用改进的sol-gel法制备锆钛酸铅薄膜及其物相转化的研究

利用改进的solgel法,在Pt/Ti/SiO2/Si衬底上制备了PbZr0.5Ti0.5O3(PZT50/50)薄膜.采用了一种新的方式,从同一前驱体溶液得到了厚度各异的单一退火层.研究了薄膜的结构和性质随单层退火厚度的改变而发生的变化,发现随着单一退火层厚度的降低,薄膜(111)取向的程度增大,同时薄膜的剩余极化和介电常量也逐渐增高.当单一退火层厚度降低到约为40nm时,可得到高度(111)择优取向的PZT薄膜.从薄膜成核机理的基础上讨论了薄膜结构变化的内在因素,认为随单一退火层厚度的增加薄膜由单一的 关键词：     

(111)择优取向的Pb(Zr0.52Ti0.48)O3铁电薄膜的制备及研究

选用不同浓度的Pb(Zr0.52Ti0.48)O3溶胶,用Sol-gel法在Pt/Ti/SiO2/Si基片上沉积一层厚度不同的Pb(Zr0.52Ti0.48)O3(PZT52)过渡层,经400℃烘烤、550℃退火等程序后,再用Sol-gel法在PZT52过渡层上沉积Pb(Zr0.52Ti0.48)O3薄膜.XRD分析表明,有PZT52过渡层的Pb(Zr0.52Ti0.48)O3薄膜具有(111)择优取向的钙钛矿结构,且随着过渡层厚度的增加,Pb(Zr0.52Ti0.48)O3薄膜的(111)择优取向程度越高.SEM分析表明,当PZT52过渡层的厚度达到14nm以上,Pb(Zr0.52Ti0.48)O3薄膜结晶程度得到明显改善,平均晶粒尺寸大大增加.介电、铁电性能测试表明,与没有过渡层的Pb(Zr0.52Ti0.48)O3薄膜相比,有PZT52过渡层的Pb(Zr0.52Ti0.48)O3薄膜具有较大的介电常数和剩余极化强度,而介电损耗则较小.     

不同衬底上Pb(Zr0.52Ti0.48)O3择优取向铁电薄膜的制备和研究

通过MOD法在Si(100)和Pt(111)/Ti/SiO₂/Si基片上制备出LaNiO₃ ( LNO)薄膜.再通过修 正的Sol-gel法，在Pt(111)/Ti/SiO₂/Si,LNO/Si(100)和LNO/Pt/Ti/SiO_{2< /sub>/Si三种衬底上 制备出具有择优取向的Pb(Zr0.52Ti0.48)O3铁电薄膜. 经XRD分析表明，L NO薄膜具有(100)择优取向的类钙钛矿结构；PZT薄膜均具有钙钛矿结构，且在Pt(111)/Ti/S iO2/Si衬底上的薄膜以(110)择优取向，在LNO/Pt/Ti/SiO2/Si和LN O/Si(100)衬底上的 薄膜以(100)择优取向.经场发射SEM分析和介电、铁电性能测试表明，在LNO/Si和LNO/Pt/Ti /SiO2/Si衬底上的PZT薄膜的平均粒径、介电常数以及剩余极化强度均比以Pt/T i/SiO2/Si为衬底的薄膜大. 关键词： 3}薄膜')" href="#">LaNiO₃薄膜 PZT铁电薄膜 择优取向 剩余极化强度     

不同衬底上Pb(Zr0.52Ti0.48)O3择优取向铁电薄膜的制备和研究

通过MOD法在Si(100)和Pt(111)/Ti/SiO2/Si基片上制备出LaNiO3 (LNO)薄膜.再通过修正的Sol-gel法,在Pt(111)/Ti/SiO2/Si,LNO/Si(100)和LNO/Pt/Ti/SiO2/Si三种衬底上制备出具有择优取向的Pb(Zr0.52Ti0.48)O3铁电薄膜.经XRD分析表明,LNO薄膜具有(100)择优取向的类钙钛矿结构;PZT薄膜均具有钙钛矿结构,且在Pt(111)/Ti/SiO2/Si衬底上的薄膜以(110)择优取向,在LNO/Pt/Ti/SiO2/Si和LNO/Si(100)衬底上的薄膜以(100)择优取向.经场发射SEM分析和介电、铁电性能测试表明,在LNO/Si和LNO/Pt/Ti/SiO2/Si衬底上的PZT薄膜的平均粒径、介电常数以及剩余极化强度均比以Pt/Ti/SiO2/Si为衬底的薄膜大.     

