Sol－Gel法合成K（Ta，Nb）O_3材料

以金属醇盐乙酸钾［Ｋ（ＯＣ２Ｈ５）］，乙醇铌［Ｎｂ（ＯＣ２Ｈ５）５］和乙醇钽［Ｔａ（ＯＣ２Ｈ５）５］为原料，用Ｓｏｌ－Ｇｅｌ法合成了Ｋ（Ｔａ，Ｎｂ）Ｏ３超细粉末和薄膜，研究了工艺参数如前驱体溶液浓度、热处理温度等因素对材料结构及物性的影响．粉料的粒径为２０～４０ｎｍ，所需合成温度约为７００℃，比通过传统的固相反应制备同种材料的合成温度低近１００℃；以ＳｒＴｉＯ３（１００）单晶作基片，采用匀胶法获得了沿（１００）高取向生长的Ｋ（Ｔａ０．６５Ｎｂ０．３５）Ｏ３薄膜，薄膜表面均匀、致密，室温时呈立方相晶格结构．研究表明，选择物理性质相似、晶格常数相匹配的材料作基片，适当控制工艺参数，尤其是前驱体溶液的浓度、升降温速度及烧结温度是获得优质薄膜的关键．     

KTN凝胶热处理过程中的反应机理研究

本文研究了Ｓｏｌ－Ｇｅｌ法制备的ＫＴａ０．６５Ｎｂ０．３５Ｏ３（ＫＴＮ）凝胶在热处理过程中的反应机理，发现钙钛矿结构的ＫＴＮ由四步反应生成：５４２℃生成Ｋ３Ｔａ５Ｏ１４．５Ｈ２Ｏ，５９３℃生成Ｋ５Ｎｂ２Ｏ６（Ｏ，ＯＨ）．ｎＨ２Ｏ（α０＝１０．５８Ａ），此两相为立方烧绿石结构，６２０℃未经中间相直接生成ＫＴＮ，６８０℃两种烧绿石结构反应生成ＫＴＮ。     

溶胶—凝胶方法制备KTa0.65Nb0.35O3薄膜的凝胶化和热处理研究

本文较系统地研究了溶胶－凝胶方法制备ＫＴａ０．６５Ｎｂ０．３５Ｏ３薄膜的凝胶化行为和热处理。用自制的金属醇盐ＫＯＣ２Ｈ５、Ｎｂ（ＯＣ２Ｈ５）５和Ｔａ（ＯＣ２Ｈ５）５为原料，无水乙醇作溶剂，配制均匀的溶液。实验结果表明，溶液浓度、介质或催化剂的使用、匀胶时的环境温度和湿度及单层膜厚等因素凝胶薄膜的形成有较大影响。条件适宜时可得到与衬底附着紧固的均匀透明的凝胶薄膜。随着热处理温度升高，薄膜首先从非晶态     

Sol—Gel法合成K（Ta,Nb）O3材料

以金属醇盐乙醇钾［Ｋ（ＯＣ２Ｈ５）］，乙醇铌［Ｎｂ（ＯＣ２Ｈ５）５］和乙醇钽［Ｔａ（ＯＣ２Ｈ５）５］为原料，用Ｓｏｌ－Ｇｅｌ法合成了Ｋ（Ｔａ，Ｎｂ）Ｏ３超细粉末和薄膜，研究了工艺参数如前驱体溶液浓度、热处理温度等因素对材料结构及物性的影响。粉料的粒径为２０￣４０ｎｍ，所需合成温度约为７００℃，比通过传统的固相反应制备同种材料的合成温度低近１００℃；以ＳｒＴｉＯ３（１００）单晶作基片，采用匀胶法获得     

离子束辅助沉积制备TiO_2-Nb_2O_5氧敏薄膜

采用离子束辅助沉积方法在Ａｌ２Ｏ３陶瓷衬底上制备了ＴｉＯ２Ｎｂ２Ｏ５氧敏薄膜。考察了薄膜组分比及退火温度对薄膜氧敏特性和结构的影响。电阻氧分压特性测试结果表明，纯Ｎｂ２Ｏ５薄膜的氧敏特性优于纯ＴｉＯ２薄膜；掺入少量的Ｔｉ可使Ｎｂ２Ｏ５薄膜的氧敏特性提高，以５ｍｏｌ％ＴｉＯ２掺杂的Ｎｂ２Ｏ５薄膜最佳；过量掺杂则使Ｎｂ２Ｏ５薄膜的氧敏特性明显变差。在５ｍｏｌ％ＴｉＯ２Ｎｂ２Ｏ５薄膜中再掺入少量的Ｐｔ（０３％０５％）可使其氧敏特性更好，而且其响应时间大大缩短。Ｘ射线衍射谱（ＸＲＤ）和Ｘ射线光电子谱（ＸＰＳ）分析表明，在退火后的ＴｉＯ２Ｎｂ２Ｏ５薄膜中Ｎｂ２Ｏ５为单斜（Ｍｆｏｒｍ）结晶相，而掺杂的Ｔｉ以非晶的ＴｉＯ２形式存在，即使在高达３４ｍｏｌ％ＴｉＯ２Ｎｂ２Ｏ５薄膜中也不例外。纯ＴｉＯ２膜为金红石结构。不同退火温度（９００１１０００Ｃ）对薄膜的氧敏特性和结构无明显影响。     

