Development of artificial neural networks for real time, in situ ellipsometry data reduction

Development of real time in situ monitoring and control of thin film depositions using ellipsometry requires both data acquisition and processing to be rapid. Present speeds of measurement and computation of basic parameters, Ψ and Δ, are sufficient for data acquisition which is essentially real time. However, computation of film parameters, such as thickness and optical properties, generally cannot keep up with the incoming data and must be performed in a batch mode after the deposition.

This work describes the development of enhanced, high speed data reduction algorithms using artificial neural networks (ANN). The networks are trained using computed data and subsequently give values of film parameters in the millisecond time regime. The ANN outputs are used as initial estimates in a variably damped least squares algorithm for accuracy improvement. The combination of these two algorithms provides very accurate solutions in 75 ms per point on a DEC VAX 8800 multiprocessor system running at a combined 12 Mips. This speed is suitable for real time film monitoring and control for growth rates up to 10 nm per second. Results for fixed angle of incidence, single wavelength, in situ data for Ni deposited on BK7 substrates are presented.     

Application of in situ ellipsometry in the fabrication of thin-film optical coatings on semiconductors

Thin-film interference filters, suitable for use on GaAs- and InP-based lasers, have been fabricated by use of the electron-cyclotron resonance plasma-enhanced chemical vapor deposition technique. Multilayer film structures composed of silicon oxynitride material have been deposited at low temperatures with an in situ rotating compensator ellipsometer for monitoring the index of refraction and thickness of the deposited layers. Individual layers with an index of refraction from 3.3 to 1.46 at 633 nm have been produced with a run-to-run reproducibility of 0.005 and a thickness control of 10 A. Several filter designs have been implemented, including high-reflection filters, one- and two-layer anitreflection filters, and narrow-band high-reflection filters. It is shown that an accurate measurement of the filter optical properties during deposition is possible and that controlled reflectance spectra can be obtained.     

Study of the substrate treatment effect on initial growth of indium tin-oxide films on polymer substrate using in situ conductance measurement

Changes in the initial growth mode of ion beam sputtered indium tin oxide (ITO) films on polycarbonate (PC) substrates were investigated by an in situ measurement of electrical conductance. The PC substrates were irradiated with l keV Ar ions in an oxygen environment (ion assisted reaction: IAR), prior to the film deposition for changing the surface energy. The electrical conduction modes in ITO films were discussed in terms of the film thickness and the surface energy of PC substrates. It was found that, in the initial part of the film growth, ITO nucleation density increased with the increase of the surface energy of PC. The change of the growth mode was discussed in both viewpoints of thermodynamics and atomic kinetics theories and verified by AFM (atomic force microscope) observations. Thermal stability of ITO films was investigated to observe the effect of the growth mode change by IAR pre-treatment of polymer substrate.     

In situ Fourier transform P-polarized infrared reflection absorption spectroscopic investigation of an interface properties of SiO2/Si(100) deposited using electron cyclotron resonance microwave plasma at room temperature

Amorphous SiO₂ films have been deposited onto the Si substrate, without heating, using sputtering-type electron cyclotron resonance (ECR) microwave plasma. In situ Fourier transform P-polarized infrared reflection absorption spectroscopy (ISFT-PIRRAS) has been used to study the properties of a-SiO₂/Si interface. The results from ISFT-PIRRAS monitoring indicated that the interface stress led to significant distortion in the local structure, which resulted in the broadening of a transverse optical mode (TO₃) located at 1050 cm⁻¹. The interface stress decreased with increased film thickness. In addition, the longitudinal optical phonon mode (LO₃, located at 1223 cm⁻¹) related to TO₃ mode was observed due to Berreman effect [B. Harbecke, Appl. Phys. A: Solids Surf. 38 (1985) 263]. This phonon mode is very sensitive to SiO₂ film thickness, which enables it to be used to detect and characterize ultra thin SiO₂ film. When the film thickness is over 30 nm, a non-linear dependence of the intensity of LO₃ mode on film thickness was observed. However, the TO₃ mode has a near linear dependence on film thickness. Thus, it is more accurate and suitable to detect thick film by monitoring TO₃ mode intensity.     

