Simple Method for Determining Slowly Varying Refractive-Index Profiles from in situ Spectrophotometric Measurements

Reliable control of the deposition process of optical films and coatings frequently requires monitoring the refractive-index profile throughout the layer. In the present research a simple in situ approach is proposed that uses a WKBJ matrix representation of the optical transfer function of a single thin film on a substrate. Mathematical expressions are developed that represent the minima and the maxima envelopes of the curves transmittance versus time and reflectance versus time. The refractive index and the extinction coefficient depth profiles of different films are calculated from simulated spectra as well as from experimental data obtained during the PECVD (plasma-enhanced chemical vapor deposition) of silicon-compound films. Variation in the deposition rate with time is also evaluated from the position of the spectra extrema as a function of time. The physical and mathematical limitations of the method are discussed.     

Optical monitoring of etching in inorganic resists

An as-deposited As₂S₃ thin film is demonstrated as a negative working inorganic resist suitable for silicon microstructure fabrication. An in situ optical technique for monitoring the etching process in inorganic resists is described for pattern delineation. The etching control in dielectric films is treated as a special case.     

Laser reflectometry in situ measurement of lead zirconate titanate film growth

A convenient method is described for optical characterization of thin films during growth. The method has been demonstrated on lead zirconate titanate (PZT) films deposited by pulsed laser ablation for various temperatures. The optical constants of the PZT films as well as the film growth rate were determined in situ by fitting (with three free parameters) the calculated reflectance as a function of film thickness to the experimental reflectance curve as a function of deposition time, as obtained by unpolarized laser reflectometry. The fitted parameters are the uniform complex PZT refractive index and the layer thickness (assumed proportional to time), with the complex refractive index of the platinum substrate being measured previously. These results compare well with the subsequent ellipsometric measurements made to assess the precision of the reflectometry technique.     

Oxygen-ion-assisted deposition of thin gold films

Thin gold films have been deposited on glass and silicon substrates using ion-assisted deposition techniques. The adhesion of the films to the substrates is assessed by a scratch test. Deposition assisted by 100 eV-1 keV oxygen ions yields highly adhesive films that can only be removed by damaging the substrate. Argon and hydrogen ions produce films with relatively poor adhesion. The results show that the reflectance of oxygen-assisted films is reduced by trapping of the oxygen in the gold but no bulk chemical or structural changes are detected. It is proposed that a thin stable layer of gold oxide is formed during film growth and diffuses into the substrate, providing a strong bond for subsequent film deposition. Highly adhesive films with bulk optical properties are deposited on glass and silicon using oxygen-ion assistance only to the point of continuous film formation.     

The effect of the ion beam energy on the properties of indium tin oxide thin films prepared by ion beam assisted deposition

Indium tin oxide (ITO) thin films have been deposited onto polycarbonate substrates by ion beam assisted deposition technique at room temperature. The structural, optical and electrical properties of the films have been characterized by X-ray diffraction, atomic force microscopy, optical transmittance, ellipsometric and Hall effect measurements. The effect of the ion beam energy on the properties of the films has been studied. The optical parameters have been obtained by fitting the ellipsometric spectra. It has been found that high quality ITO film (low electrical resistivity and high optical transmittance) can be obtained at low ion beam energy. In addition, the ITO film prepared at low ion beam energy gives a high reflectance in IR region that is useful for some electromagnetic wave shielding applications.     

Structural, morphological and optical properties of thermal annealed TiO thin films

Structural, morphological and optical properties of TiO thin films grown by single source thermal evaporation method were studied. The films were annealed from 300 to 520 °C in air after evaporation. Qualitative film analysis was performed with X-ray diffraction, atomic force microscopy and optical transmittance and reflectance spectra. A correlation was established between the optical properties, surface roughness and growth morphology of the evaporated TiO thin films. The X-ray diffraction spectra indicated the presence of the TiO₂ phase for the annealing temperature above 400 °C.     

Analysis of optical absorption in silicon nanowire arrays for photovoltaic applications

This paper presents analysis of the optical absorption in silicon nanowire arrays that have potential applications in solar cells. The effects of wire diameter, length, and filling ratio on the absorptance of nanowire arrays are simulated. The study reveals that nanowire arrays with moderate filling ratio have much lower reflectance compared to thin films. In a high-frequency regime, nanowire arrays have higher absorptance than their thin film counterparts. In low-frequency regime, nanowire arrays absorb less but can be designed to approach that of the film by changing the filling ratio.     

