基于LaNiO_3和Pt电极的Pb(Zr_(0.52)Ti_(0.48))O_3薄膜制备和电学性能研究

采用了溶胶-凝胶(sol-gel)法分别在LaNiO3/Si和Pt/Ti/SiO2/Si基底上制备Pb(Zr0.52Ti0.48)O3(PZT)薄膜。X射线衍射(XRD)结果表明,在相同的工艺参数下PZT/LaNiO3薄膜表现出高度的(100)取向,而PZT/Pt薄膜则呈现(100)和(111)多晶混合取向。扫描电子显微镜(SEM)结果显示,PZT/LaNiO3薄膜表面晶粒尺寸更加均匀。经过铁电和介电性能测试,PZT/LaNiO3和PZT/Pt薄膜的剩余极化强度分别为24.4和15.3μC/cm2,矫顽场分别为130.90和243.23 kV/cm,介电常数分别为1 125和453。电场强度100 kV/cm时,漏电流分别为10-5和10-2数量级,同时铁电疲劳性能也明显改善。这些结果表明PZT/LaNiO3比PZT/Pt薄膜具有更好的电学性能,在铁电和介电器件方面具有良好的应用前景。     

Sol-gel法制备Pb(Zr0.53Ti0.47)O3铁电薄膜

利用Sol-gel工艺在Pt/Ti/SiO2/Si衬底上制备了Pb(Zr0.53Ti0.47)O3(PZT)薄膜,研究了退火温度、保温时间和薄膜厚度对其晶相、微观结构和铁电性能的影响.在500℃退火处理的PZT薄膜开始形成钙钛矿相;在550℃退火处理的PZT薄膜基本形成钙钛矿相结构;升高退火温度(500～850℃)、延长保温时间(30～150min)、增加薄膜厚度(120～630nm)都有利于PZT晶粒的长大.在650～750℃退火的PZT薄膜具有较好的铁电性能,保温时间对PZT薄膜的铁电性能影响不大,PZT薄膜的厚度为200～300nm时可以得到比较好的铁电性能.在退火温度750℃、保温时间30min条件下退火处理厚310nm的PZT薄膜,其剩余极化值(2Pr)和矫顽电场(2Ec)分别是72μC/cm2、158kV/cm.     

低温制备Pb(Zr0.52Ti0.48)O3铁电薄膜及其性能研究

采用脉冲激光沉积技术（PLD）在（100）p-Si衬底上,低温淀积、快速退火成功地制备了具有完全钙钛矿结构的多晶PZT铁电薄膜,所制备的PZT铁电薄膜致密、均匀,表现出良好的介电和铁电性能,其介电常数和介电损耗100kHz下分别为320和0.08,剩余极化Pr和矫顽场Ec分别为14μC/cm^2和58kV/cm,＋5V电压下漏电流密度低于10^-7A/cm^2。10^7次极化反转后剩余极化仅下降10％,具有较好的疲劳特性。     

Preparation of Lanthanum-Doped Pb(Zr,Ti)O3 Ceramics Sheets by Tape Casting

The physical and electrical properties of lanthanum doped Pb（Zr,Ti）O3 ceramic sheets （PLZT） which were prepared by tape casting method were carried out. Tape casting of lanthanum modified PZT was performed using commercial cellulose acetate binders and poly（ethylene glycol） plasticizers in ethanol solvent. Tapes from these slips were casted on a polymer substrate. The PLZT green tapes were stacked for 5 units and sintered in air at 1050℃ for 1 h with heating rate 5℃/min. SEM micrographs show that the tape is dense （90.26% of theoretical density） and rather uniform with grain size of approximately 1.1 9 m. The dielectric permittivity and loss tangent of PLZT ceramics as a function of temperature at 1 kHz suggest that the compounds exhibit a phase transition of diffuse type. The transition temperature （Tm ） and piezoelectric coefficient （ d33 ） were 110℃ and 117 pC/N, respectively.     

