Phase evolution and effect of pre-heating temperature on the characteristics of PZT thin films grown by using a triol sol--gel route

Lead zirconate titanate (PZT) films were fabricated on Pt(111)/Ti/SiO₂/Si(100) using the triol sol--gel method. The effect of the pre-heating temperature on the phase transformations, microstructures, electrical properties and ferroelectric properties of the PZT thin films was investigated. Randomly-oriented PZT thin films pre-heated at 400°C for 10?min and annealed at 600°C for 30?min showed well-defined ferroelectric hysteresis loops with a remanent polarization of 26.57?µC?cm^?2 and a coercive field of 115.42?kV?cm^?1. The dielectric constant and dielectric loss of the PZT films were 621 and 0.0395, respectively. The microstructures of the thin films are dense, crack-free and homogeneous with fine grains about 15–20?nm in size.     

Secondary defects in low-energy As-implanted Si

14 /cm² dose of As ions followed by both isochronal and isothermal annealing. The elementary defects generated first during solid-phase epitaxial recovery of implantation-induced amorphous layers at temperatures of 550 °C and/or 600 °C are {311} defects 2–3 nm long. They are considered to be transformed into {111} and {100} defects after annealing at temperatures higher than 750 °C. These secondary defects show the opposite annealing behavior to the dissolution and growth by the difference of their depth positions at 800 °C. This phenomenon is explained by the diffusion of self-interstitials contained in defects. With regard to the formation and dissolution of defects, there is no significant difference between the effects of rapid thermal annealing (950 °C for 10 s) and furnace annealing (800 °C for 10 min). Received: 14 November 1997/Accepted: 16 November 1997     

Temperature dependent surface and spectral modifications of nano V<Subscript>2</Subscript>O<Subscript>5</Subscript> films

Nanocrystalline V₂O₅ films have been deposited on glass substrates at 300°C substrate temperature using thermal evaporation technique and were subjected to thermal annealing at different temperatures 350, 400, and 550°C. X-ray diffraction (XRD) spectra exhibit sharper and broader characteristic peaks respectively indicating the rearrangement of nanocrystallite phases with annealing temperatures. Other phases of vanadium oxides started emerging with the rise in annealing temperature and the sample converted completely to VO₂ (B) phase at 550°C annealing. FESEM images showed an increase in crystallite size with 350 and 400°C annealing temperatures followed by a decrease in crystallite size for the sample annealed at 550°C. Transmission spectra showed an initial redshift of the fundamental band edge with 350 and 400°C while a blue shift for the sample annealed at 550°C, which was in agreement with XRD and SEM results. The films exhibited smart window properties as well as nanorod growth at specific annealing temperatures. Apart from showing the PL and defect related peaks, PL studies also supported the observations made in the transmission spectra.     

Enhanced fatigue property of PZT thin films using LaNiO3 thin layer as bottom electrode

A highly (100)-oriented metallic LaNiO₃ film was prepared directly on a Si substrate by a simple metalorganic decomposition (MOD) technique using lanthanum nitrate and nickel acetate as the starting sources. Subsequent Pb(Zr,Ti)O₃ (PZT) thin films deposited on the LaNiO₃-coated Si substrate were obtained by a modified sol–gel method. It was found that the PZT thin films began to form a single perovskite phase at a low annealing temperature of 530 °C, and exhibited highly (100) orientation. A ferroelectric capacitor of Pt/Pb(Zr,Ti)O₃/LaNiO₃/Si annealed at 600 °C displayed a good P-E hysteresis characteristic and was fatigue-free even after 10¹¹ switching cycles. Received: 25 May 2000 / Accepted: 9 August 2000 / Published online: 30 November 2000     

Structure and magnetic properties of annealed metastable FeAg/Pt films

FeAg and FeAg/Pt films were prepared by dc magnetron sputtering at room temperature. The effects of Ag volume fraction in FeAg films and postannealing temperature and time on structure and magnetic properties of FeAg and FeAg/Pt films have been investigated. The results show that the as-deposited FeAg films are metastable. After annealing at 300°C, the phase separation of metastable FeAg films happened and the highest coercivity is obtained in Fe₅₀Ag₅₀/Pt film. With increasing annealing temperature, the ordering and the magnetic properties of the Fe₅₀Ag₅₀/Pt films were improved. When the Fe₅₀Ag₅₀/Pt films are annealed at 600°C for different annealing times, a long annealing time enhances the ordering of the metastable Fe₅₀Ag₅₀/Pt films and affects the orientation development. When the films are annealed for a long time, the grain size and the magnetic domain size also increase, which lead to an increase of correlation length due to the growth of FePt grains.     