Thermal wave measurement of wet paint film thickness

Thermal wave phase measurements are reported on the drying of wet paint films on aluminium substrates. Measurements of the change in thickness as the paint dries have also been obtained using a differential focussing technique on an optical microscope. By including the optical microscope measurements of the drying paint film thickness together with estimates for the density and thermal properties of the drying and cured paint, predictions have been made of the thermal phase/thickness relationships for the wet, dry, curing and cured paints. It is concluded that a phase measurement on the wet paints could be used to predict a final cured paint thickness with an accuracy of approximately ±2 μm. Errors in predicting cured film thickness from a wet film thermal phase measurement arises principally from uncertainty over the solvent content of the wet paint film, the state of cure, and the consequent uncertainty over the paint density and thermal properties.     

Thickness measurement of a thin-film layer on an anisotropic substrate by phase-sensitive acoustic microscope

Complex V(z) curves for single thin-film layers on anisotropic substrates are studied both experimentally and theoretically, and the application of V(z) measurement to the determination of film thickness on anisotropic substrates is discussed. Complex V(z) curves for aluminum layers (with thicknesses between 0.5 and 2 mum) on a silicon wafer have been calculated. The inverse Fourier transform of the V(z) curves, which corresponds to the reflection coefficient, shows sharp changes at critical angles of pseudosurface waves, pseudo-Sezawa waves, and Rayleigh surface waves. These critical angles strongly depend on the thickness. Complex V(z) curves for these specimens have been measured using a phase-sensitive acoustic microscope with a point focus lens at 400 MHz. The critical angles of the surface waves obtained from the measured V(z) curves are in good agreement with those obtained from the calculated V(z) curves. On the basis of this result, it is shown that the V(z) measurement is applicable to the determination of film thickness on an anisotropic substrate.     

Residual stresses and Raman shift relation in anatase TiO2 thin film

Anatase TiO₂ film (100-1000 nm thick) grown on glass, sapphire (0001), and Si (100) substrates by pulsed dc-magnetron reactive sputtering were evaluated for stress and strain analysis using Raman spectroscopy and curvature measurement techniques. The X-ray analysis revealed that films prepared for this study were purely anatase, and the measurements indicate that the film exhibit that (101) is the preferred growth orientation of the crystallites, especially for the film thicker than 100 nm. Curvature measurements and Raman spectroscopy, with 514.5 nm excitation wavelength, phonon line shift were used for stress analysis. A comparison between Raman lineshapes and peak shifts yields information on the strain distribution as a function of film thickness. The measurements of residual stresses for crystalline anatase TiO₂ thin film showed that all thin film were under compressive stress. A correlation between Raman shifts and the measured stress from the curvature measurements was established. The behavior of the anatase film on three different substrates shows that the strain in film on glass has a higher value compared to the strain on sapphire and on silicon substrates. The dominant 144 cm^− 1E_g mode in anatase TiO₂ clearly shifts to a higher value by 0.45-5.7 cm^− 1 depending on the type of substrate and film thickness. The measurement of the full width at half maximum values of 0.59-0.80 (2θ°) for the anatase (101) peaks revealed that these values are greater than anatase powder 0.119 (2θ°) and this exhibits strong crystal anisotropy with thermal expansion.     

金刚石膜/氧化铝陶瓷复合材料的介电特性和热学性能研究

研究了金刚石膜/氧化铝陶瓷复合材料作为超高速、大功率集成电路封装基板材料的可行性。采用电容法测量了复合材料的介电性质,结果表明在氧化铝上沉积金刚石膜,能有效降低基片材料的介电系数。碳离子预注入处理使介电损耗降低(从5×10^-3降低到2×10^-3),且频率稳定性更好。金刚石膜的沉积可明显提高基片的热导率,随着薄膜厚度的增加,复合材料的热导率单调递增。当薄膜厚度超过100μm时复合材料的介电系数下降到6.5、热导率上升至3.98W/cm·K,热导率接近氧化铝的20倍。     

Assessment of the Thickness Variation and Surface Roughness of Aqueous Film Coated Tablets Using a Light-Section Microscope

Abstract

The Light-Section Microscope measures the thickness and surface roughness of transparent film coats without contacting them. It enables the determination of tablet film coat thickness at different regions on a tablet surface and analysis of coat thickness variation. Examination of aqueous film coated tablets using a Light-Section Microscope has shown that the coat application conditions can influence the film density and thickness, film thickness variation and film coat surface roughness. Coat application conditions which give rise to smoother surfaces are shown to produce more dense, thinner coats which may exhibit a more even thickness on smooth substrates but larger variations in film thickness on rough substrates. The potential for film thickness and surface roughness to vary at different positions on the substrate surface has also been demonstrated, with film coats tending to be smoother and thinner at the periphery of tablet faces.     

