Characteristics of Sputter-deposited Gadolinia-doped Ceria Thin Films on Al2O3/SiO2/Si Systems

Metal oxide films prepared by thin film technology have been reported for the potential applications on thin solid electrolyte layers for solid oxide fuel cells(SOFCs). Gadolinia-doped ceria(GDC) thin films and Al2O3 layers on SiO2/Si substrates are successively deposited by RF reactive magnetron sputtering from a cerium-gadolinium (90:10 at.%) alloy target and Al target in O2/Ar gas mixture and then perform post-thermal treatments at 300-700 ℃ and 900 ℃ for 2 h, respectively. Materials characteristics and chemical compositions of GDC films and Al2O3 layers are investigated by X-ray photoelectron spectroscopy(XPS), cross-sectional scanning electron microscopy(SEM), X-ray diffraction(XRD), and atomic force microscopy(AFM). Stoichiometric Al2O3 layers with polycrystalline structures are firstly prepared onto SiO2/Si substrates. A cubic fluorite structure with columnar crystallites of GDC films is successfully deposited on Al2O3/SiO2/Si systems. The chemical composition of 700 ℃-annealed GDC films is (Ce0.91Gd0.09)O1.94 and possesses a higher film density of 7.257 g/cm3. As a result, GDC thin films prepared by RF reactive magnetron sputtering and post-thermal treatments can be used as thin solid electrolyte layers for intermediate temperature SOFCs system as compared to the well-known yttria-stabilized zirconia(YSZ).     

Influence of substrate orientation on the morphologyand orientation of LaNiO3 thin films

LaNiO₃ thin films were successfully prepared by a chemical method from citrate precursors. The LNO precursor solution was spin‐coated onto Si (100) and Si (111) substrates. To obtain epitaxial or highly oriented films, the deposited layers were slowly heated in a gradient thermal field, with a heating rate of 1° min^?1, and annealed at 700°C. The influence of different substrate orientations on the thin film morphology was investigated using atomic force microscopy and X‐ray diffraction analysis. Well‐crystallized films with grains aligned along a certain direction were obtained on both substrates. Films deposited on both substrates were very smooth, but with a different grain size and shape depending on the crystal orientation. Films deposited on Si (100) grew in the (110) direction and had elongated grains, whereas those on Si (111) grew in the (211) direction and had a quasi‐square grain shape.     

Development of RF magnetron sputtering method to fabricate PZT thin film actuator

PZT piezoelectric very thin films suitable for a microactuator have been deposited onto Invar alloy substrate using a high-temperature RF magnetron sputtering technique. PZT thin films must be deposited onto conductive substrate for a monomorph or a bimorph actuator. The chemical composition and the crystalline structure of these films were measured by ESCA and XRD, respectively. The chemical composition of PZT deposited stoichiometrically was almost the same as commercially-produced bulk PZT. Crystal planes (1 1 0) and (1 1 1) of PZT perovskite structure were observed in XRD analysis. When the substrate was heated to above 600 °C, SEM revealed only a very small number of pinholes on the surface. A thin (500 nm) film actuator has been characterized by measuring the piezoelectric property using a Laser Doppler Vibrograph. It was confirmed that the piezoelectric property has a linear relationship with the grain size, which also increased with the substrate temperature. The piezoelectric property of deposited PZT thin films showed a good agreement with a quoted value of bulk PZT, when the substrates were heated to 600 °C.     

厚度效应对Pb(Zr0.53Ti0.47)O3薄膜微结构、铁电、介电性能的影响

用改进的溶胶-凝胶法在Pt(111)/Ti/SiO₂/Si(100)衬底上制备了不同厚度的高度(111)取向的Pb(Zr_0.53Ti_0.47)O₃薄膜.运用X射线衍射(XRD)和原子力显微镜(AFM)分析了薄膜的微结构,原子力显微镜表明厚度为0.3μm和0.56μm的PZT薄膜的晶粒尺寸和表面粗糙度分别为0.2～0.3μm、2～3μm和0.92nm、34nm.0.3μm和0.56μm PZT薄膜的剩余极化(Pr)和矫顽场(Ec)分别为32.2μC/²、79.9kV/cm, 27.7μC/cm²、54.4kV/cm;在频率100KHz时,薄膜的介电常数和介电损耗分别为539、0.066,821、0.029.     

