Size Effect and Geometrical Effect of Polycrystals and Thin Film/Substrate System in Micro-indentation Test

Micro-indentation test at scales on the order of sub-micron has shown that the measured hardness increases strongly with decreasing indent depth or indent size, which is frequently referred to as the size effect. Simultaneously, at micron or sub-micron scale, the material microstructure size also has an important influence on the measured hardness. This kind of effect, such as the crystal grain size effect, thin film thickness effect, etc., is called the geometrical effect by here. In the present research, in order to investigate the size effect and the geometrical effect, the micro-indentation experiments are carried out respectively for single crystal copper and aluminum, for polycrystal aluminum, as well as for a thin film/substrate system, Ti/Si3N4. The size effect and geometrical effect are displayed experimentally. Moreover, using strain gradient plasticity theory, the size effect and the geometrical effect are simulated. Through comparing experimental results with simulation results, length-scale parameter appearing in the strain gradient theory for different cases is predicted. Furthermore, the size effect and the geometrical effect are interpreted using the geometrically necessary dislocation concept and the discrete dislocation theory. Member Price: $0; Non-Member Price: $25.00

Nanoindentation of thin-film-substrate system: Determination of film hardness and Young's modulus

In the present paper, the hardness and Young's modulus of film-substrate systems are determined by means of nanoindentation experiments and modified models. Aluminum film and two kinds of substrates; i.e. glass and silicon, are studied. Nanoindentation XP II and continuous stiffness mode are used during the experiments. In order to avoid the influence of the Oliver and Pharr method used in the experiments, the experiment data are analyzed with the constant Young's modulus assumption and the equal hardness assumption. The volume fraction model (CZ model) proposed by Fabes et al. (1992) is used and modified to analyze the measured hardness. The method proposed by Doerner and Nix (DN formula) (1986) is modified to analyze the measured Young's modulus. Two kinds of modified empirical formula are used to predict the present experiment results and those in the literature, which include the results of two kinds of systems, i.e., a soft film on a hard substrate and a hard film on a soft substrate. In the modified CZ model, the indentation influence angle, phi, is considered as a relevant physical parameter, which embodies the effects of the indenter tip radius, pile-up or sink-in phenomena and deformation of film and substrate.

Design and properties analysis of multi-layer dielectric used in pulse compressor gratings

Used in chirped-pulse amplification system and based on multi-layer thin film stack, pulse compressor gratings (PCG) are etched by ion-beam and holographic techniques. Diffraction efficiency and laser-induced damage threshold rely on the structural parameters of gratings. On the other hand, they depend greatly on the design of multi-layer. A theoretic design is given for dielectric multi-layer, which is exposed at 413.1 nm and used at 1053 nm. The influences of coating design on optical characters are described in detail. The analysis shows that a coating stack of H3L (H2L) (boolean AND) 9H0.5L2.01H meets the specifications of PCG well. And there is good agreement of transmission between experimental and the theoretic design. (c) 2005 Elsevier GmbH. All rights reserved.

Optimization of thin-film design for multi-layer dielectric grating

Thin-film design used to fabricate multi-layer dielectric (MLD) gratings should provide high transmittance during holography exposure, high reflectance at use wavelength and sufficient manufacturing latitude of the grating design making the MLD grating achieve both high diffraction efficiency and low electric field enhancement. Based on a (HLL)H-9 design comprising of quarter-waves of high-index material and half-waves of low-index material, we obtain an optimum MLD coating meeting these requirements by inserting a matching layer being half a quarter-wave of Al2O3 between the initial design and an optimized HfO2 top layer. The optimized MLD coatings exhibits a low reflectance of 0.017% under photoresist at the exposure angle of 17.8 degrees for 413 nm light and a high reflectance of 99.61% under air at the use angle of 51.2 degrees for 1053 nm light. Numerical calculation of intensity distribution in the photoresist coated on the MLD film during exposure shows that standing-wave patterns are greatly minimized and thus simulation profile of photoresist gratings after development demonstrates smoother shapes with lower roughness. Furthermore, a MLD gratings with grooves etched into the top layer of this MLD coating provides a high diffraction efficiency of 99.5% and a low electric field enhancement ratio of 1.53. This thin-film design shows perfect performances and can be easily fabricated by e-beam evaporation. (c) 2006 Elsevier B.V. All rights reserved.