Quantitative analysis of electrodeposited tin film morphologies by atomic force microscopy

This study of the electrodeposition of tin on steel substrates demonstrates that it is possible to obtain quantitative information on the thin film growth at industrially relevant substrates using atomic force microscopy (AFM) to monitor the film morphology and X-ray fluorescence (XRF) to measure the average film thickness. The effects of current density and electrolyte temperature on the film morphology, surface roughness, and grain size distribution (GSD) are reported. While the roughness of the substrates used in this study can vary by several hundred nanometers to a micrometer, we are interested in quantitative characterization of the tin films with thickness varying from a few tens of nanometers to several hundred nanometers. This study shows that for the range of film thickness and length scale studied, analysis of the AFM images can provide quantitative characterization of the thin film roughness and grain size distribution at various stages of growth with little interference from the substrate morphological inhomogeneities.     

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。     

大型水轮机组推力轴承油膜厚度在线监测研究

油膜厚度是反映推力轴承运行状态的重要参数,对油膜厚度进行实时在线监测有助于实现推力轴承的稳定运行。以某大型水轮机组推力轴承为例,结合其润滑流体的雷诺方程和油膜厚度方程,利用有限差分法分析了不同载荷和不同转速下推力轴承油膜厚度和压力分布的变化规律,并设计了一种油膜厚度实时在线监测方法。理论分析结果表明,当转速一定时,推力轴承油膜厚度先随着载荷的增大而增大,达到峰值后,随着载荷的增大而减小;当载荷一定时,油膜厚度随着转速的增大而增大。理论分析结果与该水轮机组推力轴承油膜厚度的在线监测数据完全吻合,验证了提出的油膜厚度在线监测方法的可靠性,为推力轴承运行状态的诊断提供了科学依据。     

The effects of film thickness variations on the residual stress distributions in coated Cr thin films

Generally, the residual stress of thin film coatings is calculated using Stoney's equation. However, variables in the manufacturing of the coated film, such as crystalline particle size and the unevenness of the thickness of the film, cause the radius of curvature of the beam to vary all over the beam. The cantilever beam curves not only in the axial direction but also in the transverse direction. Therefore, the residual stress in a film coating comprises not only axial residual stress but also transverse residual stress, and its distribution is also not uniform. Under such conditions, Stoney's equation must be modified. In this study, Si was used as a substrate in the production of cantilever beam specimens. Chromium thin films of various thicknesses were coated onto the Si substrates. The 3D digital image correlation technique was used to measure the out‐of‐plane displacement of the specimens at various positions. Then the modified Stoney's equation was used to obtain the axial and transverse residual stress at each measurement point to study the effect of variations in the thickness of the thin film on the magnitude and uniformity of the distribution of the residual stresses. Three thin film thicknesses 1, 2, and 3 μm were studied, and three specimens for each thickness were used. For each specimen, axial and transverse residual stresses were obtained at nine test points, and the equivalent residual stress was calculated. The results of this study reveal that as the difference between the thicknesses of the coating increased, average equivalent residual stress decreased and the distribution of stresses became more uniform. By comparing the corresponding results for the 1‐ and 3‐μm‐thick films revealed that the confidence levels in the average value and uniformity of the equivalent residual stress distribution, which increased with thickness, were 92.81% and 80.57%, respectively.     

Measurement of the physical thickness and refractive index of thin epitaxial garnet films

A technique for the measurement of refractive index and physical film thickness of epitaxial garnet films is described which utilizes variable wavelength measurements. Experimental results are presented for gadolinium gallium garnet substrates and two different bubble domain film compositions. From these results, it is concluded that the technique is not applicable to wafers with films on both sides due to the differences in film thickness of the two films. For single sided wafers, the refractive index can be determined with an accuracy of ±0.3 percent.     