Influence of target grit count and sintering temperature on pulsed laser deposition of SiC thin films

A pulsed laser deposition (PLD) technique for depositing SiC on Si(100) substrates using Nd³⁺:YAG laser at 355 nm is studied. The influence of substrate temperature, ambient pressure, and SiC powder grit size on both structure and morphology of SiC thin film is investigated. Further, the influence of the target preparation on the reduction of droplet formation during Nd³⁺:YAG laser-assisted pulsed laser deposition of SiC thin films is investigated. Experimental studies show that multicrystalline SiC film can be obtained with temperature ranging from 600 to 700 °C and at an ambient pressure of about 5.5 × 10^?3 Pa. Further, droplet formation on the deposited film was reduced significantly by selecting the grit count of SiC powder 500 and the pressure of 2 × 10^?2 Pa. SiC target sintered at 1,600 °C showed a reduced wear during the laser ablation. The X-ray diffraction (XRD) and the Raman spectroscopy studies on deposited films clearly show the multicrystalline (combined 3C-SiC and 4H-SiC) nature of SiC films. I-V characteristics of deposited SiC film on n-type c-Si substrate also indicated that SiC thin film possesses P-type semiconductor properties.     

Electron energy-loss spectroscopy study of thin film hafnium aluminates for novel gate dielectrics

We have used conventional high‐resolution transmission electron microscopy and electron energy‐loss spectroscopy (EELS) in scanning transmission electron microscopy to investigate the microstructure and electronic structure of hafnia‐based thin films doped with small amounts (6.8 at.%) of Al grown on (001) Si. The as‐deposited film is amorphous with a very thin (～0.5 nm) interfacial SiO_x layer. The film partially crystallizes after annealing at 700 °C and the interfacial SiO₂‐like layer increases in thickness by oxygen diffusion through the Hf‐aluminate layer and oxidation of the silicon substrate. Oxygen K‐edge EELS fine‐structures are analysed for both films and interpreted in the context of the films’ microstructure. We also discuss valence electron energy‐loss spectra of these ultrathin films.     

Some aspects of atom probe specimen preparation and analysis of thin film materials

Some of the factors in the preparation of atom probe specimens of metallic multilayer thin films have been investigated. A series of Ti/Nb multilayer films were sputtered deposited on n-doped Si [001] substrates with either 5 or 0.05Omega cm resistivity. Each wafer was pre-fabricated into a series of 5 microm x 5 microm x approximately 80 microm island posts by photolithography and reactive ion etching. Once the film was grown on the wafer, a Si post was mounted to either a tungsten or stainless steel fine tip needle that was mechanically crimped to a Cu tube for handling. The specimen was then loaded into a Focus Ion Beam instrument where a sacrificial Pt cap was in situ deposited onto the surface of the film and subsequently annularly ion milled into the appropriate geometry. The Pt cap was found to be an effective method in reducing Ga ion damage and implantation into the film during milling. The multilayers deposited on the high resistivity Si exhibited uncontrolled field evaporation which lead to high mass tails in the mass spectra, a reduction in the mass resolution, high background noise, propensity for "flash-failure", and a variation in the apparent layer thickness as the experiment elapsed in time. The multilayers deposited on lower resistivity Si did not suffer from these artifacts.     

The role of substrates on the structural,optical, and morphological properties of zno nanotubes prepared by spray pyrolysis

ZnO films were deposited onto glass, ITO coated glass, and sapphire substrate by spray pyrolysis, and subsequently annealed at the same temperature of 400°C for 3 h. The role of substrate on the properties of ZnO films was investigated. The structural and optical properties of the films were investigated by X‐ray diffractometer (XRD) and photoluminescence (PL) spectrophotometer, respectively. The surface morphology of the nanostructured ZnO film was investigated by scanning electron microscopy (SEM) and atomic force microscopy (AFM). Crystallographic properties revealed that the ZnO films deposited on sapphire and ITO substrates exhibit a strong c‐axis orientation of grains with hexagonal wurtzite structure. Extremely high UV emission intensity was determined in the film on ITO. The different luminescence behaviors was discussed, which would be caused by least value of strain in the film. Films grown on different substrates revealed differences in the morphology. ZnO films on ITO and sapphire substrates revealed better morphology than that of the film on glass. AFM images of the films prepared on ITO show uniform distribution of grains with large surface roughness, suitable for application in dye sensitized solar cells. Microsc. Res. Tech. 77:211–215, 2014. © 2013 Wiley Periodicals, Inc.     

Characterization of self-assembling isolated ferroelectric domains by scanning force microscopy

Lead zirconate titanate (PZT) thin films were prepared by a sol–gel process on platinized Si substrate. Their microstructure and surface morphology were characterized by XRD and Scanninn Force Microscopy. Phase transformation of the prepared PZT films from pyrochlore to ferroelectric was observed by XRD and PFM (piezoresponse force microscopy), respectively. Self-assembling nano-structured ferroelectric phases are fabricated by solution deposition technique followed by the controlling kinetics of the transformation. Complex structures of ferroelectric domains in the isolated ferroelectric phases were found in the furnace annealed PZT films in the temperature range of 400–500°C. Single ferroelectric domain structure in the isolated ferroelectric phases could be found in thinner PZT films and used to study the size effect of laterally confined ferroelectric domains.     