Enhancement of in-plane magnetic anisotropy in (111)-oriented Co0.8Fe2.2O4 thin film by deposition of PZT top layer

The CoFe₂O₄ and Co_0.8Fe_2.2O₄ single layer (CFO) as well as PZT/CoFe₂O₄ and PZT/Co_0.8Fe_2.2O₄ bilayer thin films were grown using the pulsed laser deposition technique on Pt(111)/Si substrates at 600 °C. All films had a perfect (111)-orientation and the degree of orientation of CFO films was improved by the deposition of a PZT top layer. Precision X-ray diffraction analysis (avoiding the shift of peaks due to sample misalignment) revealed that the CFO films on Pt(111)/Si substrate were under an out-of-plane contraction and the deposition of a PZT top layer led to the increase in the out-of-plane contraction. The (111)-oriented CFO single layer films had a strong in-plane magnetic anisotropy as a result of orientation as well as the stress-induced magnetic anisotropy. The magnetic properties of CFO film were altered by the deposition of a PZT top layer leading to the enhancement of in-plane magnetic anisotropy. The enhanced in-plane magnetic anisotropy was more detectable in PZT/Co_0.8Fe_2.2O₄ rather than PZT/CoFe₂O₄ bilayer film, which could be expected from its higher magnetocrystalline as well as magnetostriction constants.     

Properties of the Ce–Pd–Pt(111) overlayer system

The Pd–Pt(111) and the Ce–Pd–Pt(111) overlayer systems were studied by X-ray photoelectron spectroscopy and low-energy electron diffraction (LEED). Variations in the work function were measured by ultraviolet photoelectron spectroscopy. The Pd overlayer thicknesses were in the range of 1 to 4 monolayers (MLs). The Ce overlayer thicknesses were in the range is of 0.5 to 1.5 MLs. The interfaces were studied for annealing temperatures up to 700°C. Surface alloying or intermixing of Ce, Pd and Pt was observed. Upon deposition at ambient temperatures, Ce forms an overlayer. During annealing, both Pd and Ce were found to dissolve into the Pt substrate. For a Pd coverage of about 1 ML, the Ce–Pd–Pt(111) system was found to be Pt, terminated after annealing to 700°C. For Pd coverage above 1 ML, both Pd and Pt were found to be present at the surface. Cerium was found to be absent from the top surface layer in both cases.     

Effects of heating rate on the magneto-optical properties of bismuth-substituted yttrium iron garnet films prepared via modified metal-organic decomposition

This work investigated the effects of heating rate and annealing on the magneto-optical properties of bismuth-substituted yttrium iron garnet (Bi-YIG) thin films on glass and (111)-oriented single-crystalline gadolinium gallium garnet (GGG) substrates fabricated by metal-organic decomposition (MOD). We modified the MOD method by eliminating the pre-annealing process. We performed annealing at various temperatures to determine the optimal temperature for obtaining the Bi-YIG phase. We then annealed at the optimized temperature using various heating rates. The optimal conditions were annealing for 1 h at 750 °C at a heating rate of 30 °C/min on GGG to obtain highly crystallized fine grains. The Faraday rotation for this film was about −10.5°/μm. The optimized heating rate enhanced the magneto-optical properties due to improved crystallinity and saturated magnetization. The Bi-YIG thin films prepared by this prescribed MOD method exhibited excellent magneto-optical performance and are potential candidates for applications in optical devices.     

Curie temperatures of CoPt ultrathin continuous films

The effects of layer thickness and thermal annealing on Curie temperature have been studied for CoPt ultrathin continuous layers in AlN/CoPt multilayer structures. It is found that there exists a critical thickness below which Curie temperature rapidly decreases due to the loss of spin-spin interactions in the vicinity of interface. After high temperature annealing, the in-plane lattice constant of CoPt film is increased and the exchange coupling parameter is decreased. Consequently, Curie temperatures decrease for some films with large thickness, compared with as-deposited state. Upon annealing at 600?^°C, CoPt undergoes ordering transformation, which also contributes to the degradation of the Curie temperature. However, when the CoPt film thickness is below 2?nm, the Curie temperature is increased after annealing. Especially for 1?nm thick film, the Curie temperature is strikingly increased from 173?^°C to 343?^°C after annealing at 600?^°C. This effect is attributed to the out-of-plane lattice deformation of CoPt thin layers in AlN/CoPt multilayer structures.     

