样品厚度对薄膜法X射线荧光光谱测量的影响研究

分别以富集有Cr,Pb和Cd三种元素的尼龙薄膜样品及玻璃纤维滤膜为研究对象,采用滤膜叠加的方式,通过XRF光谱仪测量不同样品厚度下薄膜样品的XRF光谱,根据测得的尼龙薄膜样品中Cr,Pb,Cd元素及玻璃纤维滤膜中Ca,As和Sr元素特征XRF性质的变化,研究样品厚度对薄膜法XRF光谱测量的影响。结果表明：薄膜样品厚度对不同能量区间上元素特征谱线荧光性质的影响并不相同。元素特征谱线能量越大,元素特征X射线荧光穿透滤膜到达探测器的过程中损失越少;但由薄膜样品厚度增加引起的基体效应却越强,相应特征谱线位置处的背景荧光强度就越大,因此样品厚度增加所引起的基体效应对薄膜法XRF光谱测量的灵敏度影响就越大。对于特征谱线能量较低(能量小于7 keV)的元素,以增加薄膜样品厚度的方式来增加待测组分的质量厚度浓度,并不能有效地提高薄膜法XRF光谱测量的灵敏度;对于特征谱线能量较高的元素(能量＞7 keV),可以通过适当增加样品厚度以增加被测组分的质量厚度浓度的方式来提高XRF光谱测量的灵敏度,薄膜样品厚度在0.96～2.24 mm内,更有利于XRF光谱的测量与分析。该研究为大气及水体重金属薄膜法XRF光谱分析中薄样制备及富集技术提供了重要的理论依据。     

基于反射和透射光谱的氢化非晶硅薄膜厚度及光学常量计算

采用紫外-可见透射光谱仪测量了对靶磁控溅射沉积法制备的氢化非晶硅（a-Si:H）薄膜的透射光谱和反射光谱.利用T/(1-R)方法来确定薄膜的吸收系数,进而得到薄膜的消光系数|通过拟合薄膜透射光谱干涉极大值和极小值的包络线来确定薄膜折射率和厚度的初始值,并利用干涉极值公式进一步优化薄膜的厚度值和折射率|利用柯西公式对得到的薄膜折射率进行拟合,给出了a-Si:H薄膜的色散关系曲线.为了验证该方法确定的薄膜厚度和光学常量的可靠性,将理论计算得到的透射光谱与实验数据进行了比较,结果显示两条曲线基本重合,可见这是确定a-Si:H薄膜厚度及光学常量的一种有效方法.     

Synthesis and conductive properties of nanoisland Sn,Al, and Cu films

Nanoisland Sn, Al, and Cu films were synthesized on dielectric substrates and their morphology and conductive properties were investigated. It is shown that the initial effective film thickness significantly affects the morphological parameters of nanoislands. Study of the surface conductivity of the films at the condensation stage revealed the conductivity drop after termination of the deposition, which is related to the nanostructuring processes. It was found that the temperature dependences of the film conductivity include three portions: the low-temperature portion of the activation growth, the decrease upon nanostructuring, and the high-temperature portion of the activation growth.     

Multi-objective optimization of laser-scribed micro grooves on AZO conductive thin film using Data Envelopment Analysis

Laser scribing process has been considered as an effective approach for surface texturization on thin film solar cell. In this study, a systematic method for optimizing multi-objective process parameters of fiber laser system was proposed to achieve excellent quality characteristics, such as the minimum scribing line width, the flattest trough bottom, and the least processing edge surface bumps for increasing incident light absorption of thin film solar cell. First, the Taguchi method (TM) obtained useful statistical information through the orthogonal array with relatively fewer experiments. However, TM is only appropriate to optimize single-objective problems and has to rely on engineering judgment for solving multi-objective problems that can cause uncertainty to some degree. The back-propagation neural network (BPNN) and data envelopment analysis (DEA) were utilized to estimate the incomplete data and derive the optimal process parameters of laser scribing system. In addition, analysis of variance (ANOVA) method was also applied to identify the significant factors which have the greatest effects on the quality of scribing process; in other words, by putting more emphasis on these controllable and profound factors, the quality characteristics of the scribed thin film could be effectively enhanced. The experiments were carried out on ZnO:Al (AZO) transparent conductive thin film with a thickness of 500 nm and the results proved that the proposed approach yields better anticipated improvements than that of the TM which is only superior in improving one quality while sacrificing the other qualities. The results of confirmation experiments have showed the reliability of the proposed method.     

