碱催化多孔SiO_2/PI杂化薄膜的制备与力学性能研究

采用碱催化正硅酸乙酯(TEOS)的溶胶-凝胶法与分子模板法相结合,通过旋转涂覆在硅衬底上制备掺杂聚酰亚胺(PI)的纳米多孔SiO2薄膜,并在其表面制备致密过渡膜。利用差热分析(DSC-TGA)、原子力显微镜(AFM)、台阶仪(Atomic-Profiler)、微纳力学性能测试仪(Universal Nano+Micro Mechanical Tester)等对薄膜的性能进行了分析表征。结果表明,所制备的SiO2/PI杂化多孔薄膜具有较好的力学性能和热稳定性;一层膜和两层膜的平均厚度分别为917和1288nm;镀有过渡膜的样品具有最为平整的表面形貌和最小的表面动摩擦系数。     

Biomimetic formation of titania thin films: effect of amino acids on the deposition process

Different types of amino acids have been used as additives to control the aqueous deposition of titanium dioxide thin films on single-crystal Si wafers. Thin titania films can be obtained through a chemical bath deposition (CBD) process using TiCl? as a precursor in an aqueous solution at temperatures below 100 °C. The addition of amino acids to the deposition solution was shown to reduce the thickness and roughness of the films and to increase their density. These protein building blocks were employed to modify the deposition rate as well as the size of aggregates that form the film. The thickness, crystallinity, morphology and composition of the grown films were characterized by a variety of techniques, including XRD, XPS, AFM and SEM. The consequences of the type of the amino acid additive (and its concentration in the solution) on the microstructural evolutions of the deposed films are thus revealed and discussed on the basis of the organic-inorganic interactions in solution and at the film surface.     

Epitaxial silicon carbide on a 6″ silicon wafer

The results of the growth of silicon-carbide films on silicon wafers with a large diameter of 150 mm (6″) by using a new method of solid-phase epitaxy are presented. A SiC film growing on Si wafers was studied by means of spectral ellipsometry, SEM, X-ray diffraction, and Raman scattering. As follows from the studies, SiC layers are epitaxial over the entire surface of a 150-mm wafer. The wafers have no mechanical stresses, are smooth, and do not have bends. The half-width of the X-ray rocking curve (FWHM_ω?θ) of the wafers varies in the range from 0.7° to 0.8° across the thickness layer of 80–100 nm. The wafers are suitable as templates for the growth of SiC, AlN, GaN, ZnO, and other wide-gap semiconductors on its surface using standard CVD, HVPE, and MBE methods.     

Spectroscopic investigations of the stability of porous silicon structure obtained by etching Si(100) in aqueous ammonium fluoride solution

The structure of porous silicon (por-Si) obtained by electrochemical etching of Si(100) single crystal wafers in an aqueous ammonium fluoride solution with isopropyl alcohol additions has been studied using X-ray reflection spectroscopy, X-ray photoelectron spectroscopy, and external X-ray quantum yield measurements. It is established that por-Si layers obtained by the nontraditional technology (not involving hydrofluoric acid) possess a partly amorphized structure and bear a stable surface oxide film with a thickness not exceeding 5 nm.     

Thin pinhole-free carbon films

Uniform pinhole-free carbon films were prepared on silicon wafers, oxidized silicon wafers, sapphire and Al₂O₃ by the in situ thermal decomposition of a phenol-formaldehyde resin. Homogeneous and reproducible film thickness, in the range from 0.3 to 1.5 μm, as well as complete coverage of surface features was achieved by spin coating the substrates with a solution of the resin. The electrical resistivities ranged from 2 × 10^?2 to 2 × 10^?3 Ω cm depending upon the upper limit of the pyrolysis temperature.     

Co-sputtered Si-Cr resistive films

Si-Cr films of variable composition between pure silicon and pure chromium have been deposited by co-sputtering on to glass substrates and thermally oxidized silicon wafers. In order to assess the applications of the Si-Cr films to thin film resistors, the electrical characteristics of the films have been determined as a function of composition, thickness, thermal treatments, etc.     

Residual stress measurement in filament-evaporated aluminium films on single crystal silicon wafers

Shadow Moire interferometry was used to determine the residual stresses in thin, filament-evaporated aluminium films deposited on (100) p-type, 10.16 cm diameter, 0.05 cm thick, circular single crystal silicon wafers. The aluminium film thicknesses ranged from 70 to 780 nm. Benchmark experiments on wafers without aluminium films showed that wafers possess in-plane residual stresses; the centre of the wafer is under tensile stresses of the order of 30 M Pa and these stresses decrease toward the edge of the wafers to approximately 10 M Pa. The deposition of aluminium films increases these tensile residual stresses by 3 to 15 M Pa depending on the film thickness. The increase in the stress is attributed to the stresses in the films.     