The growth temperatures dependence of optical and electrical properties of InN films

InN films grown on sapphire at different substrate temperatures from 550°C to 700°C by metalorganic chemical vapor deposition were investigated. The low-temperature GaN nucleation layer with high-temperature annealing (1100°C) was used as a buffer for main InN layer growth. X-ray diffraction and Raman scattering measurements reveal that the quality of InN films can be improved by increasing the growth temperature to 600°C. Further high substrate temperatures may promote the thermal decomposition of InN films and result in poor crystallinity and surface morphology. The photoluminescence and Hall measurements were employed to characterize the optical and electrical properties of InN films, which also indicates strong growth temperature dependence. The InN films grown at temperature of 600°C show not only a high mobility with low carrier concentration, but also a strong infrared emission band located around 0.7 eV. For a 600 nm thick InN film grown at 600°C, the Hall mobility achieves up to 938 cm²/Vs with electron concentration of 3.9 × 10¹⁸ cm⁻³. Supported by the National Basic Research Program of China (Grant No. 2006CB6049), the National Natural Science Foundation of China (Grant Nos. 6039072, 60476030 and 60421003), the Great Fund of the Ministry of Education of China (Grant No. 10416), the Specialized Research Fund for the Doctoral Program of Higher Education of China (Grant No. 20050284004), and the Natural Science Foundation of Jiangsu Province of China (Grant Nos. BK2005210 and BK2006126)     

不同晶化工艺对非晶PZT纳米薄膜形核取向生长机理的影响

射频磁控溅射法室温下在Pt/Ti/SiO2/Si上制备非晶Pb(Zr048Ti052)O3薄膜，非晶PZT薄膜分别经常规炉退火(CFA)处理和快速热退火(RTA)处理晶化为（100），（111）不同择优取向的多晶薄膜. 采用x射线衍射测定了薄膜相组分、择优取向度；用原子力显微镜和压电响应力显微镜观察了薄膜表面形貌，以及对应区域由自发极化形成的铁电畴像，观察了不同取向薄膜的电畴分布特征. 结果表明，RTA晶化过程钙钛矿结构PZT结晶主要以PZT/Pt界面处的PtPb化合物为成核点异质形核并类似外延的结晶生长，沿界面结晶速率远大于垂直膜面结晶速率，而CFA晶化样品成核发生在膜内杂质缺陷处，以同质成核为主. 不同的成核机理导致了不同晶面择优取向生长. 关键词： PZT薄膜 结晶 形核 力显微技术     

KTN thin films prepared by pulsed laser deposition on transparent single crystal quartz(100)

Using the Sol-Gel method to produce the KTN ultrafine powder and the sintering technique with K2O atmosphere to prepare KTN ceramics as the targets instead of the KTN single crystal, highly oriented KTN thin films were produced on the transparent single crystal quartz (100) by the pulsed laser deposition (PLD). Since the thermal stress sustained by the quartz is relatively small, the limit temperature of the quartz substrates (300℃) is much lower than that of the P-Si substrates (560℃); the prepared thin film is at amorphous state. Increasing the pulsed laser energy density in the process incorporated with annealing the film after deposition at different temperatures converts the amorphous films into crystal. The optimal pulsed laser energy density and annealing temperature were 2.0 J/cm2 and 600℃, respectively. A discussion was made to understand the mechanism of film production at relatively low substrate temperature by PLD and effects of the annealing temperatures on the forming of the perovskite p     

Photoluminescence characteristics of ZnGa2O4 thin films prepared by chemical solution method

Zinc gallate (ZnGa₂O₄) thin film phosphors have been formed on ITO glass substrates by a chemical solution method with starting materials of zinc acetate dihydrate, gallium nitrate hydrate and 2-methoxiethanol as a solution. The thin films were firstly dried at 100 °C and fired at 500 °C for 30 min and then, annealed at 500 °C and 600 °C for 30 min under an annealing atmosphere of 3% H₂/Ar. XRD patterns of the thin film phosphors showed (311) and (220) peak indicating ZnGa₂O₄ crystalline phase in which all the (311) peaks of the film phosphors synthesized on ITO glass and soda-lime glass revealed high intensity with increasing annealing temperature from 500 °C to 600 °C. The ZnGa₂O₄ thin film phosphors represented marked change in AFM surface morphologies according to an annealing temperature under an annealing atmosphere (3% H2/Ar). The film phosphor, annealed at 600 °C, showed the embossed pattern with relatively regular spacing in AFM surface morphology. The ZnGa₂O₄ thin film phosphors formed on ITO glass, which were annealed at different temperatures and showed distinctive spectra with peak wavelengths of 434 nm and 436 nm in the blue emission region.     

