A Monte Carlo study of the thickness determination of ultra-thin films

A Monte Carlo method is utilized to simulate the energy spectra for low-energy electron backscattered from different thin films deposited on different bulk substrates. A method of thickness determination for ultra-thin films is presented, which is obtained from the analysis of the basic characteristics of the energy spectra of backscattered electrons. This method is predicted to be particularly suitable for determining the thickness of ultra-thin films, and to be useful for both cases of light film on heavy substrate and heavy film on light substrate. The thickness resolution is estimated to be as high as subnanometer scale, provided the resolution of the electron energy spectrometer used to be high enough.     

Physical background of electron backscattering

The parameters governing electron backscattering from thin films and from bulk solids are reviewed: Atomic scattering cross-section, atomic number, single/multiple scattering, film thickness, scattering angular distribution, angle of incidence, diffraction effects. Their influence on some important contrast mechanisms due to backscattered electrons in scanning electron microscopy (thickness contrast, Z/material contrast, tilting/topography contrast, crystal orientation contrast) is discussed. The most frequently used backscattering electron detection systems are briefly described.     

Mirrorlike pulsed laser deposited tungsten thin film

Mirrorlike tungsten thin films on stainless steel substrate deposited via pulsed laser deposition technique in vacuum (10(-5) Torr) is reported, which may find direct application as first mirror in fusion devices. The crystal structure of tungsten film is analyzed using x-ray diffraction pattern, surface morphology of the tungsten films is studied with scanning electron microscope and atomic force microscope. The film composition is identified using energy dispersive x-ray. The specular and diffuse reflectivities with respect to stainless steel substrate of the tungsten films are recorded with FTIR spectra. The thickness and the optical quality of pulsed laser deposition deposited films are tested via interferometric technique. The reflectivity is approaching about that of the bulk for the tungsten film of thickness ～782 nm.     

Dynamic mechanical properties of photo resist thin films

Photo resist thin films have mainly been used and investigated for versatile applications of micro electronic mechanical systems because of its outstanding aspect ratio and attainable film thickness. An accurate structure properties derived from validated material characterization is required in engineering applications. In this work, dynamic responses of photo resist thin films are tested by a nanoindentation in association with a dynamic mechanical analysis, where the thin film is coated on a silicon wafer by spin coating. The results show that the storage modulus of the photo resist thin film remains constant at the beginning and then increases as the indentation depth increases. Meanwhile, the loss modulus increases as the indentation depth increases. Varying the film thickness shows that the substrate effect plays an important role in determining the dynamic properties of thin films. However, the results agree well with the bulk material when the amplitude of nanoindentation is relatively small. It illustrates the dynamic mechanical analysis can be an efficient method to characterize the viscoelastic properties of thin films, but proper attention on the test parameters is needed.     

Anti-oxidant mechanism of TiAlN/SiN decorative films on borosilicate glass by magnetron sputtering

The black TiAlN decorative film was prepared on the borosilicate glass by the magnetron sputtering in equipment with multiple vacuum chambers. The transparent SiN protective layer was deposited on the surface of the TiAlN film to keep the black color invariant at the high temperature. The structure of the TiAlN/SiN film was characterized by scanning electron microscope (SEM), X-ray diffraction (XRD), and high-resolution transmission electron microscopy (HRTEM). The coating adhesion was measured by scratch tester. The TiAlN film has a columnar crystal structure with a thickness of 200 nm, and the top SiN layer is amorphous with a thickness of 100 nm. The coated borosilicate glass with the TiAlN/SiN films still retains the black color after oxidation at 600 °C in atmosphere. While the oxidation temperature elevates to 700 °C, the color of the TiAlN/SiN films begins to change. The top SiN layer plays a role as the barrier against oxygen diffusion into the inner TiAlN layer. The thin self-formed aluminum oxide layer was generated on the surface of the SiN layer and it contributes to the improvement of anti-oxidant property of the inner TiAlN layer. However, the thick self-formed aluminum oxide layer leads to the color change of the black TiAlN film. The thermal oxidation benefits the improvement of the adhesion for the TiAlN/SiN films with glass substrate.     

