溶胶–凝胶法制备 Pb(Zrx, Ti1–x)O3 薄膜研究进展

Pb(Zrx, Ti1-x) (PZT)铁电薄膜因具有优良的铁电性、压电性、热释电性和声光性能而受到广泛关注,其电、光性能与其制备过程密切相关。简要介绍了 PZT 薄膜制备工艺流程,系统地从前驱体溶液、摩尔比 r(Zr:Ti)、热处理工艺、电极材料以及掺杂改性等五个方面概述了 sol-gel 法制备 PZT 薄膜的研究进展,并指出了目前 sol-gel 法制备 PZT 铁电薄膜研究中存在的一些问题以及未来的研究方向。     

Pb（Zrx，Ti1-x）O3成分梯度铁电薄膜的制备、结构及电性能表征

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(Zrx,Ti1-x)O3成分梯度薄膜.经俄歇微探针能谱仪(AES)对制备的"上梯度"薄膜进行了成分深度分析,结果证实其成分梯度的存在.经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.经介电频谱测试表明,梯度薄膜的介电常数比每个单元的介电常数都大,但介电损耗相近.在10 kHz时,上、下梯度薄膜的介电常数分别为206和219.经不同偏压下电滞回线的测试表明,上、下梯度薄膜均表现出良好的铁电性质,其剩余极化强度Pr分别为24.3和26.8 μC·cm-2.经热释电性能测试表明,热释电系数随着温度的升高逐渐增加,室温下上、下梯度薄膜的热释电系数分别为5.78和4.61×10-8 C·cm-2K-1,高于每个单元的热释电系数.     

PLD法制备高介电调谐率的纳米晶BZT薄膜

用脉冲激光沉积工艺制备了Ba(ZrxTi1-x)O3(x=0.25,0.30简称BZT25和BZT30)介电薄膜。在650℃原位退火10 min,薄膜为(111)取向柱状生长的晶粒,取向度分别为0.45和0.75。BZT25和BZT30薄膜的平均晶粒尺寸分别为50 nm和60 nm。在室温、1 MHz和3×105 V/cm条件下,BZT25的最大εr和调谐率分别达到563和65%,BZT30的最大εr和调谐率分别达到441和57%。薄膜为(111)取向生长,主要是基于薄膜与底电极Pt界面层立方相结构Pt3Ti的诱导,即(111)Pt3Ti和(111)BZT的晶格匹配。     

溶胶凝胶法制备钼掺杂氧化锌薄膜及性质研究

利用溶胶凝胶法在Al₂O ₃衬底上制备出了c轴择优取向的钼掺杂氧化锌（MZO）透明导电薄膜,研究了钼的掺杂量(0~1 at%)对钼掺杂氧化锌薄膜光电性能的影响。研究结果表明：所制备的薄膜为六方纤锌矿型结构且表面平整、致密,通过高温真空退火,MZO薄膜的电阻率明显降低,且随着钼含量的增加,MZO薄膜的电阻率呈现出先减小后增大的趋势,当钼含量为0.4at.%时,获得最小电阻率为0.13 Ωcm。薄膜在近红外区域(800~2000 nm)的平均透过率大于85%,这可以有效地拓宽光电器件的光谱范围。     

Sol-Gel processing of Nb-doped Pb(Zr,Ti)O3 thin films for ferroelectric memory applications