High-mobility pentacene thin-film transistors with copolymer-gate dielectric

Pentacene thin-film transistors have been obtained using polymethyl-methacrylate-co-glyciclyl-methacrylate (PNIMA-GMA) as the gate dielectric. The optimum active layer thickness in thin-film transistors (OTFTs) was investigated. The present devices show a wide operation voltage range. The on/off current ratio is as high as 10(5). In linear region (V-DS = -2V), the field-effect mobility of device increases with the increase in gate field at low-voltage region (V-G < - 20 V), and a mobility of 0.33 cm(2)/Vs can be obtained when V-G > 20 V. In saturation region, the mobility increases linearly with the gate field, and a high mobility of 1.14 cm(2)/Vs can be obtained at V-G = -95V. The influence of voltage on mobility of device was investigated.

AMPEROMETRIC DETECTION OF AMINO-ACIDS IN A FLOW-INJECTION SYSTEM WITH A NICKEL(II)-MODIFIED ELECTRODE WITH AN EASTMAN-AQ POLYMER FILM

Amperometic flow measurements were made at +0.55 V (vs. Ag/AgCl) in 0.1 mol l-1 KOH electrolyte with an Ni(II) chemically modified electrode (CME) with an Eastman-AQ polymer film. The use and characteristics of a Ni(II)-containing crystalline and polymer-modified electrode obtained by a double coating step as a detector for amino acids in a flow-injection system using reversed-phase liquid chromatography are described. The detection of these analytes is based on the higher oxidation state of nickel (NiOOH) controlled by the applied potential. The electroanalytical parameters and the detection current for a series of amines and amino acids were investigated. The use of such a CME in the flow-injection technique was found to be suitable in a solution at low pH. The linear range for glycine is 5 X 10(-6)-0.1 mol 1-1 with a detection limit of 1.0 X 10(-6) mol l-1. A 1 X 10(-4) mol 1-1 mixture of serine and tyrosine was also detected after separation on an Nucleosil C18 column.

Squeeze-film Effects in MEMS Devices with Perforated Plates for Small Amplitude Vibration

Squeeze-film effects of perforated plates for small amplitude vibration are analyzed through modified Reynolds equation (MRE). The analytical analysis reckons in most important influential factors: compressibility of the air, border effects, and the resistance caused by vertical air flow passing through perforated holes. It is found that consideration of air compressibility is necessary for high operating frequency and small ratio of the plate width to the attenuation length. The analytical results presented in this paper agree with ANSYS simulation results better than that under the air incompressibility assumption. The analytical analysis can be used to estimate the squeeze-film effects causing damping and stiffness added to the system. Since the value of Reynolds number involved in this paper is low (< 1), inertial effects are neglected.

Assessment of Microscale Test Methods of Peeling and Splitting along Surface of Thin-Film/Substrates

Peel test methods are assessed through being applied to a peeling analysis of the ductile film/ceramic substrate system. Through computing the fracture work of the system using the either beam bend model (BB model) or the general plane analysis model (GPA model), surprisingly, a big difference between both model results is found. Although the BB model can capture the plastic dissipation phenomenon for the ductile film case as the GPA model can, it is much sensitive to the choice of the peeling criterion parameters, and it overestimates the plastic bending effect unable to capture crack tip constraint plasticity. In view of the difficulty of measuring interfacial toughness using peel test method when film is the ductile material, a new test method, split test, is recommended and analyzed using the GPA model. The prediction is applied to a wedge-loaded experiment for Al-alloy double-cantilever beam in literature.

Refractive index and thickness analysis of natural silicon dioxide film growing on silicon with variable-angle spectroscopic ellipsometry

The refractive index and thickness of SiO2 thin films naturally grown on Si substrates were determined simultaneously within the wavelength range of 220-1100 nm with variable-angle spectroscopic ellipsometry. Different angles of incidence and wavelength ranges were chosen to enhance the analysis sensitivity for more accurate results. Several optical models describing the practical SiO2-Si system were investigated, and best results were obtained with the optical model, including an interface layer between SiO2 and Si, which proved the existence of the interface layer in this work as described in other publications.

Multiscale Treatment of Thin-Film Lubrication

A multiscale technique that combines an atomistic description of the interfacial (near) region with a coarse-grained (continuum) description of the far regions of the solid substrates is proposed. The new hybrid technique, which represents an advance over a previously proposed dynamically-constrained hybrid atomistic-coarse-grained treatment (Wu et al.J. Chem. Phys., 120, 6744, 2004), is applied to a two-dimensional model tribological system comprising planar substrates sandwiching a monolayer film. Shear–stress profiles (shear stress versus strain) computed by the new hybrid technique are in excellent agreement with “exact” profiles (i.e. those computed treating the whole system at the atomic scale).