Glasslike Transitions in Thin Polymer-Melt Films Due to Thickness Constraint

The shear properties of thin films of star and linear polyisoprene (PIP) melts under high pressure were investigated as a function of sliding velocity (shear rate) using the surface forces apparatus. The results were contrasted with their bulk rheological properties; effects of thickness constraint on the shear behavior were discussed. The melts of PIP in bulk exhibit Newtonian-like constant viscosity at least at low shear rates (frequencies), which suggests that individual molecules flow with lateral sliding motion. However, thin films of PIP melts show tribological features involving apparent shear-thinning behavior, indicative of the correlated motions in confined geometries. The shear-property change from bulk rheological behavior to thin-film tribological behavior along with the thickness decrease reflects the physical states and their transitions in the systems; the thickness constraint induces glasslike transitions. Effects of molecular weights and molecular architecture (star-branched or linear) on the shear properties are also discussed.     

Modification of an EM6G electron microscope for X-ray microanalysis

A dual purpose stage has been constructed for an EM6G 100 kV transmission electron microscope. With this stage the composition of thin films and bulk specimens can be determined by X-ray microanalysis. With thin films a change of specimen cartridge then enables a full analysis of crystal defects in the film to be made using tilt controls incorporated in the stage. Modifications to the stage to reduce background effects in X-ray microanalysis spectra are also described. The alternative use of this system in the bulk analysis of specimens by an X-ray fluorescence technique is also discussed.     

Analysis of thermal diffusivity of Ti thin film by thermoreflectance and periodic heating technique

Thermal diffusivity of Ti thin film with several hundred nanometers thickness has been measured by means of thermoreflectance (TR) technique and periodic heating using front heating and front detection configuration. Ti thin films were prepared on Si substrates by dc sputtering method. Then thin Mo layers as reflection layers were coated on Ti thin films. Surface of the Mo layer is irradiated by sinusoidally intensity modulated heating laser. Temperature response at the heated area is measured by a probe laser beam with constant intensity, as a TR signal. Phase lag between the phase of TR signal and that of heating laser beam was obtained from 100 kHz to 2.6 MHz. To analyze thermal diffusivity of Ti thin films using the phase lag data, we developed a three-layer analytical model such as Mo coating (100 nm)∕thin film∕semi-infinite substrate. The calculated phase lag using analytical model is in good agreement with the experimental data for the whole frequency range. The thermal diffusivity of two Ti thin films is determined to be 5 × 10(-6) m(2)∕s, which is 53% of the bulk one.     

Spin‐coated epoxy resin embedding technique enables facile SEM/FIB thickness determination of porous metal oxide ultra‐thin films

A facile nonsubjective method was designed to measure porous nonconductive iron oxide film thickness using a combination of a focused ion beam (FIB) and scanning electron microscopy. Iron oxide films are inherently nonconductive and porous, therefore the objective of this investigation was to optimize a methodology that would increase the conductivity of the film to facilitate high resolution imaging with a scanning electron microscopy and to preserve the porous nature of the film that could potentially be damaged by the energy of the FIB. Sputter coating the sample with a thin layer of iridium before creating the cross section with the FIB decreased sample charging and drifting, but differentiating the iron layer from the iridium coating with backscattered electron imaging was not definitive, making accurate assumptions of the delineation between the two metals difficult. Moreover, the porous nature of the film was lost due to beam damage following the FIB process. A thin layer plastication technique was therefore used to embed the porous film in epoxy resin that would provide support for the film during the FIB process. However, the thickness of the resin created using conventional thin layer plastication processing varied across the sample, making the measuring process only possible in areas where the resin layer was at its thinnest. Such variation required navigating the area for ideal milling areas, which increased the subjectivity of the process. We present a method to create uniform thin resin layers, of controlled thickness, that are ideal for quantifying the thickness of porous nonconductive films with FIB/scanning electron microscopy.     

The impact of surface and retardation losses on valence electron energy-loss spectroscopy

The inelastic scattering of fast electrons transmitting thin foils of silicon (Si), silicon nitride (Si(3)N(4)), gallium arsenide (GaAs), gallium nitride (GaN) and cadmium selenide (CdSe) was analyzed using dielectric theory. In particular, the impact of surface and bulk retardation losses on valence electron energy-loss spectroscopy (VEELS) was studied as a function of the foil thickness. It is shown that for the materials analyzed, surface and retardation losses can cause a systematic, thickness-dependent modulation of the dielectric volume losses, which can hamper the determination of the bulk dielectric data as well as the identification of band-gap and interband transition energies by VEELS. For Si and GaAs, where the dielectric function is strongly peaked with high absolute values, retardation losses lead to additional intensity maxima in the spectrum. For thin films of these materials (below approximately 100 nm), the additional intensity maxima are related to retardation effects due to the finite size of the sample leading to the excitation of guided light modes. For thicker films, exceeding about 200 nm, the intensity maxima are caused by bulk retardation losses, i.e., Cerenkov losses. Although thickness-dependent modulations were observed for Si(3)N(4), GaN and CdSe, the form of the dielectric functions and their lower maxima, means that for TEM samples < 100 nm thick, the band-gap energies of these materials can be accurately identified by VEELS. Guidelines are given that allow for forecasting the impact of surface and retardation losses on VEELS.     

