Removal of epoxy-attached thin sections from glass slides by plasma etching

Thin-sectioned samples mounted on glass slides with common petrographic epoxies cannot be easily removed (for subsequent ion-milling) by standard methods such as heating or dissolution in solvents. A method for the removal of such samples using a radio frequency (RF) generated oxygen plasma has been investigated for a number of typical petrographic and ceramic thin sections. Sample integrity and thickness were critical factors that determined the etching rate of adhesive and the survivability of the sample. Several tests were performed on a variety of materials in order to estimate possible heating or oxidation damage from the plasma. Temperatures in the plasma chamber remained below 138°C and weight changes in mineral powders etched for 76 hr were less than ±4%. A crystal of optical grade calcite showed no apparent surface damage after 48 hr of etching. Any damage from the oxygen plasma is apparently confined to the surface of the sample, and is removed during the ion-milling stage of transmission electron microscopy (TEM) sample preparation.     

Two new microscopical variants of thermomechanical modulation: scanning thermal expansion microscopy and dynamic localized thermomechanical analysis

We describe two ways in which thermomechanical modulation may be used in conjunction with scanning thermal microscopy, in order to distinguish between different components of an inhomogeneous sample. The sample is subjected to a modulated mechanical stress, and the heating is supplied locally by the probe itself.
Scanning thermal expansion microscopy is an imaging mode, in which an imposed localized temperature modulation is used to generate thermal expansion, which in turn produces mechanical strain and gives thermal expansion contrast images. We present results using two types of active thermal probe. For polymer/resin samples, the depth of material contributing to the measured thermal expansion is typically a few micrometres. Under certain conditions we observe a reversal in contrast as the frequency of the temperature modulation is increased.
In dynamic localized thermomechanical analysis, the modulated stress is applied directly, and accompanied by a localized temperature change, as used in other forms of localized thermal analysis. The resulting modulated lateral force signals are obtained. The glass transition of polystyrene is detected, and shows a significant variation with frequency. The amplitude or phase signal may be used to obtain image contrast for inhomogeneous samples.     

Measuring material softening with nanoscale spatial resolution using heated silicon probes

This article describes the use of heated silicon atomic force microscopy probes to perform local thermal analysis (LTA) of a thin film of polystyrene. The experiments measure film softening behavior with 100 nm spatial resolution, whereas previous research on LTA used probes that had a resolution near 10 microm, which was too large to investigate some types of features. This article demonstrates four methods by which heated silicon probes can perform thermal analysis with nanoscale spatial resolution. The polystyrene softening temperature measured from nanoscale LTA techniques is 120 degrees C, compared to 100 degrees C, measured with bulk ellipsometry. The discrepancy is attributed to the thermal contact resistance at the end of the silicon probe tip, on the order of 10(7)K/W, which modulates heat flow between the tip and sample and governs the fundamental limits of this technique. The use of a silicon probe for LTA enables bulk fabrication, parallelization for high-throughput analysis, and fabrication of a sharp tip capable of nanoscale spatial resolution.     

The thermal behavior of electrolyte-coated metal-foil dispersive electrodes

The thermal properties of electrolyte-coated aluminum (Al) and copper (Cu) foil dispersive electrodes carrying 700 mA of electrosurgical current for 1 min were studied on seven human subjects ranging in weight from 46 to 84 kg. Calibrated thermographic imaging was used for data analyses. The mean skin temperature rise for the Al-foil electrode was 1 degrees C and for the Cu-foil electrode was 0.5 degrees C. The maximum temperatures occurred at the perimeter of both electrode types and were 3.5 degrees C for the Al-foil and 2.5 degrees C for the Cu-foil electrode. Both electrodes performed adequately under these severe test conditions.     

Effects of the sample preparation temperature on the nanostructure of compression moulded ultrahigh molecular weight polyethylene

In this study, the effects of the sample sectioning temperature on the surface nanostructure and mechanical response of compression moulded ultrahigh molecular weight polyethylene (UHMWPE) at a nanometer scale (nanomechanical properties) have been characterized. The primary focus of this work was to determine if the sample sectioning temperature significantly changed the nanostructure of UHMWPE, while the secondary focus was to characterize the effect on the mechanical response due to the changes in the sectioned surface nanostructure. The goals of this study were: (a) to investigate the potential possibility of creating surface artefacts by the sample preparation technique by sectioning at different temperatures relative to the published range of glass transition temperatures, Tg, for PE (-12, -80 and -25 degrees C); (b) to determine the possibility of molecular orientation induced by plastic deformation of the UHMWPE sample during the process of sample preparation; (c) to measure the relative difference in nanomechanical properties owing to evolution of different nanostructures as a function of sample sectioning temperature. Field emission scanning electron microscopy (FESEM), atomic force microscopy (AFM) and nanoindentation were used to demonstrate that the sectioning temperature caused a change in nanostructure of the compression moulded UHMWPE sectioned surface, explaining the change in mechanical response to indentation at a nanoscale. In this study, it was demonstrated that significant plastic deformation occurs when a shear stress is applied between the glass or diamond blade and the UHMWPE during sample preparation under ambient conditions at a temperature of 22 degrees C. These results also suggest that an optimum sample sectioning temperature should definitely be below the measured Tg of the polymer.     