Optical properties and crystallinity of hydrogenated nanocrystalline silicon (nc-Si:H) thin films deposited by rf-PECVD

Hydrogenated nanocrystalline silicon (nc-Si:H) thin films prepared in a home-built radio-frequency (rf) plasma enhanced chemical vapour deposition (PECVD) system have been studied. The rf powers were fixed in the range of 5 W-80 W. The optical properties and crystallinity of the films were studied by X-ray diffraction (XRD), Micro-Raman scattering spectroscopy, high resolution transmission electron microscope (HRTEM), and optical transmission and reflection spectroscopy. The XRD and Micro-Raman scattering spectra were used to investigate the evidence of crystallinity in order to determine the crystallite sizes and crystalline volume fraction in the films. The HRTEM image of the film was used to correlate with the crystallinity that was determined from XRD and Micro-Raman scattering spectra. Optical constants such as refractive index, optical energy gap, Tauc slope, Urbach energy and ionic constants were obtained from the optical transmission and reflectance spectra. From the results, it was interesting to found that the optical constants showed a good correlation with the crystallinity within the variation of rf power. Also, the ionic constants of the films showed an indication of the degree of crystallinity in the films. The variation of the optical energy gap with the rf power based on structure disorder and the quantum confinement effect is discussed.     

化学气相沉积金刚石薄膜生长的原位反射率测量

报道了化学气相沉积金刚石薄膜生长的原位反射率测量,提出了监控金刚石薄膜生长的激光反射多光束干涉的数学模型。通过原位反射率的测量,精确监控了金刚石薄膜的生长厚度,成功地制备了红外增透增,这种方法的测量装置简单、紧凑而且可靠。     

Spatial spectral evolution in pulsed laser deposited lead-germanate thin films by micro-infrared spectroscopy

Lead-germanate thin films were developed on silicon substrates by pulsed laser deposition from bulk glassy targets of composition 0.4PbO-0.6GeO₂, and micro-infrared transmittance measurements were performed to assess the state of the grown films. Measurements across the radius of films revealed surprisingly large spectral changes, reminiscent of lead-oxide variations in corresponding bulk glasses. To search for the origin of this effect, the infrared spectra were simulated by employing the rigorous expression for the transmittance of a bilayer system to take into full account multiple internal reflections in both thin film and substrate. The results showed that the profiles of the experimental spectra can be accurately described by using as input the complex refractive index of the target glassy material and by considering film thickness variations from the center to the edges of the film. This work demonstrates the strong influence of optical effects on the infrared spectra of thin films, and manifests also the effectiveness of infrared spectroscopy when coupled with rigorous calculations to characterize the structure of thin films.     

Optical and structural properties of Mg doped ZnO thin films by chemical bath deposition method

The chemical bath deposition method has often been employed to successfully deposit pure and Mg doped ZnO thin films on a glass substrate. The impact of Mg creates a strained stress in ZnO films affecting its structural and optical properties. XRD patterns revealed that all thin films possess a polycrystalline hexagonal wurtzite structure and Mg doped ZnO thin films (002) plane peak position is shifted towards a lower angle due to Mg doping. From the SEM image, it is understood that the Mg doped ZnO thin films are uniformly coated and are seen as dense rods like pillers deposited over the film. The energy dispersive X-ray analysis confirmed the presence of Mg in doped ZnO thin films. The transmittance spectra exhibit that it is possible for Mg doping to enhance ZnO thin films. The optical energy gap of the films was assessed by applying Tauc’s law and it is observed to show an increasing tendency with an improvement in Mg doping concentrations. The optical constants such as reflectance, index of refraction, extinction coefficient and optical conductivity are determined by using transmission at normal incidence of light by using wavelength range of 200–800 nm. In PL spectra, the band edge emission shifted to the blue with increasing amount of Mg doping.     

