A method for preparing cross sections of films on wear surfaces for transmission electron microscopy study

A method for preparing cross sections of surface layers which exist on bulk metal substrates for transmission electron microscopy (TEM) study is described. The surface layer or film is protected by a vacuum-deposited or sputtered coating of a suitable metal. A mask is placed over the surface and non-masked areas are subjected to ion beam etching until the substrate is exposed. A thick electroplated layer is then applied to the surface. This layer adheres well to the ion-etched substrate and seals the coated surface film against damage during the usual slicing and grinding steps which are required for the preparation from bulk materials of thin foils for TEM study. The method was developed specifically for the analysis of boundary and extreme pressure lubrication films on wear surfaces together with the near-surface region of the substrate. However, it is also applicable to the investigation of oxide, corrosion and other surface films.     

Prevention of fretting by ion plated film

A new technological application of the ion plating technique to the prevention of fretting has been studied. Ion plating was done using gold and silver, which are commonly employed as thin metal film lubricants and also boron carbide which has extremely good wear resistance. The anti-fretting property of the ion plated film was always superior to that of the sputtered or vacuum evaporated film. The ion plated boron carbide film showed the best resistance to fretting. The better adhesion of ion plated films was responsible for the better anti-wear property. Transmission electron microscopy was used to study ion plated films.     

Calculation of depth distribution functions in films using an electron scattering model

An electron scattering model which has proved reliable in predicting both characteristic and continuous radiation depth distributions in bulk samples is further developed to cope with the quantification of depth distribution curves in thin films. The validity of the extended model is checked by comprehensive comparisons of calculated emitted x-ray intensities with experimental data. The deviations obtained are generally small, the root-mean-square error being ～5%. The results of calculations quantifying the effect of the substrate material on the shape of the depth distribution function in the film are also presented. The curves obtained are discussed in light of known theories and of fundamental physical considerations. The new model generates curves which correspond at least qualitatively with what is to be expected from basic principles and with the results of recent Monte Carlo simulations.     

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.     

An investigation of the tribological properties of thin KCl films on iron in ultrahigh vacuum: modeling the extreme-pressure lubricating interface

The frictional properties of thin KCl films deposited onto clean iron are measured in ultrahigh vacuum using a tungsten carbide tribotip, where the observed initial rapid decrease in friction coefficient with film thickness is proposed to be due to the formation of a complete KCl monolayer where the friction coefficient of this film is ∼0.27. A 1800 Å thick KCl film shows a hardness and friction coefficient similar to those for bulk KCl when the width of the surface height distribution of the tribotip measured by atomic force microscopy (AFM) is 2000–3000 Å. This implies that the KCl film behaves like the bulk material when the film thickness exceeds the roughness of the interfaces.     

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.     

The effect of surface texturing on thin EHD lubrication films

Surface texturing has been successfully used for conformal contacts in many tribological applications in an effort to diminish friction and wear. However, the use of such a surface modifications are still in nascent as far as highly loaded contacts between non-conformal surfaces are concerned. It is mainly caused by the fact that the presence of such micro-features within these contacts can significantly influence the pressure distribution within the contact. Nevertheless, it has been shown in recent studies that the surface texturing can also have beneficial tribological effects if the depth of micro-features is properly designed. This paper is devoted to the experimental study of the effect of the micro-dents of various depths on thin lubrication films to find an experimental evidence of the micro-feature depth threshold for surface texturing applications in highly loaded non-conformal surfaces. The behaviour of an array of micro-dents within thin EHD contacts has been studied by thin film colorimetric interferometry. The influence of surface texturing on lubricant film formation has been observed under sliding/rolling conditions. The significant effect of micro-dents depth on lubricant film thickness is observed for positive slide-to-roll ratio when the disc is moving faster than the micro-textured ball. The presence of deep micro-dents within lubricated contact results in film thickness reduction downstream. As the depth of micro-dents is reduced, this effect diminishes and beneficial effect of micro-dents on film thickness formation has been observed. No significant influence of micro-dents depth on lubricant film shape has been observed in case of negative slide-to-roll conditions when micro-dents do not cause film thickness reduction regardless of their depths.     