Confined fluid compressibility predicted using molecular dynamics simulation

Fluid compressibility is investigated using molecular dynamics simulation of three fluids with distinct molecular shapes confined to various film thicknesses and subject to a wide range of loads. The effects of film thickness and fluid structure are evaluated, and the simulated densities are compared to predictions of an empirical, bulk fluid compressibility model. Results show that thin films are less compressible than their bulk counterparts and that this difference is related to the effect of confinement on molecular ordering. Additionally, it is found that molecular dynamics simulation can predict bulk compressibility if the model film thickness is sufficiently large.     

Optimum film thickness of thin metallic coatings on silicon substrates for low load sliding applications

The frictional behaviour of thin metallic films on silicon substrates sliding against 52100 steel balls is presented. The motivation of this work is to identify an optimum film thickness that will result in low friction under relatively low loads for various metallic films. Dry sliding friction experiments on silicon substrates with soft metallic coatings (silver, copper, tin and zinc) of various thickness (1–2000 nm) were conducted using a reciprocating pin-on-flat type apparatus under a controlled environment. A thermal vapour deposition technique was used to produce pure and smooth coatings. The morphology of the films was examined using an atomic force microscope, a non-contact optical profilometer and a scanning electron microscope. Following the sliding tests, the sliding tracks were examined by various surface characterization techniques and tools. The results indicate that the frictional characteristics of silicon are improved by coating the surface with a thin metallic film, and furthermore, an optimum film thickness can be identified for silver, copper and zinc coatings. In most cases ploughing marks could be found on the film which suggests that plastic deformation of the film is the dominant mode by which frictional energy dissipation occurred. Based on this observation, the frictional behaviour of thin metallic coatings under low loads is discussed and friction coefficients are correlated with an energy based friction model.     

Determination of the composition and thickness of chromel and alumel thin films on different substrates by quantitative energy dispersive spectroscopy analysis

Thin films of two alloys (chromel and alumel), with thickness less than 100 nm, were obtained by plasma deposition technique, namely filtered cathodic vacuum arc (FCVA). The elemental analyses were performed by quantitative energy dispersive spectroscopy (EDS) microanalysis and Rutherford backscattering spectrometry (RBS). The applicability of EDS to such thin films as these was established by analysis of films deposited on substrates of different atomic numbers, specifically vitreous carbon, silicon, copper, and tin. We found that a substrate with atomic number similar to the mean atomic number of the film constituents is best for reliable EDS results, when compared to RBS. The compatibility between quantitative EDS measurements and RBS measurements, as well as comparison between the thin film elemental composition and the bulk material composition, was assessed by statistical analysis. Good consistency between EDS and RBS measurements was found for both chromel and alumel thin films when copper was used as substrate material. We observed severely overlapping peaks in the RBS output for the case of alumel films so that EDS analysis was crucial. We also compared thickness measurements determined by EDS and RBS, and we found good agreement for the case of alumel film on copper substrate, and 15% agreement for chromel film on copper substrate.     

Morphological properties of Ag₂SeTe nano thin films prepared by thermal evaporation

Semiconducting silver selenide telluride (Ag₂SeTe) thin films were prepared with different thicknesses onto glass substrates at room temperature using thermal evaporation technique. The structural properties were determined as a function of thickness by X‐ray diffraction exhibiting no preferential orientation along any plane; however, the films are found to have peaks corresponding to mixed phase. The morphology of these films was studied using scanning electron microscope and atomic force microscopy respectively, and is reported. The morphological properties are found to be very sensitive to the thin film thickness. The composition of the films is also estimated using energy dispersive analysis using X‐rays and are also reported.     