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     

Effects of thermally induced anatase-to-rutile phase transition in MOCVD-grown TiO2 films on structural and optical properties

Titanium dioxide (TiO₂) films with a thickness of 550 nm were deposited on quartz glass at 300 °C by metalorganic chemical vapor deposition. The effects of post-annealing between 600 °C and 1000 °C were investigated on the structural and optical properties of the films. X-ray diffraction patterns revealed that the anatase phase of as-grown TiO₂ films began to be transformed into rutile at the annealing temperature of 900 °C. The TiO₂ films were entirely changed to the rutile phase at 1000 °C. From scanning electron spectroscopy and atomic force microscopy images, it was confirmed that the microstructure of as-deposited films changed from narrow columnar grains into wide columnar ones. The surface composition of the TiO₂ films, which was analyzed by X-ray photoelectron spectroscopy data, was nearly constant although the films were annealed at different temperatures. When the annealing temperature increased, the transmittance of the films decreased, whereas the refractive index and the extinction coefficient calculated by the envelope method increased at high temperature. The values of optical band gap decreased from 3.5 eV to 3.25 eV at 900 °C. This abrupt decrease was consistent with the anatase-to-rutile phase transition. Received: 4 October 2000 / Accepted: 4 December 2000 / Published online: 23 May 2001     

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     

(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     

微结构对Eu掺杂Bi4Ti3O12铁电薄膜铁电性能的影响

采用金属有机物分解法在Pt/Ti/Si(111)基底上制备了退火温度分别为600℃,650℃,700℃的Bi_3.15Eu_0.85Ti₃O₁₂(BET)铁电薄膜,并对其结构及铁电性能进行了测试,再使用扫描探针显微镜对BET薄膜的电畴翻转进行了实时观测.BET薄膜c畴发生180°畴变的最小电压为+6V,而r畴由于其高四方性,即使极化电压增至+12V也不会发生翻转.薄膜的铁电性主要源于c畴的极化,随着退火温度的升高,c畴的区域面积增加,BET薄膜的剩余极化强度随之增大.退火温度为700℃的BET薄膜剩余极化强度达到84μC/cm². 关键词： 铁电薄膜 电畴翻转 扫描探针显微镜     

Improving the performance of pure sulfide Cu(InGa)S2 solar cells via injection annealing system

In this study, we present an effective method of improving the performance of pure sulfide Cu(InGa)S₂ (CIGS) solar cells via injection annealing system. The injection annealing system can perform annealing at desired temperatures, and therefore, the CIGS thin film passed over the temperature range in which secondary phases occurs. Via the injection annealing system, secondary phase InS_x was effectively removed from the surface of the CIGS thin films at the temperatures over 550°C. This resulted in the formation of good-quality P–N junction CIGS devices, thereby improving significantly the performance of the CIGS solar cell. In addition, the open-circuit-voltage (V_OC) and fill factor (FF) of the CIGS devices increased gradually with increasing annealing temperature in the range of 550–640°C. It is speculated that the bulk defects were decreased as the annealing temperature increased. Finally, via injection annealing system, a pure sulfide CIGS solar cell with an efficiency of 12.16% was achieved.     

Effect of the Crystal Structure on the Electrical Properties of Thin-Film PZT Structures

A new method of two-stage crystallization of lead zirconate–titanate (PZT) films using a seed sublayer with a low excess lead content has been proposed and realized. A seed layer with a strong texture of perovskite Pe(111) grains is formed from a solution with a lead excess of 0–5 wt %; the fast growth of the grains is provided by the deposition of the main film from a solution with high lead content. As a result, a strong Pe(111) texture with complete suppression of the Pe(100) orientation forms. An analysis of current–voltage dependences of the transient currents and the distributions of the local conductivity measured by the contact AFM method reveals two various mechanisms of current percolation that are determined by traps in the bulk and at the perovskite grain interfaces.