Transport properties and microstructure of La0.7Sr0.3MnO3 nanocrystalline thin films grown by polymer-assisted chemical solution deposition

Perovskite-based materials can be widely used in the aerospace and transportation field. Perovskite manganese oxides La_0.7Sr_0.3MnO₃ (LSMO) thin films were grown on LaAlO₃ (100) and Si (100) single crystal substrates by the polymer-assisted chemical solution deposition (PACSD) method. Electronic transport behavior, microstructure, and magnetoresistance (MR) of LSMO thin films on different substrates were investigated. The resistance of LSMO films fabricated on LaAlO₃ substrates is smaller than that on the Si substrates. The magnetic field reduces resistance of LSMO films both on Si and LAO in the wide temperature region, when the insulator-metal transition temperature shifts to higher temperature. The low-field magnetoresistance of LSMO films on Si in low temperature range at 1 T is larger than that of LSMO films on LAO. However, the MR of LSMO film on LAO films at room-temperature is about 5.17 %. The thin films are smooth and dense with uniform nanocrystal size grain. These results demonstrate that PACSD is an effective technique for producing high quality LSMO films, which is significant to improve the magnetic properties and the application of automotive sensor.

     

Fabrication and its characteristics of low-temperature polycrystalline silicon thin films

In order to reduce the cost of solar cells or flat-panel display, it is very important to synthesis poly-crystalline silicon films on low cost substrate such as glass at low temperature. In this work, electron cyclotron resonance (ECR) plasma enhanced chemical vapor deposition (PECVD) system was successfully applied to synthesize poly-Si thin-film on common glass substrate using H2 as the plasma source and SiH4 (Ar:SiH4=19:1) as the precursor gas at low temperature. Since the multicusp cav- ity-coupling ECR plasma source was adopted to provide active precursors, the growth temperature decreased to lower than 200℃. In the plasma, the electron temperatures kTe are ~2―3 eV and the ion temperatures kTi≤1 eV. This leads to non-remarkable ion impacts during the film deposition. The characteristic of poly-Si films was investigated. It was shown that the crystalline fraction Xc of the films can be up to 90% even deposit at room temperature, and the film was (220) preferably oriented. The growth behaviors of the film between the interface of glass and Si films were also discussed in detail.     

脉冲激光沉积(PLD)原理及其应用

脉冲激光沉积薄膜是近年来发展起来的使用范围最广,最有希望的制膜技术.通过从激光与材料相互作用理论出发,分析了激光烧蚀材料等离子体羽辉的空间运动特征与成分分布,以LCMO为对象,对PLD系统脉冲激光沉积薄膜过程中薄膜质量与衬底温度、靶材-衬底距离、氧压、激光脉冲能量、激光频率等参数关系进行了实验研究,得出在单晶衬底上沉积LCMO薄膜的最佳实验参数.同时用XRD衍射谱和SEM分别对膜的成键情况和表面形貌作了分析,结果表明脉冲激光沉积(PLD)是一种很好的镀膜方法,所制备的膜质量较好.     

Fabrication and properties of Ag/Mg<Subscript>0.2</Subscript>Zn<Subscript>0.80</Subscript>/La<Subscript>0.67</Subscript>Ca<Subscript>0.33</Subscript>MnO/p<Superscript>+</Superscript>-Si resistive switching heterostructure devices

Mg_0.2Zn_0.8O (MZO)/La_0.67Ca_0.33MnO (LCMO) heterostructure was deposited on p⁺-Si substrates by sol-gel spin coating technique. The Ag/MZO/LCMO/p⁺-Si devices exhibit a bipolar, reversible, and remarkable current-voltage characteristic at room temperature. An obvious multilevel resistive switching effect is observed in the devices. The dominant conduction mechanism of the devices is trap-controlled space charge limited current. The resistance ratio of high resistance state and low resistance state of the devices is about six orders of magnitude, and the degradation is invisible in the devices after 250 successive switching cycles. The present results suggest that the Ag/MZO/LCMO/p⁺-Si devices may be a potential and multilevel candidate for nonvolatile memory application.     

Crystallization and Electrical Properties of （Ba0.4Pb0.3）Sr0.3TiO3 Thin Film by Pulsed Laser Deposition

（Ba0.4Pb0.3）Sr0.3TiO3 thin films were fabricated via pulsed laser deposition （PLD） technique on Pt/TiO2/SiO2/Si substrate. The crystallization of the films was characterized by XRD and FSEM, and the experimental results suggested deposition parameters, especially the deposition temperature was the key factor in forming the perovskite structure. The dielectric properties of the film deposited with optimized parameters were studied by an Agilent 4294A impedance analyzer at 1 MHz. The dielectric constant was 772, and the loss tangent was 0.006. In addition, the well-shaped hysteresis loop also showed that the film had a well performance in ferroelectric. The saturated polarization P, remnant polarization Pr and coercive field E were about 4.6 μC/cm2, 2.5 μC/cm2 and 23 kV/cm （the coercive voltage is 0.7 V）, respectively. It is suggested the film should be a promising candidate for microwave applications and nonvolatile ferroelectric random access memories （NvFeRAMs）.     