Numerical analysis of crater formation and ablation depth in thin silicon films heated by ultrashort pulse train lasers

This study numerically investigates the optical and heat transfer characteristics of thin silicon films irradiated by ultrashort (shorter than 10 ps) pulse train lasers. The one-dimensional two-temperature model (1DTTM) is extended to the two-dimensional (2DTTM) model for estimation of crater formation. In addition, the wave interference effects on the optical and energy transfer characteristics are considered to predict accurately the energy absorption rates in thin silicon films irradiated by picosecond-to-femtosecond pulse train lasers. Unlike bulk silicon, a significant change in energy absorption is found to occur in thin silicon films with the variation of film thickness due to the wave interference. The spatial distributions of energy carrier and lattice temperature show quite a different tendency at different pulse durations as well as the number of pulses because of significant changes in the optical and thermal properties. The predicted crater shapes and the ablation depths by 2DTTM are also presented.     

Image potential between closely separated quantum-size film and a metal

By theoretical analysis we have demonstrated that for degenerate films with a discrete electron energy spectrum (quantum-size (QS) films) the thickness dependences for the potential barrier height h(L) between a closely spaced QS film and a metal is quasi-oscillatory. This non-monotonic dependence of h(L) on the thickness d of the QS film, as well as the non-monotonic dependence of the main bulk characteristics of the QS film, can determine the dimensional dependence of the tunnel characteristics for spatially limited structures.     

Electron energy-loss spectroscopy study of thin film hafnium aluminates for novel gate dielectrics

We have used conventional high‐resolution transmission electron microscopy and electron energy‐loss spectroscopy (EELS) in scanning transmission electron microscopy to investigate the microstructure and electronic structure of hafnia‐based thin films doped with small amounts (6.8 at.%) of Al grown on (001) Si. The as‐deposited film is amorphous with a very thin (～0.5 nm) interfacial SiO_x layer. The film partially crystallizes after annealing at 700 °C and the interfacial SiO₂‐like layer increases in thickness by oxygen diffusion through the Hf‐aluminate layer and oxidation of the silicon substrate. Oxygen K‐edge EELS fine‐structures are analysed for both films and interpreted in the context of the films’ microstructure. We also discuss valence electron energy‐loss spectra of these ultrathin films.     

Contrast and quantitation in uniform regions of thin sections using transmission electron microscopy

A direct approach to quantitative measurements of uniform regions in thin sections is described. Accelerating voltages around 80 kV and objective aperture angles of about 9·3 mrad will provide conditions where contrast is directly proportional to specimen mass thickness. An extensive treatment of electron scattering in Formvar films for wide ranges of electron microscopic operating conditions is summarized in a simple, empirical equation. The extent to which Formvar results may be generalized to other materials, both embedding media and structures within the thin section, is treated. Using these results, precise measurements of local section thickness and of specimen density and/or dry mass of regions which penetrate the entire section thickness are possible, with the accuracy dependent upon irradiation effects and specimen makeup.     

石墨烯–铝复合冷板散热性能试验研究

传统散热冷板以铝合金为主,其导热能力有限且本身密度较大,已无法满足嵌入式计算机对高效散热及轻量化的需求。针对该问题,文中提出将具有超高导热性能的石墨烯散热片粘贴在铝合金表面得到石墨烯–铝复合冷板,以石墨烯–铝复合冷板代替传统散热材料的方法,并对不同厚度、不同功耗下的石墨烯–铝复合冷板的导热效果进行了试验研究。测试结果表明,在铝合金表面贴石墨烯散热片可保证在整体质量增加较小的情况下显著提高冷板的导热能力,在3 mm厚的铝合金表面粘接2 mm厚的石墨烯散热片时导热性能最佳,导热系数达到360 ~ 370 W/(m·K),而质量仅占6 mm厚铝板质量的66.5%。因此石墨烯–铝复合冷板可应用于高性能、高集成、小型化嵌入式计算机的散热设计。     

Specimen‐thickness effects on transmission Kikuchi patterns in the scanning electron microscope

We report the effects of varying specimen thickness on the generation of transmission Kikuchi patterns in the scanning electron microscope. Diffraction patterns sufficient for automated indexing were observed from films spanning nearly three orders of magnitude in thickness in several materials, from 5 nm of hafnium dioxide to 3 μm of aluminum, corresponding to a mass‐thickness range of ～5 to 810 μg cm^–2. The scattering events that are most likely to be detected in transmission are shown to be very near the exit surface of the films. The energies, spatial distribution and trajectories of the electrons that are transmitted through the film and are collected by the detector are predicted using Monte Carlo simulations.