和截面均主要由四方相BaTiO3组成;薄膜截面可分为过渡层、致密层和疏松层,但各层元素含量不同;微孔的存在导致Ba、Ti、O三种元素在截面区域内的分布出现突变;测得薄膜在100 Hz下的介电常数和介质损耗分别为227.3和0.043。     

微弧氧化工艺参数对BaTiO3和SrTiO3薄膜生长的影响

将工业纯Ti板(99.5%)分别置于Ba(OH)2、Sr(OH)2+NaOH溶液中微弧氧化制备BaTiO3和SrTiO3陶瓷薄膜。XRD分析表明:所制备的薄膜分别主要由四方相BaTiO3和立方相SrTiO3组成。测得最优工艺条件下所得两种薄膜在100 Hz下的介电常数分别为152.3和419.1,介质损耗(tanδ)值分别为0.096和0.045。重点研究了微弧氧化工艺参数对薄膜生长的影响规律,结果表明:随着电解液溶度、电流密度的增加以及电流频率的降低,薄膜的生长速度加快;提出并验证了薄膜生长动力学的经验公式。     

微弧氧化制备BaTiO3介电薄膜的电解液体系优化

用正交试验法对BaTiO₃薄膜微弧氧化电解液体系进行优化,并对最优电解液体系下所得薄膜的物相组成,元素分布情况、表面形貌及介电性能进行了表征。结果表明,最优电解液体系为0.5 mol/L Ba(OH)₂ +0.1 g纳米TiO₂+0.05 g乙二醇+0.2 g甘油;最优电解液体系下所得薄膜主要由四方相BaTiO₃和极少量BaCO₃组成,且薄膜表面平整、孔洞分布均匀、孔径细小,其在100 Hz下的介电常数为245.3。     

钇梯度掺杂Ba0.6Sr0.4TiO3薄膜的sol-gel法制备及介电性能

用改进的溶胶-凝胶法(sol-gel)在Pt/Ti/SiO2/Si(S)上制备了各层Y掺杂浓度分别为0.5%/0.6%/0.7%/0.8%/0.9%/1%的上梯度掺杂和1%/0.9%/0.8%/0.7%/0.6%/0.5%下梯度掺杂的Ba0.6Sr0.4TiO3薄膜。X射线衍射(XRD)表明,各薄膜主要沿(110)晶面生长,均为立方钙钛矿结构。相比均匀掺杂薄膜,梯度掺杂薄膜表现出较好的相结构衍射强度及晶化,上梯度薄膜更为显著。原子力显微镜(AFM)表明,梯度掺杂使薄膜的表面形貌得到极大改善,上梯度比下梯度薄膜具有更加光滑致密的表面相貌和更小的表面粗糙度。电压-电容曲线表明,上梯度薄膜介电性能得到明显提高,在零偏压下的电容为28.5pF(介电常数190)、介电损耗为1.63%及40V下的调谐率为52.3%,优质因子为32。     

掺杂对Na0.5Bi0.5TiO3基无铅压电陶瓷弛豫性的影响

对(Na0.5Bi0.5)TiO3-BaTiO3(NBBT)二元系压电陶瓷在准同型相界附近进行不同量的La,Mn掺杂,通过XRD、电学性能测试等,研究了掺杂对陶瓷微观结构及介电性能的影响.结果表明,La,Mn掺杂后,相变的弥散程度增大,体系的弛豫性增强.铁电体的弛豫性与基体内极性微区的有序度及尺寸、数量密切相关,对NBBT这种A位复合体系而言,La离子的介入在一定程度上引起电荷不平衡,促使微区长大;但是由于La的分隔作用,A位与B位的耦合作用大大减弱,体系整体有序度降低,弛豫性增强.Mn离子的B位掺杂有助于建立新的(AA')(BB')O3复合体系,因此也影响体系的弛豫性.     

改进水热法制备Ba0．5Sr0．5TiO3薄膜及其表征

采用改进水热法(金属Ti片与等浓度的Ba2 ,Sr2 强碱性溶液于250℃水热反应5 h,然后经过600℃,0.5 h烧结处理)制备了单一立方相的Ba0.5Sr0.5TiO3薄膜.制备的Ba0.5Sr0.5TiO3薄膜通过XRD,SEM和XPS进行表征分析.结果表明:600℃下经过0.5 h烧结处理的Ba0.5Sr0.5TiO3薄膜结晶更完整;同时,制备的Ba0.5Sr0.5TiO3薄膜表面吸附有OH,经过10 min刻蚀处理后,吸附的OH能谱峰消失.     