溶胶－凝胶法制备Pb（Zr，Ti）O_3玻璃陶瓷过程中的结构变化

本文介绍溶胶－凝胶法制备均匀ＰｂＺｒ－Ｔｉ－Ｂ－Ｓｉ凝胶玻璃，并通过适当热处理在凝胶玻璃中原位生长Ｐｂ（Ｚｒ；Ｔｉ）Ｏ３微晶的新工艺·利用ＩＲ谱考察了凝胶玻璃中的元素键合结构随温度的变化．结合热分析和ＸＲＤ；ＳＥＭ技术，研究了Ｐｂ（Ｚｒ，Ｔｉ）Ｏ３微晶在凝胶玻璃中的生长过程及该材料的结构特点．发现Ｐｂ２（Ｚｒ，Ｔｉ）２Ｏ６＋ｘ立方焦绿石介稳过渡相的纳米微晶首先出现于该体系中，并在更高的温度下先后完全转变成三方和四方Ｐｂ（Ｚｒ，Ｔｉ）Ｏ３钙钛矿相．电子显微观察结果表明，该工艺制备的Ｐｈ（Ｚｒ；Ｔｉ）Ｏ３玻璃陶瓷具有均匀的细晶结构．     

溶胶凝胶法以无机锆源制备Ba(Zr,Ti)O3的成胶机理分析

为制备高性能低成本压电陶瓷材料,以无机锆为锆源,低价的乙酸与乙二醇为溶剂,采用Sol-Gel法制备Ba(Zr,Ti)O3溶胶和纳米粉体.XRD和TEM分析显示,所制备的粉体为纯钙钛矿相,近球形,粒径在40nm左右.通过IR、GC-MS分析了锆钛酸钡溶胶的形成机理,结果表明:在锆钛酸钡的溶胶过程中乙二醇、乙酸与乙酸钡、钛酸四丁酯、柠檬酸锆发生化学反应,生成以金属氧键为中心,乙二醇与冰乙酸为中间络合支架的链状聚合体,提高了溶胶凝胶的质量和稳定性.     

Pb(Zrx Ti1-x)O3成分梯度铁电薄膜的结构及性能

采用Sol-Gel方法,通过快速热处理,在Pt/Ti/SiO2/Si衬底上制备出Pb(Zr,Ti)O3成分梯度薄膜.用俄歇微探针能谱仪(AES)对制备的上梯度薄膜进行了成分深度分析,证实其成分梯度的存在.XRD分析表明,制备的梯度薄膜为四方结构和三方结构的复合结构,但其晶面存在一定的结构畸变.介电温谱测试表明,随着温度的升高,梯度薄膜出现一个铁电-铁电相变点和两个居里点,同时出现一定的频率弥散现象.不同偏压下电滞回线的测试表明,梯度薄膜表现出良好的铁电性质.热释电性能测试表明,梯度薄膜的热释电系数随着温度的升高逐渐增加,并且其热释电系数比每个单元的热释电系数大.     

以Al2O3为过渡层脉冲激光法制备PZT铁电薄膜

为实现PZT铁电薄膜与半导体衬底的直接集成引入Al2O3为过渡层，首先用真空电子束蒸发法在Si(100)，多昌金刚石（111）衬底上生长约20nm厚的Al2O3过渡层，接着在上述衬底上采用脉冲激光淀积（PLD）法淀积PZT薄膜，衬底温度为350-550℃。X光电子能谱（XPS）测试表明，在高真空下，电子束蒸发Al2O3固态源能获得化学配比接近蒸发源的Al2O3薄膜。X射线衍射（XRD）测试说明，不论衬底是硅还是多晶金刚石，当衬底温度为550℃时，PZT在Al2O3过渡层上呈现（222）取向的焦绿石相结构，当衬底是金刚石时，通过如下工艺：（1）较低温度（350℃）淀积；（2）空气氛围650℃快速退火5min，可以在Al2O3过渡层上获得高度（101）取向的钙钛矿结构的铁电相PZT薄膜，最后AFM测试显示，在硅衬底上，PZT薄膜的表面均方根粗糙度为9.78nm；而在多晶金刚石衬底上，PZT薄膜的表面均方根粗糙度为17.2nm。     

退火工艺对溶胶凝胶Pb(Zr0.52Ti0.48)O3薄膜残余应力的影响

使用溶胶凝胶法制备了Pb(Zr0.52Ti0.48)O3 铁电薄膜,分别利用原子力显微镜、X射线衍射及面探扫描技术分析了薄膜的组织结构,并运用掠入射X射线衍射法研究了不同工艺条件下制备的薄膜的残余应力.研究表明溶胶凝胶薄膜在600℃退火30min后完全晶化,组织结构均匀.不同工艺下制备的薄膜均受残余拉应力,随着退火温度及退火时间的延长,薄膜中的残余应力逐渐增大,而随着薄膜厚度的增加,残余应力先增大然后减小.     