Terahertz paintmeter for noncontact monitoring of thickness and drying progress in paint film

We propose a paintmeter for noncontact and remote monitoring of the thickness and drying progress of a paint film based on the time-of-flight measurement of the echo signal of a terahertz (THz) electromagnetic pulse. The proposed method is effectively applied to two-dimensional mapping of the painting thickness distribution for single-layer and multilayer paint films. Furthermore, adequate parameters for the drying progress are extracted from the THz pulse-echo signal and effectively applied to monitor the wet-to-dry transformation. The THz paintmeter can be a powerful tool for quality control of the paint film on the in-process monitoring of car body painting.     

Determination of film thickness and refractive index in one measurement of phase-modulated ellipsometry

Ellipsometry is often used to determine the refractive index and/or the thickness of a polymer layer on a substrate. However, simultaneous determination of these parameters from a single-wavelength single-angle measurement is not always possible. The present study determines the sensitivity of the method to errors of measurement for the case of phase modulated ellipsometry and identifies conditions for decoupling film thickness and refractive index. For a specific range of film thickness, both the thickness and the refractive index can be determined from a single measurement with high precision. This optimal range of the film thickness is determined for organic thin films, and the analysis is tested on hydrogel-like polymer films in air and in water.     

光反射干涉谱新方法测试薄膜厚度和光学常数

依据测量薄膜和光之间相互作用可确定薄膜特性的原理,并基于光反射干涉谱与德国最新研发薄膜分析软件SCOUT的新方法可测量已知或未知材料的多层薄膜厚度及其折射率n、消光系数k。通过实际测试证明：该方法可测试单晶硅、玻璃、ITO玻璃基底上沉积薄膜的厚度,样品基本不需要特别准备,对样品无破坏性,测试精准。理论上可以测量所有透光或半透光薄膜的厚度和光学常数,操作非常简便,适合于镀膜行业的在线检测和实时监控,且SCOUT软件在多层膜及多种材料的研发、制备等方面具有应用潜力。     

Preparation and characterisation of titanium dioxide films for catalytic applications generated by anodic spark deposition

The advanced plasma electrochemical process of anodic spark deposition (ASD) was used to generate photoactive titanium dioxide films on titanium metal substrates. A shift to easier-to-machine substrates was demonstrated by the deposition of a titanium film with physical vapour deposition onto different materials such as glass, silicon, and stainless steel prior to ASD. Obtained films were characterised by scanning electron microscopy, surface area measurement (Brunnauer-Emmett-Teller method, BET), X-ray diffraction, electron-probe microanalysis, and glow discharge spectroscopy. Additionally, film thickness was determined by eddy current measurements. Standard ASD conditions were defined as 180 V applied voltage over a 180 s hold time, a voltage ramp of 20 V/s, a duty cycle of 0.5 and a frequency of 1500 Hz. Most prominent characteristics of the titanium films produced under these standard conditions are a film thickness of ≤80 μm, a surface area of approximately 51 m²/g (BET) and an anatase content of approximately 30% and rutile content of approximately 70%. Furthermore, the film formation process is elucidated and the dependence of film thickness on deposition time and the dependence of the anatase and rutile content on the deposited mass are shown for varying ASD conditions.     

In situ monitoring of film deposition with an ellipsometer based on a four-detector photopolarimeter

Ellipsometry is a sensitive and noninvasive technique for the characterization of thin films. A recently developed ellipsometer, based on the four-detector photopolarimeter, was arranged outside a UHV chemical vapor deposition chamber for the in situ monitoring of film growth processes. The instrument showed a sensitivity in the submonolayer range when used to follow the growth of germanium thin films deposited on silicon substrates. As the main instrument drawback is represented by the need to have precise alignment, an effective positioning procedure was developed to obtain a positioning error smaller than 0.1°.     

Imaging reflectometry in situ

An innovative method of in situ real-time optical monitoring of thin film deposition and etching is presented. In this technique, intensity maps of a thin film corresponding to a series of wavelengths selected by a monochromator (300-800 nm) are recorded by a CCD camera. From the maps the reflectance spectra at individual points of the sample surface can be extracted. By fitting the reflectance spectra to the theoretical ones, the maps of a thin film morphology (including optical parameters) and their temporal development during technological processes can be obtained. The method was tested by in situ observation of the growth of silicon nitride and silicon oxide thin films prepared by ion beam sputtering and by the monitoring of etching of thermally grown SiO(2) thin films.