BIMORPH-TYPE PIEZOELECTRIC THIN FILM BENDING ACTUATORS SYNTHESIZED BY HYDROTHERMAL METHOD

Lead zirconate titanium solid-solution (PZT) thin films with various thickness are synthe-sized on titanium substrates by repeated hydrothermal treatments. Young modulus, electric-field-in-duced displacement and the density of the PZT film are measured respectively. Bimorph- type bendingactuators are fabricated using these films. The model, which is used to analyze the driving ability ofbimorph-type bending actuators by hydrothermal method, is set up. It can be seen that the drivingability of bimorph-type bending actuators can be greatly improved by optimizing the thickness of PZTthin film and substrae from the theoretical analysis results. The measured values are expected to agreewith the theoretical values calculated by the above model.     

硅基PZT压电功能结构研究

PZT压电薄（厚）膜是制备MEMS传感元件和执行元件重要的功能材料,对近年PZT薄（厚）膜在MEMS领域的研究现状进行了分析,提出了一种新型的双杯PZT/Si膜片式功能结构;采用有限元方法对双杯PZT/Si膜片进行了结构优化,得到PZT和上、下硅杯的结构优化值为DPZT: D1:D2 =0.75:1.1:1;一阶模态谐振频率为13.2KHz;以氧化、双面光刻、各向异性刻蚀,以及PZT厚膜丝网印刷等工艺技术制作了双杯硅基PZT压电厚膜膜片,该膜片具有压电驱动功能。双杯PZT/Si膜片式功能结构的MEMS技术兼容性好,对芯片内其它元件或电路的影响小,适合作为MEMS片内执行元件的驱动机构。     

Piezoelectric and electromechanical properties of relaxor ferroelectric Pb(Mg1/3Nb2/3)O3(65%)-PbTiO3(35%) thin films observed by scanning force microscopy

Relaxor ferroelectric PbMg(1/3)Nb(2/3)O(3)(65%)-PbTiO(3)(35%) (PMN-35PT) thin films were grown by a sol-gel method on Pt(111)/TiO(2)/SiO(2)/Si(100) substrates. Piezoresponse and poling behavior appear to have a relation with the relaxor behavior of the materials. Piezoelectric images were studied in a number of regions on the films with subsequent statistical analysis of the obtained data using the contact mode of scanning force microscopy. Hysteresis loops were observed with external field applied over a wide range of the vibration frequency. The piezoelectric coefficient, d(33), and the crystallographic electrostrictive constant, Q(33), were also determined as 100pm/V and 2.8x10(-3)C(-2)m(4), respectively.     

Electrostatic force microscopy study on the domain switching properties of the Pb(Zr0.2Ti0.8)O3 thin films with different crystallographic orientations for the probe-based data storage

The domain switching properties of the ferroelectric Pb(Zr(0.2)Ti(0.8))O(3) (PZT) thin films with two types of crystallographic orientations were investigated by electrostatic force microscopy (EFM). The crystallographic orientations of the PZT thin films were random on the (111)Pt/MgO(100) and c-axis preferred on the (100)Pt/MgO(100), respectively. When dc bias was applied to the films for writing in micro-scale area, electrostatic force images showed that the domain switching was hard in the PZT thin films with random orientation, while the pattern could clearly be written in the PZT films with c-axis orientation. The differences in the domain switching properties of each PZT thin film were investigated in the crystallographic orientations point of view, and the domain switching dynamics were also measured by investigating the nano-sized dot switching behavior with respect to the width of the applied voltage pulse.     

锑掺杂纳米SnO2透明导电薄膜的制备与性能研究

采用溶胶-凝胶法在Si片、已镀SiO2的钠钙硅玻璃和普通钠钙硅玻璃上镀Sb掺杂摩尔分数为8%的SnO2薄膜(ATO),在450℃热处理温度下对薄膜结构,电学、光学性能进行表征。结果表明:薄膜以四方金红石结构存在,结晶完全;方阻值随镀膜层数的增加而明显降低,12层时薄膜最低方阻值为129Ω/□,可见光平均透过率在75%以上。随着波长的增大,红外波段的反射率逐渐增大,从15%增加到55%左右。     