离子束辅助沉积制备TiO2—Nb2OT氧敏薄膜

采用离子束辅助沉积方法在Ａｌ２Ｏ３陶瓷衬底上制备了ＴｉＯ２－Ｎｂ２Ｏ５的氧敏薄膜。考察了薄膜组分比及退火温度对薄膜氧敏特性和结果的影响。电阻－氧分压特性测试结果表明，纯Ｎｂ２Ｏ５薄膜的氧敏特性优于纯ＴｉＯ２薄膜；掺入少量的Ｔｉ可使Ｎｂ２Ｏ５薄膜的氧敏特性提高，以５ｍｏｌ％ＴｉＯ２掺杂的Ｎｂ２Ｏ５薄膜最佳；     

KTa1—xNbxO3薄膜的制备研究

结合自己的工作，介绍电光，热释电ＫＴａ１－ｘＮｂｘＯ３薄膜材料的制备研究进展，评述了Ｓｏｃ－ＧｅｌＰＬＤ，ＭＯＤ，ＬＰＥ和射频平面磁控溅射等技术制备ＫＴＮ薄膜的工艺特点，根据Ｓｅｌ－Ｇｅｌ技术制备ＫＴＮ材料的反应机理研究结果，指出钾含量不足是导致焦绿石结构相不能向钙钛矿结构相转变的本质原因。     

常压MOCVD制备MgO薄膜的研究

本文首次报道用常压金属有机化学气相沉积（ＡＰ－ＭＯＣＶＤ）在Ｓｉ（１００），ＳｉＯ２／Ｓｉ（１００）和Ｐｔ／Ｓｉ（１００）衬底上外延高质量的ＭｇＯ薄膜。研究了衬底温度与薄膜的取向性关系和ＭｇＯ薄膜的潮解特性。高纯ｍａｇｎｅｓｉｕｍａｃｅｔｙｌａｃｅｔｏｎａｔｅ［ｂｉｓ（２，４－ｐｅｎｔａｎｅｔａｎｅ－ｄｉｏｎｏ）ｍａｇｎｅｓｉｕｍ］［Ｍｇ（ＣＨ２ＣＯＣＨ２ＣＯＣＨ３）２］作为金属有机源，扫描电镜（ＳＥＭ），透射电镜（ＴＥＭ）和Ｘ－ＲＡＹ衍射实验显示，在较低的衬底温度（～４８０℃）下一次淀积成单晶膜。薄膜均匀，致密，结晶性和取向性很好，衬底温度（Ｔｓ）在４００℃到６８０℃之间，在Ｓｉ（１００）衬底上生长的ＭｇＯ薄膜都具有［１００］取向，在Ｓｉ（１００）、ＳｉＯ２／Ｓｉ（１００）和Ｐｔ／Ｓｉ（１００）衬底上生长的ＭｇＯ薄膜也都具有［１００］取向。     

对向靶溅射高饱和磁化强度（Fe,Ti）—N薄膜

本实验用对向靶溅射仪分别在Ｓｉ（１００），ＮａＣｌ单昌衬底上成功地制备出具有高饱和磁化强度的（Ｆｅ，Ｔｉ）－Ｎ薄膜，研究了氮气分压和衬底温度对结构与磁性的影响。氮气分压为０．０４－０．０７Ｐａ，衬底温度淡１００－１５０℃时，有利于Ｆｅ１６Ｎ２相的形成，在此条件下制备的（Ｆｅ，Ｔｉ）－Ｎ薄膜的饱和磁化强度为２．３－２。．４６Ｔ，超过纯Ｆｅ的饱和磁化强度值。     

Sol－gel生长KTa_（1－x）Nb_xO_3电光薄膜的成分和结构

采用ＸＰＳ方法研究了ｓｏｌ－ｇｅｌ工艺制备的ＫＴＮ（ｘ＝０．３５）薄膜的成分和结构．结果表明，除了表面被碳污染外，薄膜中无残余的碳和其他杂质．其成分与原料的化学计量比相近，且沿深度均匀分布．各元素的化学状态证实薄膜系钙钛矿型ＫＴＮ结构．Ａｒ＋溅射后的ＸＰＳ谱反映Ｋ严重偏低，Ｔａ和Ｎｂ的化学状态改变，是Ａｒ＋轰击引起Ｋ择优溅射及化合物分解所致．     