Simulating percolating behavior of conductive particles in anisotropically conductive composite films

A numerical scheme is developed to simulate the percolating behavior of conductive particles within a non-conductive matrix film with a preferential alignment of particles achieved via externally imposed deterministic driving forces. The sharp transition from non-conducting to conducting of the composite film is successfully revealed with the model. The percolation behavior is studied in terms of four percolation parameters, including the percolation probability, the normalized shortest percolation path, normalized gyration radius and density of the percolation cluster, subject to variation in five important system parameters. These include particle concentration, relative importance of the externally applied force, film thickness, film width and particle size. The threshold particle concentration can be reduced by increasing the strength of the deterministic driving force, decreasing film thickness, increasing film width or using smaller size particles. Our study suggests that using stronger applied force for wider and thinner films containing smaller particles may be a good practice to obtain anisotropically conductive films with a light particle loading that possess good conduction capability in the thickness direction and good insulation in the planar direction. Received: 19 February 2001 / Accepted: 30 May 2001 / Published online: 30 August 2001     

Sputtered deposited nanocrystalline ZnO films: A correlation between electrical, optical and microstructural properties

Zinc oxide thin films were prepared by dc (direct current) and rf (radio frequency) magnetron sputtering on glass substrates. ZnO films produced by dc sputtering have a high resistance, while the films produced using rf sputtering are significantly more conductive. While the conductive films have a compact nodular surface morphology, the resistive films have a relatively porous surface with columnar structures in cross section. Compared to the dc sputtered films, rf sputtered films have a microstructure with smaller d spacing, lower internal stress, higher band gap energy and higher density. Dependence of conductivity on the deposition technique and the resulting d spacing , stress, density, band gap, film thickness and Al doping are discussed. Correlations between the electrical conductivity, microstructural parameters and optical properties of the films have been made. PACS 73.25.+i; 81.15.cd; 81.05.ys     

薄膜厚度对GZO透明导电膜及其LED器件性能的影响

采用射频磁控溅射的方法制备了GZO透明导电薄膜,通过原子力显微镜(AFM)、X射线衍射仪(XRD)、霍尔效应测试仪及紫外-可见光分光光度计等手段研究了厚度对于GZO薄膜性能的影响,并制备了相应的LED器件。实验结果表明:随着薄膜厚度增加,薄膜结晶质量提高,薄膜的电阻率也随之降低。当厚度为500 nm时,薄膜的电阻率最低为2.79×10^-4 Ω·cm,同时其在460 nm蓝光区域的光透过率高达97.9%。对所制备的以GZO薄膜为透明电极的LED器件进行了测试分析,发现GZO薄膜厚度对LED的正向电压影响不大,但对LED芯片的出光效率有较大影响。     

基于FTO/VO2/FTO结构的VO2薄膜电压诱导相变光调制特性

采用直流磁控溅射和后退火工艺在掺氟的SnO₂(FTO)导电玻璃衬底上制备VO₂薄膜, 研究了不同退火时间和不同比例的氮氧气氛对VO₂薄膜性能的影响, 对VO₂薄膜的结晶取向、表面形貌、表面元素的相对含量和透过率随波长变化进行了测试分析, 结果表明在最佳工艺条件下制备得到了组分相对单一的VO₂薄膜. 基于FTO/VO₂/FTO结构在VO₂薄膜两侧的透明导电膜上施加电压并达到阈值电压时, 观察到了明显的电流突变. 当接触面积为3 mm×3 mm时, 阈值电压为1.7 V, 阈值电压随接触面积的增大而增大. 与不加电压的情况相比, FTO/VO₂/FTO结构在电压作用下高低温的红外透过率差值可达28%, 经反复施加电压, 该结构仍保持性能稳定, 具有较强的电致调控能力.     

用于高速摄影变象管的软X射线光电阴极

光阴极由衬底(包括介质阴极的导电基底)和光电发射膜构成。采用了聚丙烯、Formvar和Paylene三种有机薄膜作阴极衬底。建立了这些薄膜的制备技术。用一台自制的软X射线单色仪在277—7469ev光子能量范围内测量了这些薄膜的透过率。 研究了CsI、CsBr、Au和MgF₂四种光电阴极的光电发射特性和光电发射与阴极厚度的关系,找出了最佳阴极厚度。用软X射线单色仪在277—7469ev光子能量范围内测量了最佳厚度阴极的绝对量子效率,四种阴极最大值分别为4.50、2.90、0.25和0.12。我们还在同一阴极衬底上分区制备了四种阴极,在变象管荧光屏上比较其亮度,结果和测量的一致。 用LAB5型表面分析仪对CsI和Au阴极的光电子初能量分布作了测量,CsI阴极光电子初能量分布半高宽远小于Au。因此CsI是适用于高速摄影变象管比较理想的软X射线光电阴极。     

Laser direct imaging of transparent indium tin oxide electrodes using high speed stitching techniques