FIRST–PRINCIPLE ANALYSYS ON FINE STRUCTURE OF Pb0.5Sr0.5TiO3

在广义梯度近似下, 采用基于密度泛函理论框架下的第一性原理和虚拟晶体近似 (VCA) 方法, 计算了Pb_0.5Sr_0.5TiO₃ (PST)电子结构及其属性. 分析了PST固溶体总体能量变化趋势, 确定了A位离子在铁电相的平衡构型. 计算结果表明: 在PST固溶体中, 当Ti原子相对于氧八面体沿[001]方向发生约0.012 nm偏心位移, PST出现能量极小值.O 2p和Ti 3d轨道的强杂化以及部分O---Pb和O---Sr轨道杂化间接增强了TiO₆八面体的畸变, 体系总能量降低, 促进了PST铁电畴变的形成.     

Dielectric properties of low-temperature sintered Ba0.6Sr0.4TiO3 thick films prepared by reactive sintering method

Screen printed Ba_0.6Sr_0.4TiO₃ (BST6/4) thick films were fabricated by reactive sintering at a low temperature below 900 °C. The dielectric properties in radio frequency range were measured on samples of sandwich structure MIM capacitors by impedance analyzer, while that in microwave frequency range were measured on samples of thick films without top and bottom electrodes by split-post dielectric resonator method. The thick films exhibited a low permittivity, while at the same time, maintained a high tunability. The permittivity and dielectric loss at 1 MHz were 228.8 and 0.007, respectively. The corresponding values measured at 9.9 GHz were 82.24 and 0.109, respectively. The tunability was as high as 72.4% (150 kV/cm, 10 kHz). This method provides a simple and effective route to obtain thick films with great potential in applications in Low Temperature Co-fired Ceramic (LTCC) and microwave tunable devices.     

Sinterability and dielectric properties of Ba0.55Sr0.4Ca0.05TiO3-CaTiSiO5-Mg2TiO4 composite ceramics

The composite ceramics of Ba_0.55Sr_0.4Ca_0.05TiO₃-CaTiSiO₅-Mg₂TiO₄ (BSCT-CTS-MT) were prepared by the conventional solid-state route. The sintering performance, phase structures, morphologies, and dielectric properties of the composite ceramics were investigated. The BSCT-CTS-MT ceramics were sintered at 1100 °C and possessed dense microstructure. The dielectric constant was tailored from 1196 to 141 as the amount of Mg₂TiO₄ increased from 0 to 50 wt%. The dielectric constant and dielectric loss of 40 wt% Ba_0.55Sr_0.4Ca_0.05TiO₃-10 wt% CaTiSiO₅-50 wt% Mg₂TiO₄ was 141 and 0.0020, respectively, and the tunability was 8.64% under a DC electric field of 8.0 kV/cm. The Curie peaks were broadened and depressed after the addition of CaTiSiO₅. The optimistic dielectric properties made it a promising candidate for the application of tunable capacitors and phase shifters.     

Characterization of sol-gel synthesised lead-free (1 − x)Na0.5Bi0.5TiO3-xBaTiO3-based ceramics

The crystal structure, microstructure, dielectric and ferroelectric properties of (1 − x)Na_0.5Bi_0.5TiO₃-xBaTiO₃ ceramics with x = 0, 0.03, 0.05, 0.07 and 0.1 are investigated. A structural variation according to the system composition was investigated by X-ray diffraction (XRD) analyses. The results revealed that the synthesis temperature for pure perovskite phase powder prepared by the present sol-gel process is much lower (800 °C), and a rhombohedral-tetragonal morphotropic phase boundary (MPB) is found for x = 0.07 composition which showing the highest remanent polarization value and the smallest coercive field. The optimum dielectric and piezoelectric properties were found with the 0.93Na_0.5Bi_0.5TiO₃-0.07BaTiO₃ composition. The piezoelectric constant d₃₃ is 120 pC/N and good polarization behaviour was observed with remanent polarization (P_r) of 12.18 pC/cm², coercive field (E_c) of 2.11 kV/mm, and enhanced dielectric properties ?_r > 1500 at room temperature. The 0.93Na_0.5Bi_0.5TiO₃-0.07BaTiO₃-based ceramic is a promising lead-free piezoelectric candidate for applications in different devices.     

Improving leakage currents of Pt/Ba0.8Sr0.2TiO3/Pt capacitors using multilayered structures

Pt/Ba_0.8Sr_0.2TiO₃ (BST)/Pt capacitors fabricated by the sol–gel process generally show abnormally high leakage currents. In this paper, we report the reduction of this leakage current in multilayered sol–gel Pt/BST/Pt thin film capacitors. The multilayered structure also provided the flexibility of adjusting the dielectric constant of the film. The thin films were fabricated by a step-by-step annealing scheme at 750 °C except that the top and bottom layers were annealed at less than 750 °C. The observed results are explained by an amorphous/polycrystalline structure, which was confirmed by scanning electron microscopy and X-ray diffraction analysis.     