A direct atomic layer deposition method for growth of ultra-thin lubricant tungsten disulfide films

We describe a direct atomic layer deposition method to grow lubricant tungsten disulfide (WS₂) films. The WS₂ films were deposited on a Si (100) substrate and a zinc sulfide (ZnS) film coated the Si (100) substrate using tungsten hexacarbonyl and hydrogen sulfide as precursors. The ZnS film served as an intermediate layer to facilitate the nucleation and growth of the WS₂ films. The thickness of the WS₂ films was measured via scanning electron microscope, the microstructure was probed with an X-ray diffractometer and a transmission electron microscope. The friction coefficient was measured with a ball-on-disk tester under dry nitrogen. The results reveal that the WS₂ films deposited on both substrates are ~175 nm and have (002) and (101) crystal orientations. The WS₂ film deposited on the ZnS coated Si substrate exhibits a stronger (002) orientation and a denser crystal structure than that deposited on the Si substrate. The WS₂ films on both substrates have low friction coefficients. However, due to the stronger (002) orientation and denser crystal structure, the friction coefficient of the WS₂ film deposited on ZnS coated Si substrate is smaller with longer wear life.     

Synthesis of aligned carbon nanotubes by thermal chemical vapor deposition

Single crystal silicon was found to be very beneficial to the growth of aligned carbon nanotubes by chemical vapor deposition with C₂H₂ as carbon source. A thin film of Ni served as catalyst was deposited on the Si substrate by the K575X Peltier Cooled High Resolution Sputter Coater before growth. The growth properties of carbon nanotubes were studied as a function of the Ni catalyst layer thickness. The diameter, growth rate and areal density of the carbon nanotubes were controlled by the initial thickness of the catalyst layer. Steric hindrance between nanotubes forces them to grow in well-aligned manner at an initial stage of growth. Transmission electron microscope analysis revealed that nanotubes grew by a tip growth mechanism. Funded by the National Natural Science Foundation of China (No. 50435030)     

Preparation and characterization of SrTiO<Subscript>3</Subscript> thin film on functional organic self-assembled monolayers

SrTiO₃ thin film was successfully prepared on the functionalized organic self-assembled monolayers (SAMs) by the Liquid Phase Deposition (LPD) method. The as-prepared samples were characterized by X-ray diffraction (XRD), atomic force microscope (AFM), scanning electron microscopy (SEM) and metallographic microscope. Measurement of contact angle showed that the hydrophobe substrate was changed into hydrophile by UV irradiation. AFM photographs of octadecyl-trichloro-silane self-assembled monolayer (OTS-SAM) surface approved that UV irradiation did change the morphology of OTS monolayer and provided evidence for the conversion of hydrophilic characteristic. Photographs of Metallographic Microscope showed that OTS-SAM had an active effect on the deposition of SrTiO₃ thin film. XRD and SEM indicated that the thin film was of pure cubic phase SrTiO₃ and composed of nanosized grains with a size in the range of 100–500 nm. The formation mechanism of the SrTiO₃ film was proposed.     

Effect of acetic acid on electrochemical deposition of carbon-nitride thin film

Electrochemical deposition method was employed to prepare CNx thin film from methanol-urea solution,and it was shown that adding a little acetic acid in the solution significantly affected the deposition process.After optimizing the experiment conditions,we obtained polycrystalline grains with sizes of about 3―7μm on the faces of single crystal silicon.X-ray diffraction spectrua indicate that the grains are mainly composed of cubic phase mixed with a small amount of β and α phases.     

Second-harmonic generation in UV-pulsed laser poled amorphous 80GeS2-15Ga2S3-5CdS chalcogenide film

With the pulsed laser deposition （PLD） method, amorphous 80GeS2-15Ga2S3-5CdS chalcogenide film was deposited on glassy substrate. Obvious second harmonic generation （SHG） was observed in the ultraviolet （UV）-polarized film and the SHG intensity increased with the increase in single pulse energy and irradiation time. Through Raman spectra and transmission spectra, the mechanism of SHG was studied. The experimental results demonstrated that effective electron traps and hole traps were generated in the UV- polarized film. The energy of electrons and holes was using up due to the collision with other particles and crystal fields during their movement and finally they were captured by the traps and fixed, which made the electric charge distribution nonuniform in the film and destroyed the spatial isotropy. In the meantime, the center of positive and negative charges separated and a built-in electric field was formed which generated the optical second-order nonlinearity of the film.     