Reconstruction of the electric charge density in thin films from the contrast transfer function measurements

The radial distribution of the beam-induced charge in thin films is investigated using the contrast transfer properties of the transmission electron microscope. The phase shift due to charging is measured as the phase difference between the contrast transfer functions of two photos taken with and without film at the back focal plane. Solving the inverse Laplace problem with this input data recovers the charge density of the measured film. The electric potential function in the whole area is reconstructed using the boundary integral method and the analytical solution of the Laplace equation for the electric potential is induced from unit step-wise surface charge. The phase shift of electron waves is derived in a weak lens approximation. In this way, the radial dependence of the charge density and the magnitude of the electrostatic potential at the thin film are obtained. The surface charge density reaches quasi-equilibrium state after the first 30 min of the electron beam pre-irradiation. The hydrocarbon contamination layer on the surface of the film is considered to be the main source of charging. An explanation of the qualitative behavior of the charge density, based on the contamination diffusion theory, is proposed.     

Femtosecond laser-induced simultaneous surface texturing and crystallization of a-Si:H thin film: morphology study

Hydrogenated amorphous silicon (a-Si:H) thin films have been considered for use in solar cell applications because of their significantly reduced cost compared with crystalline bulk silicon; however, their overall efficiency and stability are less than that of their bulk crystalline counterparts. Limited work has been performed on solving the efficiency and stability issues of a-Si:H simultaneously. Surface texturing and crystallization on a-Si:H thin film can be achieved through one-step femtosecond laser processing, which can potentially alleviate the disadvantages of a-Si:H in solar cell applications. In this study, submicrometer conical and pillar-shaped spikes are fabricated by irradiating a-Si:H thin films deposited on glass substrates with hundreds of 800 nm-wavelength, 130 fs-duration laser pulses in air, and water environments, respectively. The formation mechanisms for the surface spikes are discussed, and the differences in the surface feature characteristics are also presented and explained within the context of the different processing environments. The effect of laser processing on light absorption and crystallinity will be studied later.     

Influence of surface roughness features on mixed‐film lubrication

An optical technique (three‐dimensional spacer layer imaging) has been developed to map accurately lubricant film thickness in thin‐film elastohydrodynamic (EHD) contacts. This experimental technique has been used to study the influence of surface roughness features, asperity height, and slope on EHD film thickness and pressure. Single ridges transverse to the entrainment direction were used to represent asperities. It was found that the ridges with lower slopes generate films of greater minimum thickness. Below a certain entrainment speed, the minimum film thickness declined at a rate dependent on the ridge slope. At low speeds, the ridges with higher slopes entrapped a larger volume of lubricant ahead of the ridge and along the entrainment direction. For all speeds, the highest ridges entrapped the most lubricant. Both ridge slope and ridge height had a negligible effect on mean film thickness in the contact. Asperity pressure increased with higher ridge slope, but was not influenced by entrainment speed. An increase in pressure was found where lubricant is entrapped upstream of a ridge.     

Vacuum ellipsometry as a method for probing glass transition in thin polymer films

A vacuum ellipsometer has been designed for probing the glass transition in thin supported polymer films. The device is based on the optics of a commercial spectroscopic phase-modulated ellipsometer. A custom-made vacuum chamber evacuated by oil-free pumps, variable temperature optical table, and computer-based data acquisition system was described. The performance of the tool has been demonstrated using 20-200 nm thick poly(methyl methacrylate) and polystyrene films coated on silicon substrates at 10(-6)-10(-8) torr residual gas pressure. Both polymers show pronounced glass transitions. The difficulties in assigning in the glass transition temperature are discussed with respect to the experimental challenges of the measurements in thin polymer films. It is found that the experimental curves can be significantly affected by a residual gas. This effect manifests itself at lower temperatures as a decreased or even negative apparent thermal coefficient of expansion, and is related to the uptake and desorption of water by the samples during temperature scans. It is also found that an ionization gauge--the standard accessory of any high vacuum system--can cause a number of spurious phenomena including drift in the experimental data, roughening of the polymer surface, and film dewetting.     