Piezoelectric and dielectric properties of Dy2O3-doped (Bi0.5Na0.5)0.94Ba0.06TiO3 lead-free ceramics

(Bi_0.5Na_0.5)_0.94Ba_0.06TiO₃ + x wt% Dy₂O₃ with x = 0-0.3 ceramics were synthesized by conventional solid-state processes. The effects of Dy₂O₃ on the microstructure, the piezoelectric and dielectric properties were investigated. X-ray diffraction pattern confirmed that the coexistence of tetragonal and rhombohedral phases in the (Bi_0.5Na_0.5)_0.94Ba_0.06TiO₃ composition was not changed by adding 0.05-0.3 wt% Dy₂O₃. SEM images indicate that all the ceramics have pore-free microstructures with high density, and that doping of Dy₂O₃ inhibits the grain growth of the ceramics. The addition of Dy₂O₃ shows the double effects on decreasing the piezoelectric and dielectric properties for 0 < x < 0.15 when Dy³⁺ ions substitute B-site Ti⁴⁺ ions, and increasing the properties for 0.15 < x < 0.3 when Dy³⁺ ions enters into A-site of the perovskite structure. The optimum electric properties of piezoelectric constant d₃₃ = 170 pC/N and the dielectric constant ?_r = 1900 (at a frequency of 1 kHz) are obtained at x = 0.3.     

纳米Si3N4 对TC4钛合金微弧氧化层微观结构和性能的影响

在基电解液中加入氮化硅纳米颗粒,对TC4钛合金进行微弧氧化（MAO）处理,研究了Si₃N₄浓度对微弧氧化层表面形貌、耐蚀性和耐磨性的影响。添加Si₃N₄的MAO层呈现多孔结构,当Si₃N₄浓度为1 g/L时,涂层厚度最大,且经过7 d的酸腐蚀试验,该涂层的耐蚀性良好,腐蚀速率最低,约为0.057 mg·cm^-2·d^-1。随着Si₃N₄的加入,MAO涂层的抗菌性能先升高后降低。当Si₃N₄的添加量为1 g/L时,该MAO层的抗菌性能最好。Si₃N₄的加入能明显提高涂层在模拟海水中的耐磨性。当Si₃N₄的添加量为3和4 g/L时,所得涂层的摩擦系数低且稳定,且添加3 g/L Si₃N₄制备来的MAO涂层表现出优异的耐磨性。     

(Pb_(0.5)Sr_(0.5))TiO_3粉体与薄膜的合成、结构与电性能研究(英文)

使用溶胶凝胶法合成(Pb0.50Sr0.50)TiO3(缩写为PST)粉体和薄膜。用X射线衍射(XRD)和扫面电镜(SEM)观察PST粉体的相形成和形貌特征。结果表明,800℃退火处理的凝胶样品还有中间相碳酸盐存在;850℃退火的干凝胶样品,晶化完成后为多晶钙钛矿结构,而650℃经快速热处理的薄膜样品为多晶结构,平均晶粒尺寸为60nm。PST薄膜在100kHz频率测量情况下,介电常数与损耗分别为561.5和0.022。     

Synthesis and characterization of Al2O3-Ce0.5Zr0.5O2 powders prepared by chemical coprecipitation method

Al₂O₃-Ce_0.5Zr_0.5O₂ catalytic powders were synthesized by the coprecipitation (ACZ-C) and mechanical mixing (ACZ-M) methods, respectively. As-synthesized powders were characterized by XRD, Raman spectroscopy, surface area and thermogravimetric analyses. It was found that the mixing extent of Al³⁺ ions affected the phase development, texture and oxygen storage capacity (OSC) of the Ce_0.5Zr_0.5O₂ powder. Single phase of ACZ-C could be maintained without phase separation and inhibit α-Al₂O₃ formation up to 1200 °C. The specific surface area value of ACZ-C (81.5 m²/g) was larger than that of ACZ-M (62.1 m²/g) and Ce_0.5Zr_0.5O₂ (17.1 m²/g) powders, which were calcined at 1000 °C. In comparison with ACZ-C and Al₂O₃, which were calcined at high temperature (900–1200 °C), it was found that the degradation rate of specific surface area of ACZ-C was lower than that of Al₂O₃. ACZ-C sample showed a higher thermal stability to resist phase separation and crystallite growth, which enhanced the oxygen storage capacity property for Ce_0.5Zr_0.5O₂ powders.