The ferroelectric properties of Nb-doped PZT thin films prepared by a sol-gel method were evaluated relative to memory device application requirements. Within the range of 0 to 4 mol %, Nb-doping of PZT compositions near the morphotropic phase boundary region (i.e. PZT 53/47) enhanced overall ferroelectric properties by reducing the te-tragonal distortion of the unit cell. A 4 mol % Nb-doped PZT 53/47 thin film (0.26 μm) had a coercivity of 8 V/ μm, a remanence ratio of 0.54, a switchable polarization of 45 μC/cm², and a specific resistivity of 3 x 10⁹ Ω-cm. Nb-doping levels in excess of 5 mol had a detrimental effect on the resulting thin film ferroelectric properties. X-ray diffraction (XRD) analysis of highly doped films showed development of a significant PbO phase accompanied by diffraction line broadening of the perovskite phase. As such, it was postulated that the creation of excessive lead vacancies in the PNZT lattice resulted in PbO accumulation at the grain boundaries which impeded grain growth, and hence, adversely affected ferroelectric switching performance. The fatigue performance of the sol-gel derived thin film capacitor system was a function of switching voltage. At switching fields sufficient to saturate the polarization, the endurance of the thin film capacitor was greater than 10⁹ cycles. Cycling with lower fields reduced endurance values, but in all cases, the switchable polarization decreased linearly with the logarithm of cycles. Nb-doping did not have a significant effect on the fatigue performance.     

无机sol-gel法制备二氧化钒薄膜的研究

采用无机sol-gel法,以分析纯V2O5为原料,在Si衬底、玻璃衬底上空气中加热制备了V2O5薄膜,在不同温度下真空退火,得到了具有择优取向的VO2薄膜。研究了其制备工艺和显微结构。结果表明:在玻璃衬底和硅衬底上薄膜的最佳真空退火工艺均为480℃/2h。所制备的VO2薄膜具有沿<110>晶向生长的择优取向。薄膜表面形貌良好,颗粒尺寸分布均匀。     

Sol-gel法制备SrTiO_3薄膜的电阻开关性能研究

采用sol-gel法制作了28nm厚的SrTiO3薄膜和Au/SrTiO3/LaNiO3/Si(100)三明治结构的器件,并研究其物理性能。结果显示:室温下,用直流电压可以使薄膜的电阻在高低阻态间进行转换。最大的电阻变化率约为10309。对I-V特性的分析,发现在高阻态时,有空间电荷限制电流机制(SCLC)和肖特基势垒导电机制存在。应用在高场区有非对称电子陷阱中心的空间电荷限制电流理论,解释了这种电阻开关现象。     

sol-gel法制备ZAO薄膜的结构与光学性能研究

采用溶胶—凝胶法在普通玻璃衬底上制备了ZAO(ZnO:A1)薄膜,利用XRD、SEM、紫外—可见光谱和光致发光光谱对所制备的AZO薄膜进行了表征,研究了ZAO薄膜的结构和光学性能.结果表明:ZAO薄膜的微晶晶相与ZnO一致,且具有c轴择优取向;ZAO薄膜在可见光区的透过率超过了88％,在350～575 nm范围内有强的...     

sol-gel法制备掺Al的ZnO薄膜及其表面形貌表征

用原子力显微镜,观察了sol-gel法制备之掺Al的ZnO薄膜的表面形貌,计算了薄膜的表面高度–高度相关函数H(r)-r,并用分形表面高度–高度相关函数的唯象表达式,对薄膜表面高度–高度相关函数进行拟合。结果表明:掺Al的ZnO薄膜表面具有典型的分形特征,Al掺杂量的增加和退火温度升高,使掺Al的ZnO薄膜的表面粗糙度w从1.39增大到5.47,分形维数Df由2.12减小到2.08,水平相关长度ξ从31.25增到76.17。     

sol-gel法制备WO3电致变色薄膜的研究

采用正交实验设计方法,优化了钨粉过氧化聚钨酸sol-gel法制备WO3薄膜的配方,并且通过测定薄膜的物相结构、光透过率和循环伏安特性等研究了薄膜的电致变色性能。结果表明,制备WO3薄膜的最优配方为:钨粉(纯度为99.5%)6g、浓双氧水20mL、无水乙醇22mL、冰醋酸6mL。该配方所制备的薄膜具有非晶态结构,且薄膜在着色态、褪色态下的透过率之差达到50%以上。     

La0.7Ca0.3MnO3多晶薄膜的sol-gel法制备及表征

以La、Ca、Mn的无机盐替代相应的醇盐,以冰乙酸为溶剂,乙酰丙酮(AcAc)为螯合剂,采用sol-gel法在Si(110)衬底上制备了La0.7Ca0.3MnO3(LCMO)多晶薄膜,并用FTIR、XRD、SEM、EDS和TEM等分析手段对薄膜进行了表征,通过不同磁场下电阻一温度(R-T)曲线,研究了样品的输运性质及...     