The electronic structure and grain boundary segregation by boron addition

The electronic structure and grain boundary segregation caused by boron addition to Ni₃Al have been studied by X-ray photoelectron spectroscopy and Auger electron spectroscopy, respectively. The obtained results show that the Ni2p_3/2 electron binding energy rises gradually in the sequence of pure Ni<Ni₇₆Al₂₄<Ni₇₄Al₂₆<Ni₇₅Al₂₅, while it reduces monotonously with an increase in boron addition to Ni₃Al. Besides, it is found that the grain boundary segregation of boron occurring in Ni₃Al is a combined equilibrium and non-equilibrium type in nature. Based on the concept of the bonding environmental inhomogeneity, measured by the shift in Ni2p_3/2 electron binding energy from the nickel atoms in the simple substance nickel to those in the intermetallic compound Ni₃Al (ΔE _B), being responsible for the brittle behavior of the alloy, a binding energy shifting criterion for the brittle-ductile fracture transition in Ni₃Al is presented; when ΔE _B>0, the brittle failure occurs in Ni₃Al; when δE _B<0, the ductile one appears. Combined with the above experimental rules, the criterion predicts that pure Ni₃Al is brittle, and there exist the stoichiometric effect and concentration effect in the ductilization process for Ni₃Al by boron addition. Hence the criterion can be taken as a theoretical guide to alloy design in developing ductile intermetallics. Project supported by the National Natural Science Foundation of China.     

玻璃衬底沉积氮化硅薄膜性能研究

为了改善玻璃衬底上制备的薄膜太阳电池的转换效率,采用高纯氮气作为等离子体气源,以质量分数为5%的SiH_4(Ar稀释)作为前驱气源,利用电子回旋共振-等离子体增强化学气相沉积技术在玻璃衬底上低温制备了氮化硅薄膜;利用各种测试设备分析了薄膜的成分、光学性能和表面形貌.结果表明:实验制备的非晶薄膜含氢量较低;薄膜的折射率随着衬底温度和微波功率的增加而增加.在衬底温度为350℃、微波功率为650 W时,薄膜的折射率在2.0左右,平均粗糙度为1.45 nm,还说明薄膜具有良好的光学性能和较高的表面质量.在此条件下,薄膜的沉积速率达到10.7 nm/min,表明本实验能在较高的沉积速率下制备均匀、平整、优质的SiN薄膜.     

La0.7Ca0.3MnO3多晶材料制备及其电磁特性

以化学溶液分解法制备La0.7Ca0.3MnO3粉体,常压烧结制备多晶块体样品。对La0.7Ca0.3MnO3样品的磁矩、磁致电阻效应（CMR）和电脉冲诱导电阻转变效应（EPIR）进行了研究。磁矩零场冷和场冷试验结果发现,居里温度以下,零场冷和场冷条件下磁矩具有较大差别。这说明材料中缺少真正的长程磁有序。La0.7Ca0.3MnO3多晶具有磁致电阻效应,在9 T磁场作用下,磁致电阻变化大约为70%。在80 V,20 ns电脉冲作用下,材料具有电脉冲诱导电阻转变效应。从理论上对磁致电阻效应与电脉冲诱导电阻转变效应的机理进行了分析。     

Optical, mechanical and laser-induced damage threshold properties of 1 064 nm, 532 nm frequency-doubled antireflection coating for LBO

1 064 nm, 532 nm frequency-doubled antireflection (AR) coatings with buffer layer of SiO2 between the coating and the substrate were fabricated by the electron beam evaporation technology on the substrate of lithium triborate (LiB3O5 or LBO) crystals. The residual reflectance of the sample is 0.07% and 0.11% at 1 064 nm and 532 nm, respectively. The adhesion and the laser-induced damage threshold (LIDT) of the sample are greater than 200 mN and 18.6 J/cm2. The strengthening mechanism of adhesion and LIDT of the buffer layer of SiO2 were discussed by considering full plastic indentation and shear theory, and spallation of a plated film induced by thermal shock stress, respectively.     

Magnetic Properties of NiCuZn Ferrite Thin Films Prepared by the Sol-gel Method

Ni0.4Cu0.2Zn0.4Fe2O4 thin films were fabricated on Si substrates by using the sol-gel method and rapid thermal annealing （RTA）, and their magnetic properties and crystalline structures were investigated. The samples calcined at and above 600 ℃ have a single-phase spinel structure and the average grain size of the sample calcined at 600 ℃ is about 20 nm. The initial permeability μi, saturation magnetization M and coercivity H of the samples increase with the increasing calcination temperature. The sample calcined at 600 ℃ exhibits an excellent soft magnetic performance, which has μi=33.97 （10 MHz）, Hc=15.62 Oe and Ms=228.877 emu/cm^3. Low-temperature annealing can enhance the magnetic properties of the samples. The work shows that using the sol-gel method in conjunction with RTA is a promising way to fabricate integrated thin-film devices.     