A reclaiming process for solar cell silicon wafer surfaces

The low yield of epoxy film and Si3N4 thin-film deposition is an important factor in semiconductor production. A new design system using a set of three lamination-shaped electrodes as a machining tool and micro electro-removal as a precision reclaiming process of the Si3N4 layer and epoxy film removal from silicon wafers of solar cells surface is presented. In the current experiment, the combination of the small thickness of the anode and cathodes corresponds to a higher removal rate for the thin films. The combination of the short length of the anode and cathodes combined with enough electric power produces fast electroremoval. A combination of the small edge radius of the anode and cathodes corresponds to a higher removal rate. A higher feed rate of silicon wafers of solar cells combined with enough electric power produces fast removal. A precise engineering technology constructed a clean production approach for the removal of surface microstructure layers from silicon wafers is to develop a mass production system for recycling defective or discarded silicon wafers from solar cells that can reduce pollution and lower cost.     

Effect of platinum distribution on the hydrogen gas sensor properties in tin oxide thin films

Tin oxide and platinum layers were deposited on oxidized silicon wafers by ion-beam sputtering. The hydrogen gas sensing properties of undoped films and platinum-doped films were examined at 300°C for films annealed at 500°C. It was observed that the surface platinum when annealed together with the tin oxide film increased the sensitivity and reduced the response time compared with those of undoped films. Longer annealing tended to shift the optimum sensor thickness to a thicker side; the optimum thickness changed from 17 to 37 nm as the annealing time increased from 2 to 50 h. The interdiffusivity between the platinum and the tin atoms in the bulk was negligibly small at 300°C.     

Spectroscopic ellipsometry characterization of SiNx antireflection films on textured multicrystalline and monocrystalline silicon solar cells

We present a spectroscopic ellipsometry study of silicon nitride based antireflection films deposited on chemically textured multi- and monocrystalline silicon wafers. The ellipsometric parameters were measured from the near infrared to the ultra violet spectral region. We report the effective thickness and complex index of refraction parameters of the antireflection films from all studied surfaces, regardless of their microscopic morphology. We report on a method to make ellipsometric measurements of the effective optical constants and thickness parameters of thin films deposited on alkaline etched (100)-oriented monocrystalline silicon. The effect of the texture on the complex index of refraction can be described within an effective medium approximation approach. The optical properties are consistent with those obtained from a series of reference films deposited on flat silicon surfaces.     

AES/XPS Thickness measurement of the native oxide on single crystal Si wafers

The thickness determination of a native oxide film at the semi-conductor surface is the subject of this work. The study has been carried out on silicon wafers obtained by produ$\text{c}$tion plant and after different shaping operations. XPS and Auger spectroscopies have been used to evaluate and characterize the oxide layer. Five different methods of measurement, based on spectroscopic parameters proportional to the film width, are proposed. The results obtained show that Auger spectroscopy gives the simplest and the fastest method to measure the native oxide thickness routinely.     

X-ray reflectivity study of r.f.-sputtered thin SiO2 films

X-ray reflectivity investigations have been performed on thin amorphous SiO₂ films obtained by r.f.-sputtering of fused quartz onto Si single crystals in an argon atmosphere.This is a non-destructive technique to determine thickness and density as well as the interface and surface roughness. For the SiO₂/Si system (small differences in density) the X-ray reflectivity is sufficiently sensitive to provide precise information on the occurence of an intermediate layer we obtained only on well-polished silicon wafers.The thickness of the films is compared with that obtained from ellipsometry data and mechanical scanning measurements (stylus method).     

The preparation and characterization of photocatalytically active TiO2 thin films and nanoparticles using Successive-Ionic-Layer-Adsorption-and-Reaction

Photocatalytically active TiO₂ thin-films were deposited on silicon wafers using the Successive-Ionic-Layer-Adsorption-and-Reaction technique and subsequent hydrothermal and/or furnace annealing. Atomic-force-microscopy images and X-ray diffraction measurements of the TiO₂ films obtained under various annealing conditions show how changes of the micro-scale surface structure depend on the post-SILAR treatment. The hydrogen evolution over various TiO₂ films was measured. Hydrothermally treated TiO₂ films show a higher photocatalytic activity and a much better mechanical stability compared to furnace-annealed films. The optical transmittance of TiO₂ thin films on glass substrates was also studied. A red shift was observed with increasing film thickness. TiO₂ nanoparticles (∼10 nm) that were peeled off from the TiO₂ films were investigated using high-resolution-transmission-electron-microscopy.     

Chemical solution deposition of thin TiO2-anatase films for dielectric applications

Thin films of TiO₂ have been prepared using chemical solution deposition on 6 n-type Si(1 0 0) wafers. Thin film thickness in the range from 70 to 210 nm could be achieved via control of the number of deposition sequences. The final annealing temperature of 700 °C resulted in an anatase phase structure with fine elongated grains and smooth surface topography. The capacity of the thin films is shown to depend on thickness, and could be interpreted assuming a series capacity with an SiO₂ interfacial layer. The resulting dielectric constant of the TiO₂ thin film has been calculated to be 23. The leakage current behavior and the break-down field also depend on film thickness. It is shown that thinner films are higher break-down fields.     