To accomplish an electrode patterning in large area, we present a high speed stitching technique used in an ultraviolet laser processing system and investigate the interaction between laser beams and indium tin oxide (ITO) thin films deposited on glass substrates. After optimizing the process parameters of the laser direct imaging (LDI) for the large-area electrode patterning, the ablated lines looked like regularly fish-scale marks of about a 40 μm diameter and a 120 nm depth around the processing path. The parameters includes the laser power of 1W, the scanning speed of galvanometers of 800 mm/s, and the laser pulse repetition frequency of 50 kHz. Moreover, the resistance value of the ablated ITO thin film is larger than 200MΩ that is electrically insulated from the other regions of electrode structure. LDI technology with UV laser beam has great potential applications in patterning on wafer or sapphire substrates and patterning a conductive layer deposited on the touch panels for semiconductor and optoelectric industries, respectively.     

Optodynamic analysis of direct laser writing of graduation lines

The direct laser writing of graduation lines in Cr thin films on glass substrates has been investigated. The Nd-YAG laser and the astigmatic optical system have been used to write rectangular holes in the Cr film. The optimal writing parameters: the laser pulse energy, the Cr layer thickness and the substrate-objective distance were determined using the optoacoustic probe beam deflection method to detect the evaporation of the material. The evaporation is concluded to be the essential process in the laser writing of graduation lines. The rims formed by the surface tension gradient at the hole edges indicate that the laser writing of graduation lines is a typical two-phase removal process.     

利用透射光谱与X射线反射谱精确测量溶胶-凝胶TiO2薄膜厚度和光学常数

在洁净K9玻璃基底上沉积TiO2薄膜,将透射光谱和X射线反射光谱相结合分析获得膜层的厚度和光学常数。X射线反射谱拟合能精确得到膜层的厚度、电子密度及表面和界面粗糙度,其中膜层厚度的数值为透射光谱的分析提供了重要参考。基于Forouhi-Bloomer色散模型拟合膜层透射光谱,得到薄膜折射率和消光系数,理论曲线和实验曲线吻合良好。对于同一样品,两种光谱拟合分析得到的厚度数值非常接近,差值最大为4.9nm,说明两种方法的结合能够提高光学分析结果的可靠性。     

Elaboration of (1 1 1)-oriented La-doped PZT thin films on platinized silicon substrates

PLZT thin films with different thickness were deposited in situ on platinum coated silicon substrates using a multi-target sputtering system. The purpose was to grow (1 1 1)-textured PLZT films on Pt (1 1 1). To this aim, the role of some key parameters on both crystalline quality and electrical properties was investigated. An ultra-thin TiO₂ seeding layer was deposited, prior to PLZT, which strongly affected the crystallographic orientation of the films. The relation between temperature deposition and film crystallinity is analysed. TEM observations show the presence of some very small grains of Zr_0.9La_0.1O_1.95 at the film bottom interface. In the range of thickness investigated, the plot of the inverse capacitance as a function of the film thickness split up into two different curves, each with a linear shape, which however allows determination of a single value of interface capacitance. Above a thickness of 400-500 nm a saturation of the dielectric properties seems to be reached.     

Optical parameters in SnO2 nanocrystalline textured films grown on p-InSb (111) substrates

Spectroscopic ellipsometry and photoluminescence (PL) measurements on SnO₂ nanocrystalline textured films grown on p-InSb (111) substrates by using radio-frequency magnetron sputtering at low temperature were carried out to investigate the dependence of the optical parameters on the SnO₂ thin film thickness. As the SnO₂ film thickness increases, while the energy gap of the SnO₂ film decreases, its refractive index increases. The PL spectra show that the broad peaks corresponding to the donor-acceptor pair transitions are dominant and that the peak positions change with the SnO₂ film thickness. These results can help improve understanding for the application of SnO₂ nanocrystalline thin films grown on p-InSb (111) substrates in potential optoelectronic devices based on InSb substrates.     

Laser welding of glasses using a nanosecond pulsed Nd:YAG laser

This work reports on laser welding of two 1 mm thickness borosilicate glasses through the irradiation with a nanosecond pulsed laser, as a novel alternative to the use of ultrashort pulsed lasers for welding of transparent materials. Two different methodologies were investigated and compared in terms of interface quality. In a first approach, the glasses were joined without any absorbing intermediate layer. However, the bond interface possesses defects. To improve the resulting bond interface, the use of a titanium ultrathin intermediate layer was proposed to weld the glasses substrates, acting as a sealant between them. The laser parameters were optimized to achieve the best joining conditions of the Ti film. The use of the Ti layer gives rise to a bond interface more homogeneous and free of damages. As a further step, thin glasses of 86 µm thickness, of great technological value, were joined through the Ti film as well. The joined interfaces were inspected through optical microscopy and scanning electron microscopy (SEM) while the bond quality was evaluated by Scanning Acoustic Microscopy (SAM).     