PLD法制备PZT-YBCO结构的铁电薄膜的研究

本文利用脉冲准分子激光在LaAlO3单晶基片上淀积了YBCO和Zr/Ti为94/6的PZT铁电薄膜,并通过高频溅射将Pt蒸镀在PZT薄膜上作为上电极;用X射线衍射表征了该多层膜的晶相结构,测量了PZT的铁电性能和介电特性,讨论了PZT/YBCO薄膜的制备工艺,以及工艺条件对晶相结构和薄膜性能的影响.     

(111)择优取向的Pb(Zr0.52Ti0.48)O3铁电薄膜的制备及研究

选用不同浓度的Pb(Zr_0.52Ti_0.48)O₃溶胶，用Sol-gel法在Pt/Ti/SiO₂/Si基片上沉积一层厚度不同的Pb(Zr_0.52Ti_0.48)O₃ (PZT52)过渡层，经400℃烘烤、550℃退火等程序后，再用Sol-gel法在PZT52过渡层上沉积Pb(Zr_0.52Ti_0.48)O _{关键词： PZT铁电薄膜 择优取向 过渡层 剩余极化强度}     

(111)取向生长Pb(Zr0:95Ti0:05)O3纳米晶薄膜的铁电与热释电特性

" 在Pt/Ti/SiO2/Si基片上用溶胶-凝胶法与快速退火工艺制备了300 nm厚的锆钛酸铅Pb(Zr0:95Ti0:05)O3 (PZT95/5)反铁电薄膜．结果显示600~700 ℃晶化处理的钙钛矿PZT95/5薄膜具有高度(111)取向生长特性．薄膜的电性能测量采用金属-铁电-金属电容器结构．在20 V电压作用下,600~700 ℃晶化处理的PZT95/5薄膜显示出饱和电滞回线．在1 kHz下,600、650和700 ℃晶化的薄膜介电常数与损耗分别为519与0.028、677与0.029、987     

CoPt(FePt)-C纳米复合膜的结构与磁性

用磁过滤脉冲真空电弧沉积方法制备了CoPt(FePt) C纳米复合薄膜，并在不同温度下进行了退火处理，研究了薄膜中碳的含量以及退火温度对薄膜结构与磁性能的影响.制备态薄膜经过足够高的温度退火后，x射线衍射和磁力显微镜分析发现，在碳基质中生成了面心四方相的CoPt(FePt)纳米颗粒.对于特定组分为Co24Pt31C45和Fe43Pt35C22的薄膜，矫顽力以及颗粒尺寸都随退火温度的升高而增大，当退火温度为700℃时，Co24Pt31C45薄膜的矫顽力为21×105A/m，晶粒尺寸为17nm;当退火温度为650℃时，Fe43Pt35C22相应值分别为28×105A/m和105nm. 关键词： 磁记录材料 磁性薄膜 CoPt FePt纳米复合薄膜     

脉冲高能量密度等离子体沉积(Ti,Al)N薄膜组织及其性能研究

利用脉冲高能量密度等离子体技术在室温条件下在45＃钢基材表面沉积了高硬度耐腐蚀(Ti, Al)N薄膜. 利用扫描电子显微镜、X射线衍射、X射线光电子能谱、俄歇电子能谱分析了薄膜的显微组织.利用纳米压痕仪测试了薄膜的纳米硬度.测试了薄膜在05mol/L H2SO4水溶液中的耐蚀性. 测试结果表明：薄膜主要组成相为(Ti, Al)N，同时含有少量的AlN,薄膜的纳米硬度高达26 GPa,薄膜具有良好的耐蚀性，与1Cr18Ni9Ti奥氏体不锈钢相比，耐蚀性提高了一个数量级. 关键词： 脉冲高能量密度等离子体 薄膜 纳米硬度 耐蚀性     