Preparation and Properties of IrO2 Thin Films Grown by Pulsed Laser Deposition Technique

Highly conductive IrO2 thin films were prepared on Si （100） substrates by means of pulsed laser deposition technique from an iridium metal target in an oxygen ambient atmosphere. Emphasis was put on the effect of oxygen pressure and substrate temperature on the structure, morphology and resistivity of IrO2 films. It was found that the above properties were strongly dependent on the oxygen pressure and substrate temperature. At 20 Pa oxygen ambient pressure, pure polycrystalline IrO2 thin films were obtained at substrate temperature in the 300-500℃ range with the preferential growth orientation of IrO2 films changed with the substrate temperature. IrO2 films exhibited a uniform and densely packed granular morphology with an average feature size increasing with the substrate temperature. The room-temperature resistivity variations of IrO2 films correlated well with the corresponding film morphology changes. IrO2 films with the minimum resistivity of （42 ±6）μΩ·cm was obtained at 500℃.     

离子束辅助沉积非晶硅薄膜红外光学特性研究

为了得到非晶硅（a-Si）薄膜红外光学常数与工艺参数之间的关系,采用Ar离子束辅助电子束热蒸发技术制备a-Si薄膜,并利用椭偏仪和分光光度计测量了薄膜的光学常数,分析了薄膜沉积速率、基底温度和工作真空度对a-Si薄膜折射率和消光系数的影响.实验结果表明：影响a-Si薄膜光学常数的主要工艺因素是沉积速率和基底温度,工作真空度的影响最小.当沉积速率和基底温度升高时,薄膜的折射率先增大后减小;当工作真空度升高时,薄膜的折射率增大.在波长1~5μm之间,a-Si薄膜的折射率变化范围为2.47~3.28.     

Chemical vapor deposition of SiC at different molar ratios of hydrogen to methyltrichlorosilane

Chemical vapor deposition (CVD) of SiC from methyltrichlorosilane (MTS) was studied at two different molar ratios of H₂ to MTS (n(H₂)/n(MTS)). The total pressure was kept as 100 kPa and the temperature was varied from 850 to 1 100 °C at a total residence time of 1 s. Steady-state deposition rates as functions of reactor length and of temperature, investigated at different n(H₂)/n(MTS) values, show that hydrogen exhibits strongly influences on the deposition rate. Especially, the deposition of Si co-deposit can be obtained in broader substrate length and at higher temperatures with increasing hydrogen partial pressure. Influence of hydrogen on the deposition process was also studied using gas phase composition and deposit composition analysis at various n(H₂)/n(MTS). SEM micrographs directly show the variation of surface morphologies at various n(H₂)/n(MTS). It can be found that the crystal grain of the deposit at 1 100 °C is better developed and the crystallization is also improved with increasing n(H₂)/n(MTS).     

Orientation of Bi<Subscript>3.2</Subscript>La<Subscript>0.8</Subscript>Ti<Subscript>3</Subscript>O<Subscript>12</Subscript> ferroelectric thin films with different annealing schedules

Fatigue-free Bi_3.2La_0.8Ti₃O₁₂ ferroelectric thin films were successfully prepared on p-Si (100) substrates using metalorganic solution deposition process. The orientation and formation of 5-layers thin films were studied under different processing conditions using XRD. Experimental results indicate that increase in annealing time at 700 °C after preannealing for 10 min at 400 °C can remarkably increase (200)-orientation of the films derived from the precursor solutions with two contents of citric acid. Meanwhile, high content of citric acid increases the film thickness and is conducive to the a-orientation of the films with the preannealing, and low concentration of the solution is conducive to the c-orientation of the films without the preannealing.     

Stable biomimetic film on Fe3Al surface for corrosion resistance in seawater

Stable superhydrophobic n-tetradecanoic acid (CH₃(CH₂)₁₄COOH) film was prepared by means of sol-gel and self-assembly techniques, with a very high seawater contact angle (158°) and a small sliding angle (<5°). There are many microconvexities with binary structure uniformly distributed on the surface atop the film with an average diameter of about 80 nm by observation of scanning electron microscope (SEM), and the film surface structure is similar to that of lotus surface. The corrosion resistance behavior of intermetallic Fe₃Al with the biomimetic superhydrophobic film surface is improved obviously when compared with pure Fe₃Al sample by measurement of electrochemical impedance spectroscopy (EIS). Supported by the Excellent Mid-youthful Scientist Encouraging Foundation of Shandong Province (Grant No. 2006BS04021) and the National Natural Science Foundation of China (Grant Nos. 50672090 and 50702053)