Measurement of thermal properties of thin films up to high temperatures--pulsed photothermal radiometry system and Si-B-C-N films

A new arrangement of two-detector pulsed photothermal radiometry measurement system has been developed enabling temperature dependence measurement of thermal properties of thin films up to high temperatures. Only a few methods are available in this temperature range for thin films' thermal properties investigation, but there is a need for their knowledge in the fields of high-temperature electronics and high-speed machining. The present system enables simultaneous determination of the thin film effusivity, thermal conductivity, and volumetric specific heat in the temperature range from room temperature to 600?°C. The samples are placed in a vacuum chamber. The temperatures in the system were verified by an independent measurement and the system was tested on known bulk samples. Advantages and shortcomings of the method when used at higher temperatures and in the vacuum are described and discussed. Furthermore, Si-B-C-N thin films were studied. These amorphous ceramic materials possess an interesting set of mechanical and thermal properties. In particular, the films of the investigated chemical composition exhibit an excellent thermal stability at temperatures of up to 1700?°C. In the studied temperature range, from 20 to 600?°C, the thermal conductivity increased with increasing temperature from 1.72 to 1.89 W m(-1) K(-1) and volumetric specific heat increased from 2.65 to 3.76 × 10(6) J m(-3) K(-1).     

The Formation of Viscous Surface Films by Polymer Solutions: Boundary or Elastohydrodynamic Lubrication?

The film-forming properties of a range of polymer solutions have been studied down to very thin film thickness using ultrathin film interferometry.

It has been found that, at very slow rolling speeds, some polymers generate much thicker films than predicted from theory. It appears that these polymers form adsorbed layers between three and 15 nanometers thick on the two solid surfaces. These layers have a viscosity many times higher than that of the bulk solution. Therefore, under slow speed, low film thickness conditions, the contact effectively operates within a viscous boundary layer, generating an elastohydrodynamic-type film much thicker than predicted from the viscosity of the bulk lubricant. As the speed is raised the contact emerges from this boundary layer and reverts to elastohydrodynamic behavior based upon the viscosity of the bulk polymer solution.     

Particle-surface interaction in thin vitrified films for cryo-electron microscopy

The concentration of particles in thin vitrified films of suspensions is described as a function of various parameters such as the type of particles observed, the time the sample is left on the grid and the effect of different washing procedures. The thin films are prepared for cryo-electron microscopy by the classical, single-side blotting method or by blotting both sides of the grid simultaneously. The two-side blotting method gives the most faithful representation of the bulk solution. The single-side blotting method results in particles preferentially adsorbing to the non-blotted surface. This has the advantage that the concentration of particles in the thin vitrified film is higher than in the original suspension. The energy involved in adhesion of particles to the surface seems to be generally small. In most cases, it does not cause significant deformation of the particles or of the surface of the film. However, there are cases, as for example with lipid vesicles, where the particles are broken as a result of adsorption. Since particles remain adsorbed to the air-liquid interface, it is possible to wash or dialyse the solution directly on the grid with negligible loss of particles. This represents a very rapid and handy method for micro-dialysis. A thin film is then formed by blotting the specimen and vitrified by rapid cooling.     

Failure Mechanisms of CVD Diamond Wafers and Thin Films During Polishing

This article investigates the failure mechanisms of CVD diamond wafers and thin films during a fast dynamic friction polishing process. To explore the evolution of temperature and stress fields, a comprehensive finite element analysis was systematically carried out, with the aid of experimental examination. It was found that the discontinuity and sharp change of the stresses across the film-substrate interface causes debonding failure of a CVD diamond thin film specimen. In the case of a CVD diamond wafer, however, the high surface tensile stress and bulk bending is responsible for the cracking. It was concluded that specimen cracking is sensitive to the polishing pressure, and that the polishing window for the CVD thin films is smaller. Polishing time is a critical factor, because a longer time corresponds to a higher thermal stress. This article points out that using the combination of a smaller polishing load and a greater sliding speed is a good option in selecting polishing parameters. To minimize cracking, a stepwise polishing process can be used. With the proper parameters obtained in this study, very smooth, high-quality surfaces of CVD diamond wafers and thin films can be produced in a short polishing duration of minutes.     