PbTiO3/PbZr0.3Ti0.7O3/PbTiO3夹心结构铁电薄膜子晶层的优化

用Sol-Gel法制备了Pb(1 x)TiO3/PbZr0.3Ti0.7O3/Pb(1 x)TiO3(PT/PZT/PT)夹心结构及PZT铁电薄膜,为了获得高质量的PT/PZT/PT夹心结构铁电薄膜,使用不同过量Pb配比(x)的PbTiO3 (PT)层进行制备,以获得优化的PT子晶层.X射线衍射和原子力显微镜分析结果表明PT层中过量Pb配比(x)对薄膜的微结构影响很大,只有PT层中Pb过量配比x＝0.10-0.15的薄膜为表面晶粒大小均匀致密的纯钙钛矿结构.X射线电子能谱对薄膜微区进行元素成分分析表明,对x=0.00的薄膜,在表面和界面处Pb明显的缺乏;而x=0.20时的薄膜,Pb则明显的过量.薄膜的铁电性能、疲劳特性和漏电流特性等电学性能与PT层中过量Pb配比(x)没有明显的变化趋势,但与薄膜的结晶性能密切相关.结晶性能较好的薄膜,其电学性能也较好.说明PT层中过量Pb配比(x)是通过影响PT子晶层自身的结晶,而影响整个薄膜的结晶行为,并进一步影响到整个薄膜的电学性能.因此,在其他工艺参数都相同时,PT层中合适的过量Pb配比应为x=0.10-0.15.优化的子晶层不仅能获得结晶性能较好的薄膜,而且薄膜的电学性能也好.     

Texture control of Pb(Zr, Ti)O3 thin films with different post-annealing processes

The non-crystalline Pb(Zr, Ti)O₃ thin films sputtered on Pt(1 1 1)/Ti/SiO₂/Si(1 0 0) substrates at room temperature were crystallized by conventional furnace annealing (CFA) and rapid thermal annealing (RTA), respectively. It was found that the RTA process favored the (1 1 1)-preferred orientation in lead zirconate titanate (PZT) thin films while the CFA process favored the (1 0 0)-preferred orientation. The origin of the different orientation selection might be due to the different epitaxial nucleation mechanism. The long heating duration would lead to the aggregation of Pb and the formation of PbO(1 0 0) on film surface; therefore, the nucleation at the PbO(1 0 0)/PZT interface on film surface might lead to the (1 0 0)-preferred orientation. However, the nucleation at the PZT/Pt(1 1 1) electrode interface by RTA process would result in the formation of (1 1 1)-preferred orientation. The RTA-derived (1 1 1)-preferentially oriented PZT thin films exhibited a high remnant polarization of 35 μC/cm².     

Annealing effect of platinum-based electrodes on physical properties of PZT thin films

This study examined the crystal structure and surface morphology, including the Ti segregation mechanism on the surface due to the inter-diffusion between Pt, Ti and TiO_x as a glue layer, according to the annealing temperature and growth orientation of a Pt film. In addition, the fatigue mechanism of ferroelectric PZT thin films deposited on a Pt-based electrode was also investigated. The nano-structure, orientation mapping, and micro-morphologies of the triangular Pt hillocks were investigated by scanning electron microscopy with an electron backscatter diffraction (EBSD) function. The D–E hysteresis loop of the ferroelectric films was measured using a Sawyer–Tower circuit at 1 kHz to obtain the remanent polarization and coercive field.     