Microstructure and roughness improvement of polycrystalline Bi thin films upon pulsed-laser melting

Bismuth films with different thicknesses have been grown by do sputtering on substrates held at room temperature. The films are always formed by columnar crystals with a grain size comparable to the film thickness which lead to surface roughness. It increases with the thickness of the films and has a strong influence on the film optical properties. The films have been irradiated with nanosecond laser pulses, and real-time reflectivity measurements during the irradiation were used to follow the changes in the film optical properties. It will be shown that pulsed-laser irradiation of films thinner than 100 nm improves substantially their surface roughness and their crystalline quality by increasing the grain size at least one order of magnitude.     

Fractional-dimensional approach for excitons in GaAsfilms on AlxGa1-xAs substrates

Binding energies of excitons in GaAs films on Al_xGa_1-xAs substrates are studied theoretically with the fractional-dimensional approach. In this approach, the real anisotropic “exciton+film” semiconductor system is mapped into an effective fractional-dimensional isotropic space. For different aluminum concentrations and substrate thicknesses, the exciton binding energies are obtained as a function of the film thickness. The numerical results show that, for different aluminum concentrations and substrate thicknesses, the exciton binding energies in GaAs films on Al_xGa_1-xAs substrates all exhibit their maxima with increasing film thickness. It is also shown that the binding energies of heavy-hole and light-hole excitons both have their maxima with increasing film thickness.     

Au层退火温度对ZnO/Au/ZnO多层膜的结构、光学及电学性质的影响

采用金属有机化学气相沉积(MOCVD)技术在蓝宝石衬底上制备出晶体质量较好的透明导电的ZnO/Au/ZnO(ZAZ)多层膜,其中,Au夹层是通过射频磁控溅射的方法获得。通过对Au夹层进行不同温度的退火处理,研究了Au层退火温度对ZAZ多层膜的结构特性、电学性能和光学特性的影响。利用原子力显微镜(AFM)、扫描电子显微镜(SEM)、X射线衍射(XRD)仪、霍尔效应测试和透射谱分析等测试手段对ZAZ多层膜的性质进行了分析。测试结果表明,在200 ℃下对Au夹层进行快速退火处理,多层膜的结构、电学和光学性质达到最优,表面等离子体效应也更明显。其中,XRD(002)衍射峰的半高宽为0.14°,电阻率为2.7×10^-3 Ω·cm,载流子浓度为1.07×10²⁰ cm^-3,可见光区平均透过率为75.3%。     

Low-frequency Raman spectra of paradichlorobenzene thin films

The low-frequency Raman spectra of paradichlorobenzene nanofilms with a thickness of about 30 μm, 1 μm, and 400 nm are experimentally measured. With decreasing film thickness, the spectral lines shift to lower frequencies and broaden and some additional lines appear, the intensity of which increases with decreasing film thickness. The film structure is modeled using the method of molecular dynamics, and the histograms of lattice vibration spectra are calculated by the Dean method. It is found that a decrease in the film thickness leads to an increase in the lattice parameters and to a higher orientational disorder both inside the film and, especially, at the film surface. The film structure is similar to the structure of the α-paradichlorobenzene single crystal. To correctly interpret the spectra of lattice vibrations, it is necessary to take into account surface vibrations and existence of vacancies in the structure.     

Surface structure and composition of flat titanium thin films as a function of film thickness and evaporation rate

To correlate flat titanium film surface properties with deposition parameters, titanium flat thin films were systematically deposited on glass substrates with various thicknesses and evaporation rates by electron-beam evaporation. The chemical compositions, crystal structure, surface topographies as well as wettability were investigated by using X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), atomic force microscopy (AFM) and water contact angle measurement, respectively. The films consisted mainly of TiO₂. Small percentages of Ti₂O₃ and metallic Ti were also found at the film surface using high-resolution XPS analysis. Quantitative XPS showed little differences regarding elemental compositions among different groups of films. The films were obtained by varying the deposition rate and the film thickness, respectively. XRD data showed consistent reflection patterns of the different titanium samples deposited using different film thicknesses. Without exception measurements of all samples exhibited contact angles of 80° ± 5°. Quantitative AFM characterization demonstrated good correlation tendency between surface roughness and film thickness or evaporation rate, respectively. It is important to notice that titanium films with different sizes of grains on their surfaces but having the same chemistry and film bulk structure can be obtained in a controllable way. By increasing the film thickness and evaporation rate, the surface roughness increased. The surface morphology and grain size growth displayed a corresponding trend. Therefore, the control of these parameters allows us to prepare titanium films with desired surface properties in a controllable and reproducible way for further biological investigations of these materials.