纳米多孔SiO2/PI杂化薄膜的制备与性能研究

采用碱催化正硅酸乙酯(TEOS)的溶胶-凝胶法与分子模板法相结合,通过旋转涂覆在硅衬底上制备了掺杂聚酰亚胺(PI)的纳米多孔SiO2薄膜,并利用差热分析(DSC-TGA)、红外吸收光谱(FTIR)、原子力显微镜(AFM)、X射线衍射(XRD)、台阶仪(Atom-ic-Profiler)等对薄膜的性能进行了分析表征.结果表明,所制备的SiO2/PI杂化多孔薄膜为多孔的无定型结构,具有较好的热稳定性及力学性能,一层膜和两层膜的平均孔径分别为68和72nm,厚度分别为917和1288nm.     

Temperature‐Sensitive Hydrogel‐Particle Films from Evaporating Drops

A simple method to prepare temperature‐sensitive films composed of micrometer‐sized colloidal hydrogel particles using evaporating drops of colloidal suspensions is demonstrated. The films range in thickness from a monolayer to approximately fifty particle diameters depending on initial particle volume fraction. Sessile droplets of hydrogel‐particle suspensions are evaporated on silicon wafers. The film is formed from particles spread densely over the air–water interface which then cross‐link and are deposited on the surface during the evaporation process. The resultant thin films exhibit a temperature‐responsiveness characteristic of the individual particles permitting modulation of size, shape, porosity, and optical transmission.     

Effects of porosity on ferroelectric properties of Pb(Zr0.2Ti0.8)O3 films

The sol-gel deposition method has been successfully applied to obtain Pb(Zr_0.2Ti_0.8)O₃ thin films on platinized silicon wafers. Addition of different amounts (7-15 wt.%) of organic macromolecular polyvinylpyrrolidone in the precursor solution prior to spin coating proves to be an excellent method for obtaining porous films. The crystal structure of as deposited films was analyzed by X-ray diffraction. The porous films show perovskite phase after annealing at 650 °C. The surface morphology has been studied by Atomic Force Microscopy and Scanning Electron Microscopy. The surface profile indicates a roughness of the film of 5 nm and no microcracks on the surface. The ferroelectric behavior was proved for each film, by hysteresis loops and by the “butterfly” shape of the capacitance-voltage characteristics. The remnant polarization and the coercive field decrease while the amount of added PVP increases.     

Using thin film stress to produce precision, figured X-ray optics

We are studying the possibility of producing precision, aspherical mirrors for X-rays and visible light. Our study examines the use of ultrastructure processing to replace mechanical methods of material removal. The method starts with a chemically-mechanically polished, flat silicon wafer. The aim is to preserve atomic scale smoothness of the surface wafer while the wafer is bent to a desired figure. We report measurements of the mechanical properties of various stressing layers. This involves measuring the deformation of several thin silicon wafers coated with chemically vapor deposited nickel and boron films of known thickness. We have found that, under normal conditions, the film does not add to the microroughness of the substrate on either the front or the back surfaces. Film and substrate thicknesses, however, vary by as much as 10%. This is the present limit on figure accuracy. We have developed a model that describes bending of B/Si and Ni/Si structures. The model relates stress and Young's modulus to the measured thickness of the film, and the thickness and curvature of the substrate. This approach is used to measure the stress and Young's modulus for boron and nickel films. The Young's modulus E_f was 3.05 x 10¹² Pa for the boron films and 1.4 x 10¹⁰ Pa for the nickel films. From the relationship developed and verified for predicting the radii of curvature of the substrate, if may be possible to define a film thickness pattern which would provide a desired optical figure.     

Effect of the nanographite film thickness on the optical rectification pulse

The phenomenon of optical rectification during pulsed laser irradiation was studied in nanographite films of various thicknesses obtained by plasmachemical deposition on silicon substrates. The amplitude of the optical rectification pulse (ORP) strongly depends on the film thickness h and reaches a maximum at h ∼ 2.5 μm. At a smaller film thickness, the ORP is accompanied by a photoelectric signal of microsecond duration, which arises in the silicon substrate. For the nanographite films with h > 2.5 μm, the ORP is observed in the absence of any signal from the substrate, which allows such films to be used in fast-response detectors of pulsed laser radiation in a broad spectral range.     

溶胶—凝胶法制备TiO2—SiO2复合薄膜的研究

采用溶胶－凝胶方法在单晶Ｓｉ基片上制备了ＴｉＯ２－ＳｉＯ２复合薄膜，研究了溶剂、ｐＨ值对先体溶液成胶时间的作用，溶液的浓度、甩胶时的旋转速度、涂覆层数以及热处理温度对薄膜厚度、光学性能的影响。薄膜的折射率随温度增大，其主要贡献来自于薄膜中结构的变化。并测量了薄膜的Ｉ－Ｖ、Ｃ－ｆ特性，由于薄膜中的热击穿效应而使得ＴｉＯ２含量较高的薄膜２的Ｉ－Ｖ呈非线性变化。