Preparation and crystallization of Pb(Zr0.95Ti0.05)O3 thin films deposited by radio-frequency magnetron sputtering with a stoichiometric ceramic target

0.95 Ti_0.05)O₃ (PZT 95/5) thin films of perovskite structure were prepared on various substrates by the radio-frequency magnetron sputtering with a stoichiometric ceramic target. The crystal structure of the films showed a strong dependency on the crystal structure of the substrates. After conventional-furnace annealing at 750 °C, crack-free and transparent epitaxial PZT 95/5 films were successfully obtained on SrTiO₃(100) substrates, and highly oriented films on LaAlO₃(012). The films on r-sapphire exhibit slightly preferred orientation along both the (040) and (122) axes of the orthorhombic PZT 95/5 phase. The films on YSZ(100) consist principally of the perovskite PZT 95/5 phase with random orientation with a small portion of unknown phase. However, the formation of the perovskite PZT 95/5 phase was not observed in the films on Si(110) or (111)Pt-coated Si substrates. The crystallization of the perovskite PZT 95/5 on these substrates could be improved by rapid thermal annealing (RTA). Single perovskite phase was obtained in the films on (111)Pt/Si which had RTA at 750 °C for 1 min. No tangible loss of Pb from the films occurred during either the sputtering or annealing. Received: 17 April 1997/Accepted: 18 November 1997     

Influence of plasma pressure on the growth characteristics and ferroelectric properties of sputter-deposited PZT thin films

PZT thin films of thickness (320-1040) nm were synthesized on Si/SiO₂/Ti/Pt multilayered substrates by radio frequency magnetron sputtering. The influence of plasma pressure in the range of (0.24-4.9) Pa, during deposition, on the structural, electrical and ferroelectric properties of the PZT films was systematically studied. X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and cross-sectional transmission electron microscopy (XTEM) were employed for structural study. Nano-probe Energy Dispersive (EDX) line scanning was employed to investigate the elemental distribution across the film-bottom electrode interface. I-V characteristics and polarization-electric field (P-E) hysteresis loop of the films were measured. The study reveals that the plasma pressure has a strong influence on the evolution and texture of the ferroelectric perovskite phase and microstructure of the films. At an optimum plasma pressure of 4.1 Pa, PZT films are grown with 93% perovskite phase with (1 1 1) preferred orientation and uniform granular microstructure. These films show a saturation polarization of 67 μC/cm², remnant polarization of 30 μC/cm² and coercive field of 28 kV/cm which, according to the literature, seem to be suitable for device applications.Transmission electron microscopy (TEM) study shows that at a plasma pressure of 4.1 Pa, the PZT/bottom Pt interface is sharp and no amorphous interlayer is formed at the interface. At a higher plasma pressure of 4.9 Pa, poor I-V and P-E hysteresis loop are observed which are interpreted as due to an amorphous interlayer at the film-bottom electrode interface which is possibly enriched in Pb, Zr, O and Pt.     

Investigation the effects of the excess Pb content and annealing conditions on the microstructure and ferroelectric properties of PZT (52-48) films prepared by sol-gel method

The effects of the PbO volatilization, excess Pb content of PbZr_0.52Ti_0.48 (PZT) precursor, PbTiO₃ (PT) seeding layers and annealing condition on the microstructures, surface morphologies, preferred orientation and ferroelectric properties of PbZr_0.52Ti_0.48 films were systematically investigated. PZT films with a variety of excess Pb (0-20%) were spin-deposited on Si(1 0 0) and Pt(1 1 1)/Ti/SiO₂/Si(1 0 0) substrates by sol-gel technique. The films composition, Pb/Zr/Ti/O atom rate and Pb loss were semiquantitative analyzed by X-ray photoelectron spectrometer (XPS). When the excess Pb of PZT precursor was 10%, the Pb/Zr/Ti/O atomic rate of the fabricated films was very close to the designed rate of 1:0.52:0.48:3. The XRD and AFM investigations confirmed that PT seeding layer promoted the PZT films perovskite phase transformation and grains growth with (1 1 0) plane preferred orientation, accordingly lowered perovskite phase crystallization temperature and reduced Pb loss. The PZT films annealed in O₂ flow demonstrated better microstructure and ferroelectric properties comparing with films annealed in air by double remnant polarization increase and 8% coercive field increase. The underlying mechanism was also investigated.     