Optical properties of silicon thin films related to LPCVD growth condition

In this paper we study the changes in the microstructural and optical properties of silicon thin films produced by the variation of the parameters (temperature and pressure) of the low-pressure chemical vapour deposition (LPCVD) process. Silicon thin films prepared by LPCVD on oxidized silicon substrates over a large range of process parameters (T_dep=500-615°C, p_dep=20-100 Pa) have been characterized by Raman spectroscopy, spectroscopic ellipsometry (SE), X-ray diffraction (XRD) and atomic force microscopy (AFM) techniques. The phase transition of as-deposited silicon from an amorphous to a crystalline phase via an intermediate mixed phase (few grains in amorphous silicon matrix) can be monitored by the changes in the optical properties and in the Raman spectra. LPCVD parameters, which control the deposition kinetics, are able to influence the optical properties, the structure and/or morphology of the as-deposited LPCVD silicon films. The SE and Raman results prove that it is possible to grow by LPCVD (from pure silane), a silicon film in a (poly)crystalline state at a temperature as low as 500°C.     

A low‐cost and reliable optical inspection system for rapid surface roughness measurements of polycrystalline thin films

Excimer laser crystallization is a well‐known industrially used technique to produce high‐performance polycrystalline silicon thin films on the commercially available inexpensive glass substrates for the development of high‐performance low temperature polycrystalline silicon thin‐film transistors in active matrix flat panel displays. A rapid optical measurement system for rapid surface roughness measurement of polycrystalline silicon thin films was developed in this study. Two kinds of thicknesses of polycrystalline silicon thin films were used to study rapid surface roughness measurements. Six different incident angles were employed for measuring surface roughness of polycrystalline silicon thin films. The results reveal that the incident angle of 20° was found to be a good candidate for measuring surface roughness of polycrystalline silicon thin films. Surface roughness (y) of polycrystalline silicon thin films can be determined rapidly from the average value of reflected direct current voltage (x) measured by the optical system developed using the trend equation of y = –8.9854x + 91.496. The maximum measurement error rate of the optical measurement system developed was less than 5.72%. The savings in measurement time was up to 83%.     

Large area ZnO:Al films with tailored light scattering properties for photovoltaic applications

Aluminum-doped zinc oxide films on glass are promising substrates for use in thin film solar cells based on amorphous and amorphous/microcrystalline silicon absorber material. The films can be produced by magnetron sputtering on large scale at relative low cost. Especially reactive sputtering of metallic Zn/Al compound targets is a cheap way to produce films at high deposition rate. One drawback of amorphous silicon is the low absorption in the near infrared spectral range. Wet chemical etching has been used to produce a rough TCO surface that enables light trapping in the absorber. The etching behaviour of ZnO:Al films can be tuned by changing oxygen partial pressure during deposition. The etching behaviour is compared to ZnO structure and discussed regarding the performance of solar cells deposited onto the etched films.     

A study of silicon oxynitride film prepared by ion beam assisted deposition

A SOI-based optoelectronic device needs a high-quality antireflection coating on both faces of the device to minimize the optical reflectance from the face. In this work amorphous silicon oxynitride films were deposited on silicon substrates by ion beam assisted deposition (IBAD). The main purpose was to use silicon oxynitride film as single layer anti-reflection coating for SOI-based optoelectronic devices. This application is primarily based on the ability to tune the silicon oxynitride optical functions to the optimal values by changing deposition parameters. The chemical information was measured by X-ray photoelectron spectroscopy (XPS). Spectroscopic ellipsometry (SE) was applied to measure the refractive index and thickness. Single-side polished silicon substrate that was coated with silicon oxynitride film exhibited low reflectance. Double-side polished silicon substrate that was coated with silicon oxynitride film exhibited high transmittance. In addition, the Fresnel losses could be reduced to 0.08 dB by depositing silicon oxynitride films onto double-side polished silicon substrates. The results suggested silicon oxynitride film was a very attractive single layer anti-reflection coating for SOI-based optoelectronic device.     

Influence of Al concentration on structural and optical properties of Al-doped ZnO thin films

Undoped ZnO and Al-doped zinc oxide (ZnO:Al) thin films with different Al concentrations were prepared onto Si (100) substrate by pulsed filtered cathodic vacuum arc deposition system at room temperature. The influence of doping on the structural and optical properties of thin films was investigated. The preferential (002) orientation was weakened by high aluminum doping in films. Raman measurement was performed for the doping effects in the ZnO. Atomic force microscopy images revealed that the surface of undoped ZnO film grown at RT was smoother than that of the Al-doped ZnO (ZnO:Al) films. The reflectance of all films was studied as a function of wavelength using UV–Vis–NIR spectrophotometer. Average total reflectance values of about 35 % in the wavelength range of 400–800 nm were obtained. Optical band gap of the films was determined using the reflectance spectra by means of Kubelka–Munk formula. From optical properties, the band gap energy was estimated for all films.     