锌铌酸铅-锆钛酸铅(PZN-PZT)压电陶瓷和陶瓷纤维的制备

以乙酸铅、丙酸锌、五乙氧基铌、四丙氧基锆和四正丁氧基钛为原料,用溶胶-凝胶法制备了锌铌酸铅-锆钛酸铅(PZN-PZT)凝胶纤维.该纤维经热解、烧结后成为直径约25μm的陶瓷纤维.陶瓷纤维的表面和断面形貌的电子扫描图像显示:该陶瓷纤维均匀致密,呈圆柱形.X射线分析表明:烧结温度影响陶瓷的晶相纯度.当烧结温度高于1250℃时,该陶瓷及陶瓷纤维呈现纯净的钙钛矿晶相.阿基米德法测得陶瓷和陶瓷纤维的密度分别为7.70×10³kg/m³和7.80×10³kg/m³.对陶瓷含量为63%的PZN-PZT陶瓷纤维/环氧树脂1-3复合材料压电片,测得其机电转换常数kt、压电常数d₃₃和相对介电常数ε分别为:0.65、403pC/N和1300.以溶胶-凝胶法制备的超细粉体为原料烧结成的PZN-PZT陶瓷,其k_t、d₃₃和ε分别为0.48、600pC/N和2627.     

Characterization of sol-gel Pb(Zr0.53Ti0.47O3) in thin film bulk acoustic resonators

The behavior of {f111g}-textured Pb(Zr(0.53Ti0.47O3) (PZT) deposited by the sol-gel technique in thin film bulk acoustic resonators (TFBAR's) was investigated at a resonance frequency of about 1 GHz. The resonators were fabricated on Si wafers using deep silicon etching to create a membrane structure and using platinum as top and bottom electrodes. The best response of the resonators was observed at a bias voltage of -15 kV/cm with values of about 10% for the coupling constant and about 50 for the quality factor. This voltage corresponds to optimal values of piezoelectric constant d33 and dielectric constant measured as a function of the electric field. The influence of a bias voltage on the resonance frequency, antiresonance frequency, and coupling constant were observed. Both the resonance and antiresonance frequency show a hysteretic change with applied bias. This effect can be used to shift the whole band of a filter by applying a voltage. The TFBAR structure also allowed us to extract values for materials parameters of the PZT film. Dielectric, piezoelectric, and elastic properties of the f111g-textured PZT film are reported and compared to direct measurements and to literature values.     

The effect of LaNiO3 buffer layer thickness on the electric properties of Pb(Zr0.53Ti0.47)O3 thin films deposited on titanium foils

Sol-gel derived Pb(Zr_0.53Ti_0.47)O₃ (PZT) thin films were prepared on LaNiO₃ (LNO) buffered titanium foils. The effect of LNO buffer layer thickness on the electric properties of PZT thin films was investigated. The room temperature dielectric constant of PZT thin films increased with increasing LNO thickness. The remnant polarization of PZT thin films on 150 and 250 nm LNO was about 20 uC/cm². Curie temperatures of PZT thin films were 310, 330 and 340 °C for LNO of 250, 150 and 50 nm respectively. The current-voltage characteristics of PZT thin films were examined for different LNO buffer layer thicknesses, and the space charge limited conduction model was followed in PZT thin films on 50 nm LNO.     

Ferroelectric properties of Pb(Zr,Ti)O3 films fabricated using a modified sol-gel based process

Ferroelectric PZT(20/80) thick films were fabricated by the screen printing method. And the PZT precursor solution was spin-coated on the PZT thick films to obtain a densification. Electrical properties of the thick films as a function of the firing temperature of the PZT precursor solution were investigated. The thickness of all thick films was approximately 60-62 μm. The porosity increased with increasing the firing temperature of the sol, and the porous microstructure and some large pores were observed above 700 °C due to the PbO evaporation. The relative dielectric constant, remanent polarization and dielectric breakdown strength of the specimen fired at 650 °C were 222, 16.5 μC/cm² and 73 kV/cm, respectively.     