静电辅助气溶胶化学气相沉积法制备Al_2O_3薄膜

以乙酰丙酮铝为前驱体,N,N-二甲基甲酰胺为溶剂,采用静电辅助的气溶胶化学气相沉积(ESAVD)方法,在Si(100)衬底上制备了Al2O3薄膜,并采用场发射扫描电镜、能谱仪、X射线衍射仪和自动划痕仪等设备对制备的薄膜进行了表征。结果表明:采用ESAVD法制备的Al2O3薄膜平整致密而且晶粒细小,薄膜与基体之间及薄膜内部都未出现开裂现象;薄膜与基体的结合力约为5.56 N;沉积得到的薄膜为化学计量比为2∶3的氧化物薄膜;退火前的薄膜为非晶态,在1 200℃退火保温2 h后薄膜转变为-αAl2O3。     

Microstructure and Magnetic Properties of Sputtered Co5 Sm Films

Co5Sm/Cr bilayer films were deposited on Si and glass slides by means of a Direct-Current(DC)magnetron sputtering system with substrate heating.Magnetic properties measurements show that the sample with glass substrate has a comparatively large coercivity(Hc=2 141.2 Oe)with a relatively low optimal temperature(Ts=350 ℃).X-ray diffraction patterns indicate that Cr presents a hexagonal-close-packed(hcp)texture on Si,while a body-centered-cubic(bcc)structure on glass substrate,which leads to Co5Sm films having different lattice constants on Si and glass substrates.At their optimal temperature,the grain size of the sample on glass slide is smaller with its size distribution more uniform.Concurrently,the shape of magnetic domain is more regular and ordered.The value of magnetic switching volume(V)for the film on glass is 1.65×10-18 cm3,smaller than that for films on Si.For the film on glass,the magnetization reversal mechanism is mainly influenced by magnetocrystalline anisotropy,the shape of the crystal grain and the stress in the film.     

基于薄膜退火的MoS_2/SiO_2/Si异质结太阳能电池光伏性能提高

为了制备高效的MoSi/SiO_2/Si异质结太阳能电池,利用磁控溅射技术制备MoS_2薄膜,并在硫气氛下对MoS_2薄膜进行退火处理。分别用退火和未退火的MoS_2薄膜制备MoS_2/SiO_2/Si异质结太阳能电池,研究了退火对MoS_2薄膜的微观结构和MoS_2/SiO_2/Si异质结太阳能电池光电性能的影响。实验结果显示,相比于未退火的,经过退火处理的MoS_2薄膜的拉曼峰半高宽(FWHM)变窄,峰强增强,显微荧光光谱中也出现明显的激子发光峰。由此表明,退火处理使MoS_2薄膜由非晶向晶态转变,薄膜的体缺陷减少,异质结太阳能电池的开路电压和填充因子得到提升,器件转换效率从0.94%提高到1.66%。不同光照强度下的J-V测量和暗态的J-V测量结果表明,经退火处理的MoS_2薄膜的异质结太阳能电池具有较高的收集电压和更接近于1的理想因子,这归因于退火导致MoS_2薄膜的体缺陷的减少,近而降低了MoS_2/SiO_2/Si异质结太阳能电池器件的体缺陷复合。     

Patterned crack-free PZT thick films for micro-electromechanical system applications

The fabrication and structuring of multilayer-thick film piezoelectric (PZT-lead zirconate titanate) structures, using composite sol-gel techniques and wet etching is described. The composite sol-gel technique involves producing a PZT powder/sol composite slurry which when spun down, yields films a few micrometres thick. Repeated layering and infiltration has been used to produce PZT films between 10 and 40 μm thick. Due to the low firing temperature (<720°C), it has also been possible to produce PZT films with embedded thin (ca. 100 nm thick) metal electrodes. The PZT thick films have also been structured using a wet etching technique. Examples of features and cavities with lateral dimensions in the order of tens of micrometres are presented. The ability to fabricate and structure thick functional films with embedded metal electrode structures offers the possibility to create novel micro-device structures suitable for use in micro-electromechanical systems (MEMS).     

纳米硅-氧化硅薄膜的XPS测量

利用XPS能很好地分辨出硅基纳米硅-氧化硅膜层中的n-Si和n-SiO2。对Si2P峰进行的拟合处理，可计算出n-Si和n-SiO2的含量，其结果与RF-磁控溅射沉积薄膜中所用的复合靶Si和SiO2的面积比基本一致。     

A Monte Carlo study of the thickness determination of ultra-thin films

A Monte Carlo method is utilized to simulate the energy spectra for low-energy electron backscattered from different thin films deposited on different bulk substrates. A method of thickness determination for ultra-thin films is presented, which is obtained from the analysis of the basic characteristics of the energy spectra of backscattered electrons. This method is predicted to be particularly suitable for determining the thickness of ultra-thin films, and to be useful for both cases of light film on heavy substrate and heavy film on light substrate. The thickness resolution is estimated to be as high as subnanometer scale, provided the resolution of the electron energy spectrometer used to be high enough.