Optical properties of ZnO thin films prepared by sol-gel process

The present study focused on ZnO thin films fabricated by sol-gel process and spin coated onto Si (1 0 0) and quartz substrates. ZnO thin films have a hexagonal würtzite structure with a grain diameter about 50 nm. Optical properties were determined by photoluminescence (PL) and absorption spectroscopy. The absorption spectrum is dominated by a sharp excitonic peak at room and low temperatures. At room temperature, two transitions were observed by PL. One near to the prohibited energy band in ultraviolet (UV) region and the other centered at 640 nm, characteristic of the electronic defects in the band-gap. The spectrum at 6 K is dominated by donor-bound exciton lines and donor-acceptor pair transition. LO-phonon replica and two-electron satellite transitions are also observed. These optical characteristics are a signature of high-quality thin films.     

sol-gel 法制备ATO薄膜的结构与光学性能研究

采用sol-gel法在玻璃衬底上制备ATO(SnO2∶Sb)薄膜,并用XRD、SEM、紫外-可见光谱和光致发光对薄膜进行了表征,研究了ATO薄膜的结构和光学性能。结果表明:ATO薄膜微晶晶相与SnO2一致,仍然是四方金红石结构;ATO薄膜在可见光区的透过率超过80%,当r(Sb∶Sn)为0.15时,ATO薄膜的透过率最高达87%;ATO薄膜在344～380nm处有一个很强的紫外-紫光发射带,随着Sb掺杂量的增加,发射峰逐渐变强,在r(Sb∶Sn)为0.25时,发射峰相对强度达302.4。     

Pb_(0.88)La_(0.08)(Zr_xTi_(1–x))O_3铁电厚膜介电与储能性能研究

采用溶胶-凝胶法在La Ni O3/Si(100)底电极上成功制备了厚度为1μm的Pb0.88La0.08(Zrx Ti1–x)O3(PLZT,x=0.30,0.55,0.80)铁电厚膜。研究了不同Zr/Ti比对PLZT铁电厚膜的介电与储能性能的影响。结果表明,随着PLZT中Zr含量的增加,厚膜材料的储能密度与储能效率均增大,Pb0.88La0.08(Zr0.8Ti0.2)O3厚膜在1 400×103V/cm的储能密度为23.8 J/cm3,储能效率为60%。     

Structural, electrical and optical analysis of ITO thin films prepared by sol-gel

We present the results of the preparation and characterization of ITO transparent conducting layers (In₂O₃:Sn) on glass substrates by the sol-gel process. The chemical and physical parameters in the preparation of the solution and during the deposition of the films were changed, in order to analyze the structural, optical and electrical results having in mind the great technological applications of this material. The crystallographic properties and the average grain size were studied by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The optical parameters (band gap, refraction index and absorption coefficient) were determined by spectral transmittance and using a simulation software. The electrical characterization was done by the four-point probe method to determine the sheet resistance and resistivity. The films with a sheet resistance of 167.3 Ω/□, and 92.7% transmittance, average grain size of 32.7 nm and cubic structure with a lattice parameter of 10.12 Å were obtained. With the obtained appropriate parameters, low resistivity and highly transparent films, ideal for applications as contact in optical windows in solar cells, smart windows and others can prepared.     

Microstructure and domain configurations in ferroelectric PbTiO3 and Pb(Zr,Ti)O3 thin fims

Ferroelectric domain configurations in PbTiO₃ and Pb(Zr_xT_1−x)O₃ (PZT, x = 0.3 or 0.5) thin films have been studied by transmission electron microscopy. The PbTiOg and PZT thin films have been deposited by the ionized cluster beam technique and radio frequency sputtering, respectively. The grain size in these thin films is typically less than 0.5 μm. Lamellar 90°-domain features have been observed in both PbTiO₃ and PZT (30/70) samples. The domain walls correspond to the {011} twin boundaries. La-doping and Ca-modification are shown to affect the microstructure of the PZT films. No clear domain feature occurs in the PZT thin film that has composition near the morphotropic phase boundary. The effects of grain sizes are briefly discussed.     