磁控溅射工艺参数对Pb(Zr,Ti)O3薄膜织构的影响

利用RF磁控溅射法制备了Pb(Zr,Ti)O3(PZT)铁电薄膜,利用X射线衍射(XRD)法研究了薄膜的相组成及溅射工艺参数对薄膜织构的影响.结果表明,在小靶基距时,过高溅射功率不利于获得纯钙钛矿相的PZT铁电薄膜.溅射功率及溅射气压影响PZT薄膜的织构及其织构散漫度,提高溅射气压及溅射功率,(111)织构漫散度随之提高.在靶基距为80mm时,选择150w、0.7Pa的溅射工艺可获得具有最佳(100)织构的PZT薄膜.     

TiOx interlayer characterization for sol–gel derived Pb(Zr, Ti)O3 thin films on titanium foil

Pb(Zr, Ti)O₃ films were prepared on titanium foil using sol–gel processing. The films were of large area, crack-free, uniform, with perovskite structure and exhibiting strong adhesion to the titanium foil substrate. Films and the interface region between the film and the substrate were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy, and dielectric property measurements. The measurements revealed the formation of a TiO_x layer at the interface between the film and the foil. The thickness of the TiO_x interlayer increases with increasing annealing temperature, and was amorphous when annealed below 600 °C. The dielectric properties of films depend on the thickness of the TiO_x interlayer. Films on Ti foil with dielectric constant of 200–400, dielectric loss <5%, leakage current of <1×10^–7 A cm^–2 at 100 kV cm^–1 and breakdown field strength of 0.6–1.13 MV cm^–1 were demonstrated. The TiO_x interlayer resulted in asymmetric C–V hysterisis behavior attributed to trapped charge in the vicinity of the TiO_x interlayer and to elastic mismatch strain.     

Pb(Zr0.52Ti0.48)O3 nanotubes synthesis and infrared absorption properties

Herein a useful methodology to synthesize the lead zirconate titanate (PZT) nanotubes via a dip-coating deposition process with anodic aluminum oxide (AAO) template is proposed. The nano-porous AAO templates were produced using a controlled two-step electrochemical anodization technique. The PZT/AAO composite was formed using the dip-coating wetting technique. The prepared PZT precursor solution was driven into the nanopore channels of AAO template under the driving force of capillary action, subsequently the sintering process of the as-filled templates was carefully tuned to obtain Pb(Zr_0.52Ti_0.48)O₃ nanotubes of crystalline tetragonal phase with uniform pore size and ordered arrange. Fourier transform infrared spectroscopy (FTIR) results show that in the 1200–1900 cm⁻¹ band, the composite structure of PZT/AAO has obvious absorption peaks at 1471.56 cm⁻¹ and 1556.09 cm⁻¹, the absorption intensity of the composite structure is about six times of pure AAO template. The unusual optical properties found in PZT/AAO composite will stimulate further theoretical and experimental interests in ferroelectric nanostructures.     

LaNiO3缓冲层对Pb(Zr,Ti)O3铁电薄膜的影响

采用化学溶液法在Pt／Ti／SiO2／Si衬底上制备了PbZr0．4Ti0.6O3／LaNiO3(PZT／LNO)多层薄膜。X射线衍射测量表明LNO缓冲层的引入使PZT薄膜(111)择优取向度减小,(100)取向增加。原子力显微镜测量表明引入LNO缓冲层使得PZT薄膜表面更加平整、致密。在LNO缓冲层上制备的PZT薄膜具有优良的铁电特性和介电特性：LNO缓冲层厚度为40nm时,500kV／cm的外加电．场下。剩余极化(Pr)为37．6μC／cm^2,矫顽电场(Ec)为65kV／cm;100kHz时,介电常数达到822,并且发现LNO缓冲层的厚度为40nm,PZT的铁电、介电特性改进最为显著。     

Measurement and modeling of dielectric properties of Pb(Zr,Ti)O3 ferroelectric thin films

In this study, the real and imaginary parts of the complex permittivity of lead zirconate titanate ferroelectric thin films are studied in the frequency range of 100 Hz to 100 MHz. The permittivity is well fitted by the Cole-Cole model. The variation of the relaxation time with the temperature is described by the Arrhenius law and an activation energy of 0.38 eV is found. Because of its nonlinear character, the dielectric response of the ferroelectric sample depends on the amplitude of the applied ac electric field. The permittivity is composed of three different contributions: the first is due to intrinsic lattice, the second is due to domain wall vibrations, and the third is due to domain wall jumps between pinning centers. This last contribution depends on the electric field, so it is important to control the field amplitude to obtain the desired values of permittivity and tunability.