A Surface Layer Model for Thin Film Lubrication

A rheological model has been developed which can be applied to thin film lubrication. It is known that great differences are seen between behavior in thin (molecular scale) films and in bulk (macroscopic) rheological measurements. There appear to be layers near the surface in which viscosity is increased by many orders of magnitude. The model contains three material property parameters, i.e., the conventional viscosity, the thickness of the surface layer, and a surface layer viscosity. A modified Reynolds equation is developed. Behavior of correction factors to Reynolds' equation and to the shear stress are shown. Results are computed for a one-dimensional converging wedge contact. The effect of increasing the layer thickness parameter is to increase the load and reduce the friction coefficient. Increasing the surface layer vicosity also tends to increase the load and reduce the friction coefficient.     

Maximum entropy reconstruction of compositional depth profiles from electron probe microanalysis data

Electron probe microanalysis (EPMA) is a powerful method for the quantitative determination of the elemental composition of micro-regions of a sample surface. Here, we report on the development of a method of reconstructing compositional depth profiles in thin films from EPMA data measured over a range of electron beam energies, using maximum entropy data processing. The method gives quantitative information on film compositions up to approximately 1 μm in depth, with a lateral spatial resolution of approximately 1 μm. The method is tested using both simulated data and measured experimental data from well-characterized model sample structures.     

Measurement of the refractive index dispersion of As2Se3 bulk glass and thin films prior to and after laser irradiation and annealing using prism coupling in the near- and mid-infrared spectral range

The prism coupling technique has been utilized to measure the refractive index in the near- and mid-IR spectral region of chalcogenide glasses in bulk and thin film form. A commercial system (Metricon model 2010) has been modified with additional laser sources, detectors, and a new GaP prism to allow the measurement of refractive index dispersion over the 1.5-10.6 μm range. The instrumental error was found to be ±0.001 refractive index units across the entire wavelength region examined. Measurements on thermally evaporated AMTIR2 thin films confirmed that (i) the film deposition process provides thin films with reduced index compared to that of the bulk glass used as a target, (ii) annealing of the films increases the refractive index of the film to the level of the bulk glass used as a target to create it, and (iii) it is possible to locally increase the refractive index of the chalcogenide glass using laser exposure at 632.8 nm.     

Direct and transmission milling of suspended silicon nitride membranes with a focused helium ion beam

Helium ion milling of suspended silicon nitride thin films is explored. Milled squares patterned by scanning helium ion microscope are subsequently investigated by atomic force microscopy and the relation between ion dose and milling depth is measured for both the direct (side of ion incidence) and transmission (side opposite to ion incidence) regimes. We find that direct-milling depth varies linearly with beam dose while transmission-milling depth varies with the square of the beam dose, resulting in a straightforward method of controlling local film thickness.     

A new shell casting process based on expendable pattern with vacuum and low-pressure casting for aluminum and magnesium alloys

A new shell casting process, with the adoption of the foam pattern of lost foam casting (LFC) as prototype and the combination of the thin shell fabrication technology of investment casting and vacuum and low-pressure casting process, was proposed for manufacturing complicated and thin-walled aluminum and magnesium alloy precision castings. Loose-sand uniting vacuum was used in the new process to further reinforce the thin shell, and the new process proves to be a process with simple process, low cost, and high thin shell strength. Because the molten metal filling and solidification are completed under air pressure and vacuum level, the filling capability and feeding capacity of the molten metal are greatly improved, and the castings become denser. This paper mainly investigated the fabrication technology of thin shell based on foam pattern prototype, the removing foam and roasting shell process and vacuum and low-pressure casting process. The few-layer compound thin shell of silica sol–sodium silicate was adopted for the new process. Removing foam pattern was carried out at 250°C for 30 min, and the shell was roasted at 800°C for 1 h. Combined with the vacuum and low-pressure casting process, this new shell casting process has successfully produced thin wall and complex aluminum and magnesium alloy parts with high quality. In addition, comparisons in terms of filling ability, microstructure, mechanical properties, porosity, and surface roughness among this new shell casting, gravity casting, and LFC were also made to show the characterization of this new shell casting process.