纳米TiO2薄膜的脉冲激光沉积及其光学特性

采用脉冲激光沉积技术(PLD)在硅基片上生长了二氧化钛纳米晶氧化物薄膜, 系统讨论了基片温度、氧分压等因素对薄膜结构特性的影响.X射线衍射结果表明在氧气氛下, 生长的薄膜为锐钛矿结构, 其结晶性随着基片温度的升高而增强, 在750℃、5Pa氧压的情况下为完全c轴取向的锐钛矿相TiO₂薄膜, 在750℃、5Pa氩气氛下则为(110)取向的金红石相薄膜. 场发射扫描电子显微镜结果表明薄膜表面致密, 呈纳米晶结构, 其晶粒尺寸在35nm左右.用傅立叶红外光谱和拉曼光谱对不同条件下制备的TiO₂薄膜进行了表征.紫外-可见透射光谱的测试结果表明, 薄膜在可见光区具有良好的透过率, 计算得到制备的锐钛矿和金红石相TiO₂薄膜在550nm处的折射率分别为2.3和2.5, 其光学带隙分别为3.2和3.0eV.因此通过沉积条件的改变可得到结晶性能和光学性能都不同的TiO₂薄膜.     

Fabrication and optical property of vertically-aligned ZnO/Si double nanostructures

We fabricated the vertically-aligned zinc oxide (ZnO)/silicon (Si) double nanostructures by simple processes using the metal-assisted chemical etching and a subsequent hydrothermal synthesis, and their optical property was investigated. For efficient antireflection characteristics, Si nanostructures were optimized by changing the size of the dewetted silver (Ag) at different etching times. The thermally dewetted Ag nanoparticles or semi-island films as metal catalysts were controlled by the Ag film thickness and dewetting temperature. To form the ZnO/Si double nanostructures, ZnO nanorods were synthesized on the chemically etched Si nanostructures using a thin sputtered ZnO seed layer. The grown ZnO nanorod arrays (NRAs) exhibited good crystallinity and further reduced the surface reflection due to their antireflective property. The ZnO/Si double nanostructures showed the increased peak intensity of X-ray diffraction as well as the significantly reduced solar weight reflectance of 6.05% compared to 11.71% in the ZnO NRAs on the flat Si substrate. Also, the enhanced antireflection property of ZnO/Si double nanostructures was theoretically analyzed by performing the rigorous coupled wave analysis simulation.     

Defect formation in hafnium dioxide thin films

Hafnium dioxide thin films were deposited by reactive electron-beam evaporation at six different substrate temperatures on fused-silica substrates. During the depositions, the scattering of light caused by the growth of defects in the films was recorded with in situ total internal reflection microscopy. After deposition the films were analyzed by angle-resolved scatterometery, spectrophotometric measurement of film reflectance and transmittance, atomic force microscopy, and x-ray diffraction. We explore the effects of film defect formation on film optical properties and film surface topography using these data.     

Substrate biasing effects on the microstructure of magnetron-sputtered AlN films investigated by in situ reflectance interferometry

In situ reflectance interferometry (RI) at 400 nm wavelength was used to investigate the effect of the substrate negative bias on the microstructure of aluminium nitride (AlN) films deposited at room temperature on Si substrates by magnetron sputtering. Their surface reflectance recorded during film deposition promptly yields real-time information on the microstructures developed under oxygen contamination and bias change. Specifically, the refractive index n and the extinction coefficient k are deduced from reflectance using appropriate multilayer optical models and validated by spectroscopic ellipsometry. These optical constants correlate appreciably with the microstructure that evolves between columnar-crystallized and purely amorphous phases including in-between amorphous states containing dispersed nano-AlN grains. These microstructures were identified using ex situ energy dispersive X-ray spectroscopy, transmission electron microscopy and diffraction, X-ray diffraction and Auger electron spectroscopy. The simple and cost-effective in situ RI thus appears a powerful tool in controlling the microstructures of thin AlN films for desired applications.