Electrical properties of Pb(Zr,Ti)O3 films prepared on ITO glass

Pb(Zr,Ti)O₃ thin films were successfully prepared on a Pt bottom electrode with indium tin oxide coated glass substrates using RF magnetron sputtering. Use of the indium tin oxide coated glass substrate reduced the fatigue characteristics and provided for excellent crystallization of the Pb(Zr,Ti)O₃ thin films. The polarization versus fatigue characteristics showed 10% degradation after 10⁹ cycles. These results indicate that Pt/indium tin oxide double electrodes can be improved both in terms of fatigue and ferroelectric properties through the use of Pb(Zr,Ti)O₃ thin films on glass substrates, resulting in better performance than metal electrodes.     

集成光学器件的PLZT薄膜溶胶-凝胶法制备与性能研究

在掺铌钛酸锶(NST)的衬底上, 通过加入抑制开裂剂聚乙二醇对异辛基苯基醚(triton X-100), 利用溶胶-凝胶法制备了厚达4.6μm的 锆钛酸铅镧(PLZT)薄膜,从而有效地减小了其在集成光学器件应用中的传输损耗。实验分析 了triton X-100的加入量对薄膜质量的影响,并通过优化triton X-100的加入量可有效抑制薄 膜开裂。利用光学显微镜、扫描电子显微镜(SEM)、X射线衍射仪(XRD)、棱镜耦合波导 测试仪和台阶 仪等对制备的薄膜性能进行分析。结果表明,经过650℃快速退火处 理后,得到了表面平整度小于30nm、 粒径为50~100nm的钙钛矿结构PLZT薄膜,测得PLZT(8/65/35)和PL ZT(11/65/35)薄膜在 1550nm波长处的折射率分别为2. 4029和2.388。本文方法制备的 薄膜可以用于PLZT电光器件的制作。     

Electrical properties of sputtered (Ba, Sr)TiO3 thin films prepared by two-step deposition method

The influence of two-step deposition on the electrical properties of sputtered (Ba,Sr)TiO₃ thin films was investigated. BST thin films with thickness 40 nm were deposited by a simple two-step radio frequency-magnetron sputtering technique, where the BST thin film consisted of a seed layer and a main layer. The dielectric constant was strongly dependent on the thickness of seed layer, but there was no dependence on deposition temperature of the seed layer. For a 2 nm seed layer, the dielectric constants were higher by about 29% than those of single-step BST thin films due to higher crystallinity and the leakage current was nearly the same as that of a single-step sample in bias voltage from −2 to 2.5 V. However, an improvement of the dielectric constant was not observed for samples having above 4 nm thick seed layers. A 40 nm thick BST film with 2 nm thick seed layer deposited by a two-step method exhibited a SiO₂ equivalent thickness of 0.385 nm and a leakage current density of 2.74 × 10⁻⁸A/cm²at+1.5V after post-annealing under an atmosphere of flowing N₂ for 30 min at 750°C.     

Influences of embossing technology on Pb(Zr0.3,Ti0.7)O3 ferroelectric thin film

The ferroelectric random access memory (FRAM) which uses ferroelectric thin film as memory material is considered to be a candidate for the next generation memory application. In this work, we apply nano-embossing technology to fabricate Pb(Zr_0.3,Ti_0.7)O₃ (PZT) ferroelectric thin film nanostructures and investigate the influence of the patterning process on the material and ferroelectric properties by using SEM, XRD and Precision Ferroelectric Tester. Embossing process has been optimized for embossing depth and pattern profile. It was found that embossing will result in (1 0 0) preferred orientation of the PZT thin film. The electrical characteristics of patterned and un-patterned PZT films have been also studied for comparison.