单晶PMnN-PZT铁电薄膜制备与表征

利用磁控溅射方法,在MgO基底上沉积三元系铁电薄膜6%PMnN-94%PZT(6%Pb(Mn1/3,Nb2/3)O3-94%Pb(Zr0.45,Ti0.55)O3),采用淬火方法对薄膜进行后期热处理。分别运用面内和面外X射线衍射(XRD)技术分析薄膜长相及晶体结构,运用高分辨率扫描电镜(SEM)观察薄膜的晶粒表面及截面结构。实验结果表明,所沉积薄膜为单晶钙钛矿结构薄膜,薄膜结构优良。     

KTa0.6Nb0.4O3粉体溶剂热和水热法合成的对比研究

以Nb2O5和Ta2O5为前驱反应物，KOH为矿化剂，采用水热法和溶剂热法两种合成工艺制备了KTa1-xNbxO3（KTN）陶瓷粉体．实验结果表明，反应溶剂（水／异丙醇）和矿化剂KOH的摩尔浓度是影响KTN粉体结构和形貌的关键因素．采用水热工艺制备的KTN粉体，当KOH浓度达到3mol／L、反应温度为523K、反应时间8h时，开始出现以焦绿石结构为主的KTN粉体；随着KOH的浓度和反应温度的增加，粉体中的钙钛矿结构成分随之增加，而焦绿石结构则逐渐减少，但始终难以完全消除．采用溶剂热法，在KOH浓度1-2mol／L、反应温度523K、反应时间8h的条件下，合成了立方相钙钛矿结构KTa0.6Nb0.4O3陶瓷粉体，KTN晶粒形状呈规则的立方体，尺寸约为30-50nm；最后对溶剂热法合成纳米粉体的机理进行了分析讨论．     

硅基Bi4Ti3O12薄膜的C-V特性研究

Bi4 Ti3O12是典型的层状钙钛矿结构铁电材料,具有优良的压电、铁电、热释电和电光等性能,可广泛应用于铁电存储器、压电和电光等器件.本文在硅衬底上利用溶胶凝胶法制备出Bi4 Ti3O12铁电薄膜,并且对其性能进行了研究.测量不同退火温度下得到的Ag/BTO/p-Si结构的C-V曲线,结果表明Bi4 Ti3O12薄膜在合适的制备工艺下可望实现极化型存储.     

新型脉冲激光能量计用无铅(Na_(1-x)K_x)_(0.5)Bi_(0.5)TiO_3铁电薄膜的制备及其激光感生热电电压信号的研究

采用脉冲激光沉积(PLD)技术,分别在LaA lO3(LAO)、(La,Sr)(A l,Ta)O3(LAST)及SrTiO3(STO)三种不同的单晶衬底上制备了一系列无铅(Na1-xKx)0.5B i0.5TiO3(x=0.00,0.08,0.19,0.30,NKBT)铁电薄膜材料。利用X射线衍射(XRD)仪对薄膜结构进行了分析,结果表明在单晶平衬底上生长的薄膜都是单取向生长的外延膜,其中摇摆曲线的半高宽(FWHM)显示在(La,Sr)(A l,Ta)O3单晶衬底上生长的薄膜结晶质量最好。另外,在20°倾斜的(La,Sr)(A l,Ta)O3单晶衬底上生长的(Na1-xKx)0.5B i0.5TiO3铁电薄膜中还首次观察到了激光感生热电电压(LITV)信号。发现在能量为0.48mJ/pulse的紫外脉冲激光辐照下,其最大激光感生热电电压为31mV,完全满足了制作脉冲激光能量计探测元件的要求,有望开发出可集成的新型脉冲激光能量计。     

Synthesis of lead-free (K, Na)(Nb, Ta)O3 nanopowders using a sol-gel process

Lead-free (K0.5Na0.5)(Nb0.7Ta0.3)O3 piezoelectric material was successfully synthesized via a sol-gel process. Crystalline (K0.5Na0.5)(Nb0.7Ta0.3)O3 nanopowders were obtained after heat treatment at 700 degrees C. The particle size was estimated to be 87nm +/- 23 nm. The transmission electron microscopy images showed that individual nanoparticles were single crystalline and had a pseudo-cubic structure with a lattice parameter of -3.96 angstroms. Both X-ray diffraction and scanning electron microscopy studies consistently showed that the crystallization of the (K0.5Na0.5)(Nb0.7Ta0.3)O3 occurred slightly above 500 degrees C. The samples have an appropriate stoichiometry as found via energy dispersive X-ray spectroscopy. The demonstration of the synthesis of (K0.5Na0.5)(Nb0.7Ta0.3)O3 via a sol-gel process as presented in this paper can provide an important foundation for the development of a synthetic route towards (K0.5Na0.5)(Nb0.7Ta0.3)O3 doped with various other elements for high performance piezoelectric devices.     