Crystallization behaviour of PZT in multilayer heterostructures

Microstructural and electrical properties of PZT (lead zirconate titanate) thin films prepared by sol-gel techniques at annealing temperatures in the range from 550°C to 900°C are studied. Perovskite (Pe) grain nucleation in PZT film starts but not completes at 550°C. Along with formation of round Pe (111) grains on the Pt (111) interface, the film contains small Pe and pyrochlore (Py) grains. Films annealed at the temperatures higher than 600°C demonstrate column structure of Pe grains, the amount of Py inclusions reduces with the annealing temperature and practically disappears at 700°C. An increase of annealing temperature leads to enhancement of (100) Pe orientation as a result of Ti diffusion on the Pt surface. Polarization decreases with the annealing temperature (maximum at 600°C), whereas permittivity increases up to the annealing temperature of 750°C.     

Effect of Pb2Ru2O7-x (PRO) conductive interfacial layers on ferroelectric properties of Pt/Pb(Zr0.35Ti0.65)O3/Pt capacitors for nonvolatile memory applications

A conductive material, Pb₂Ru₂O_7-x (PRO), containing Pb in a cubic structure was introduced into a Pt/PZT interface in an attempt to improve the ferroelectric properties of PZT films. PRO and PZT films were prepared by rf magnetron sputtering and chemical solution deposition, respectively. The resistivity of PRO thin films in a hybrid-type electrode (PRO/Pt) structure was approximately 35–45 μΩ·cm and the surface roughness remained constant with increasing annealing temperature. The PRO interlayers suppressed the loss of Pb in PZT layers by diffusion to the Pt/PZT interface. The increase in remanent polarization was largely dependent on the PRO interlayers inserted at the bottom-Pt/PZT interface rather than at the top-Pt/PZT interface. In addition, the leakage-current behavior of PZT films in a sandwich structure was improved substantially compared to the case of PRO interlayers only at the bottom-Pt/PZT interface. Thus, the PRO interlayers play an important role in improving the ferroelectric properties of PZT thin films for use in nonvolatile memory device applications. PACS 68.55.-a; 73.40.Rw; 73.61.Ng; 77.55.+f; 81.15.Cd     

Nanoscale domain switching mechanism in Pb(Zr,Ti)O<Subscript>3</Subscript> thin film

Pb(Zr,Ti)O₃ (PZT) ferroelectric thin film was prepared by the sol-gel technique and crystallized with a (111) preferred orientation. The domain structure and polarization reversal behavior were investigated by using scanning force microscopy (SFM) piezoresponse mode at the nanometer scale. A step structure of approximately 30 nm in width was directly observed, which was formed during the polarization reversal process. The presence of the step structure reveals that the forward domain-growth mechanism is the dominant domain-switching process in our PZT thin films. Received: 6 August 2002 / Accepted: 9 August 2002 / Published online: 28 October 2002 RID="*" ID="*"Corresponding author. Fax: +86-21/5241-3122, E-mail: huarongzeng@163.net     

Crystallization kinetics in ferroelectric thin films: Viability of atomic force microscopy

The pyrochlore to perovskite phase transformation was studied in lead zirconate titanate (PZT) thin films. The films were fabricated on platinum electrodes and annealed by rapid thermal processing (RTP). The phases which formed and their location in the film were analyzed using glancing angle XRD and depth profiling was demonstrated. Grain size and structure, nucleation sites and surface morphology were determined with transmission electron microscop (TEM) and atomic force microscopy (AFM). The role of AFM in this type of transformation study was assessed.

The PZT films crystallized with a (100) orientation which was preferentially nucleated at the platinum/film interface. RTP at 650°C for 15 s was sufficient to complete the transformation. However, columnar grain growth and improvements in the ferroelectric properties were obtained with increased RTP time. A PZT film with RTP at 650°C for 1 min possessed a remanent polarization of 25 μC/cm² and a dielectric constant of ε = 650.