Size Dependent Nanoindentation of a Soft Film on a Hard Substrate

Nanoindentation experiments on Al/glass systems show that, as the indentation depth increases, the hardness decreases during a shallow indentation, and increases when the indenter tip approaches the film–substrate interface. We associate the rise in hardness during two stages with the strong strain gradient effects, the first stage is related with the small scale effects and the second stage with the strain gradient between the indenter and the hard substrate. Using the strain gradient theory proposed by Chen and Wang and the classical plasticity theory, the observed nanoindentation behavior is modeled and analyzed by means of the finite element method, and it is found that the classical plasticity cannot explain the experiment results but the strain gradient theory can describe the experiment data at both shallow and deep indentation depths very well. The results prove that both the strain gradient effects and substrate effects exist in the nanoindentation of the film–substrate system.

Characterization of the Fracture Work for Ductile Film Undergoing the Micro-Scratch

The interface adhesion strength (or interface toughness) of a thin film/substrate system is often assessed by the micro-scratch test. For a brittle film material, the interface adhesion strength is easily obtained through measuring the scratch driving forces. However, to measure the interface adhesion strength (or interface toughness) for a metal thin film material (the ductile material) by the microscratch test is very difficult, because intense plastic deformation is involved and the problem is a three-dimensional elastic-plastic one. In the present research, using a double-cohesive zone model, the failure characteristics of the thin film/substrate system can be described and further simulated. For a steady-state scratching process, a three-dimensional elastic-plastic finite element method based on the double cohesive zone model is developed and adopted, and the steady-state fracture work of the total system is calculated. The parameter relations between the horizontal driving forces (or energy release rate of the scratching process) and the separation strength of thin film/substrate interface, and the material shear strength, as well as the material parameters are developed. Furthermore, a scratch experiment for the Al/Si film/substrate system is carried out and the failure mechanisms are explored. Finally, the prediction results are applied to a scratch experiment for the Pt/NiO material system given in the literature.

Determination Ofinterfacial Mechanical Parameters For An Al/Epoxy/Al2O3 System Byusing Peel Test Simulations

Peel test measurements and simulations of the interfacial mechanical parameters for the Al/Epoxy/Al2O3 system are performed in the present investigation. A series of Al film thicknesses between 20 and 250 microns and three peel angles of 90, 135 and 180 degrees are considered. Two types of epoxy adhesives are adopted to obtain both strong and weak interface adhesions. A finite element model with cohesive zone elements is used to identify the interfacial parameters and simulate the peel test process. By simulating and recording normal stress near the crack tip, the separation strength is obtained. Furthermore, the cohesive energy is identified by comparing the simulated steady-state peel force and the experimental result. It is found from the research that both the cohesive energy and the separation strength can be taken as the intrinsic interfacial parameters which are dependent on the thickness of the adhesive layer and independent of the film thickness and peel angle.

Inverse Analysis Determining Interfacial Properties Between Metal Film And Ceramic Substrate With An Adhesive Layer

In the present study, peel tests and inverse analysis were performed to determine the interfacial mechanical parameters for the metal film/ceramic system with an epoxy interface layer between film and ceramic. Al films with a series of thicknesses between 20 and 250 mu m and three peel angles of 90 degrees, 135 degrees and 180 degrees were considered. A finite element model with the cohesive zone elements was used to simulate the peeling process. The finite element results were taken as the training data of a neural network in the inverse analysis. The interfacial cohesive energy and the separation strength can be determined based on the inverse analysis and peel experimental result.

Properties of high k gate dielectric gadolinium oxide deposited on Si(100) by dual ion beam deposition (DIBD)

Gadolinium oxide thin films have been prepared on silicon (100) substrates with a low-energy dual ion-beam epitaxial technique. Substrate temperature was an important factor to affect the crystal structures and textures in an ion energy range of 100-500 eV. The films had a monoclinic Gd2O3 structure with preferred orientation ((4) over bar 02) at low substrate temperatures. When the substrate temperature was increased, the orientation turned to (202), and finally, the cubic structure appeared at the substrate temperature of 700 degreesC, which disagreed with the previous report because of the ion energy. The AES studies found that Gadolinium oxide shared Gd2O3 structures, although there were a lot of oxygen deficiencies in the films, and the XPS results confirmed this. AFM was also used to investigate the surface images of the samples. Finally, the electrical properties were presented. (C) 2004 Elsevier B.V. All rights reserved.