氧化物La-Ca-Mn-O巨磁电阻薄膜的制备及其结构特性的研究

采用磁控溅射方法在ＺｒＯ２（００１）、Ｓｉ（００１）和玻璃衬底上成功地制备了ＬａＣａＭｎＯ（以下简称为ＬＣＭＯ）巨磁电阻薄膜。Ｘ－射线分析表明，ＺｒＯ２的晶格常数与ＬＣＭＯ的晶格常数失配虽然较大，仍可得到较好的ＬＣＭＯ薄膜。在Ｓｉ片上难以制备出致密完整的ＬＣＭＯ薄膜，其原因有待查明。玻璃衬底上可以获得纯相的ＬＣＭＯ巨磁电阻薄膜，在ＺｒＯ２衬底上制备的ＬＣＭＯ薄膜，其巨磁电阻效应在１５０Ｋ，３０００Ｇａｕｓ下达１３％左右。     

Structure and dielectric performance of K-doped (Pb0.5Ba0.5)ZrO3 thin films

In the present investigation (Pb_0.5Ba_0.5)ZrO₃ (PBZ) thin films doped by K (KPBZ) from 0 to 5 mol% were successfully deposited on Pt-buffered silicon substrates by a sol-gel method. The K content dependence of microstructure and electrical properties of KPBZ thin films were studied in detail. It was found that, although all the films displayed a pure perovskite structure without obvious difference, the surface roughness of KPBZ films was decreased with increasing K content. Dielectric measurements showed that the figure of merit (FOM) values of KPBZ thin films were greatly increased by K-doping, and at the same time that the temperature-dependent stability was also improved. Thus, K doping is a promising way to optimize the overall electrical properties of PBZ thin films for potential application in tunable devices.     

Fabrication of multi-layer optical waveguide by LPE technique

Multi-layer structure optical waveguides, consisting of Li(Nb,Ta)O₃ and LiTaO₃ thin films, were fabricated on LiTaO₃ substrates (Z- and Y-plates) by LPE technique. Solution compositions appropriate for Li(Nb,Ta)O₃ optical waveguiding layers and LiTaO₃ cladding layers were examined from the viewpoints of lattice matching, refractive indices and saturation temperature for LPE dipping. Based on determined solutions, multi-layer film consisting of Li(Nb,Ta)O₃ and LiTaO₃ were epitaxially grown alternately onto the substrates. Optical propagation losses in Li(Nb,Ta)O₃ waveguiding layers were 0.5 ～ 0.9 dB/cm.     

Orientation-dependent phase transition and dielectric properties of Ba0.85Ca0.15Ti0.9Zr0.1O3 thin films

Polycrystalline Ba_0.85Ca_0.15Ti_0.9Zr_0.1O₃ (BCZT) thin films with (100) preferential and random orientation are prepared on the LaNiO₃ electrodes coated on Si substrates by chemical solution deposition process. The results show that the two types of films stabilize in the pure perovskite structure. The ferro-paraelectric phase transitions of two types of films occur at the temperature ranges of 280.2–297.8 K and 278.4–287.6 K, respectively. The dielectric constant, relaxation time and tunability of the random orientation film are smaller than those of the (100) preferential film but both almost have the similar leakage current characteristics. The mechanism associated with the change of the electrical properties of the thin films is also discussed.     

Preparation of complex oxide thin films under hydrothermal and hydrothermal-electrochemical conditions

Thin-film growth of complex oxides including BaTiO₃, SrTiO₃, BaZrO₃, SrZrO₃, KTaO₃, and KNbO₃ were studied by the hydrothermal and the hydrothermal-electrochemical methods. Hydrothermal-electrochemical growth of ATiO₃ (A = Ba, Sr) thin films was investigated at temperatures from 100° to 200°C using a three-electrode cell. Current efficiency for the film growth was in the range from ca. 0.6% to 3.0%. Tracer experiments revealed that the ATiO₃ film grows at the film/substrate interface. AZrO₃ (A = Ba, Sr) thin films were also prepared on Zr metal substrates by the hydrothermal-electrochemical method. By applying a potential above ca. +2 V vs. Ag/AgCl to the Zr substrates, AZrO₃ thin films were formed uniformly. KMO₃ (M = Ta, Nb) thin films were prepared on Ta metal substrates by the hydrothermal method. Perovskite-type KTaO₃ thin films were formed in 2.0 M KOH at 300°C. Pyrochlore-type K₂Ta₂O₆ thin films were formed at lower temperatures and lower KOH concentrations. Morphotropic phase changes were also revealed in the hydrothermal system KTaO₃-KNbO₃.