Experimental investigation of transient and thermal effects on lubricated non‐conformal contacts

In this work, thermal and transient effects on non‐conformal lubricated contacts are investigated through experimental analyses. Experiments between a ball and a plane surface of a disc are described. Friction coefficients and film thicknesses are measured (the film thickness only for the glass‐on‐steel contact). A paraffin base mineral oil is used as a lubricant. First experiments are carried out under steady‐state conditions. To include effects due to different thermal properties of contacting materials, a steel‐on‐steel and a glass‐on‐steel contact with different slide‐to‐roll ratios are tested. If the contacting materials have different thermal properties, as in the case of a glass‐on‐steel contact, thermal effects like the temperature–viscosity wedge action could clearly be shown. It is found that the friction coefficients are influenced by the slide‐to‐roll ratio and the thermal properties of the contacting materials. Under transient conditions, the entraining velocity is varied with a sinusoidal law. Squeeze effects explain ‘loops’ of friction and film thickness found also in previous works. The formation of friction loops is related to the measured film thickness differences. However, also under non‐steady‐state conditions, thermal effects, like the temperature–viscosity wedge action, influence the friction coefficients. Copyright © 2007 John Wiley & Sons, Ltd.     

Beam heating of a moderately thick cold stage specimen in the SEM/STEM

A mathematical model for the electron beam heating problem of thick specimens (thickness less than the electron range) in the cold stage of SEM/STEM is proposed, and an analytic solution for the problem is provided. The use of the model is demonstrated by calculating the maximum temperature rise in a red blood cell mounted on a metallized polymer film, for a large range of operating conditions. With a probe size of 20 nm and probe current of less than 10 nA the temperature rise was found to be on the order of 5 K. This temperature rise increases proportionally to the probe current if all other variables are kept constant. Although the amount of energy dissipated in thick specimens is large relative to thin films, temperature rise can be minimized by mounting the thick sample on a metal stub or on a metallized film thus providing large heat transfer area through a high thermal conductivity substrate. Of course our calculations only have meaning if the specimen is in good thermal contact with the underlying support.     

Spatially and temporally resolved thermal imaging of cyclically heated interconnects by use of scanning thermal microscopy

A scanning thermal microscope with a Wollaston probe was used to investigate the spatial distribution and temporal variation of temperature in interconnect structures subjected to thermal cycling. The probe, utilized in passive temperature sensing mode, was calibrated from 20 degrees C to 200 degrees C using a single-layer aluminum microdevice. Spatial measurements were performed on nonpassivated aluminum interconnects sinusoidally heated by a 6 MA/cm(2) current at 200 Hz. The interconnects were determined to have temperatures that decreased with position from a maximum located at the center of both the interconnect length and width. Time-resolved temperature measurements were performed on the same structures sinusoidally heated by a 6 MA/cm(2) current at 2 Hz. Both the peak-cycle temperature and average-cycle temperature were found to decrease with increasing distance from the center of the width of the interconnects.     

Development of thermal models of footwear using finite element analysis

Thermal comfort is increasingly becoming a crucial factor to be considered in footwear design. The climate inside a shoe is controlled by thermal and moisture conditions and is crucial to attain comfort. Research undertaken has shown that thermal conditions play a dominant role in shoe climate. Development of thermal models that are capable of predicting in-shoe temperature distributions is an effective way forward to undertake extensive parametric studies to assist optimized design. In this paper, two-dimensional and three-dimensional thermal models of in-shoe climate were developed using finite element analysis through commercial code Abaqus. The thermal material properties of the upper shoe, sole, and air were considered. Dry heat flux from the foot was calculated on the basis of typical blood flow in the arteries on the foot. Using the thermal models developed, in-shoe temperatures were predicted to cover various locations for controlled ambient temperatures of 15, 25, and 35 degrees C respectively. The predicted temperatures were compared with multipoint measured temperatures through microsensor technology. Reasonably good correlation was obtained, with averaged errors of 6, 2, and 1.5 per cent, based on the averaged in-shoe temperature for the above three ambient temperatures. The models can be further used to help design shoes with optimized thermal comfort.     

Modeling high-temperature glass molding process by coupling heat transfer and viscous deformation analysis

Glass molding is as an effective approach to produce precision micro optical elements with complex shapes at high production efficiency. Since glass is deformed at a high temperature where the mechanical and optical properties depend strongly on temperature, modeling the heat transfer and high-temperature deformation behavior of glass is an important issue. In this paper, a two-step pressing process is proposed according to the non-linear thermal expansion characteristics of glass. Heat transfer phenomenon was modeled by considering the temperature dependence of specific heat and thermal conductivity of glass. Viscosity of glass near the softening point was measured by uniaxially pressing cylindrical glass preforms between a pair of flat molds using an ultraprecision glass molding machine. Based on the numerical models and experimentally measured glass property, thermo-mechanical finite element method simulation of temperature rise during heating and material flow during pressing was carried out. The minimum heating time and pressing load changes were successfully predicted.     

A piezo-thermal probe for thermomechanical analysis

Thermomechanical analysis (TMA) is widely used to characterize materials and determine transition temperatures and thermal expansion coefficients. Atomic-force microscopy (AFM) microcantilevers have been used for TMA. We have developed a micromachined probe that includes two embedded sensors: one for measuring the mechanical movement of the probe (deflection) and another for providing localized heating. The new probe reduces costs and complexity and allow for portability thereby eliminating the need for an AFM. The sensitivity of the deflection element ((ΔR∕R)∕deflection) is 0.1 ppm∕nm and its gauge factor is 3.24. The melting temperature of naphthalene is measured near 78.5 °C.     

Compact cantilever force probe for plasma pressure measurements

A simple, compact cantilever force probe (CFP) has been developed for plasma pressure measurements. It is based on the pull-in phenomenon well known in microelectromechanical-system electrostatic actuators. The probe consists of a thin (25 mum) titanium foil cantilever (38 mm of length and 14 mm of width) and a fixed electrode separated by a 0.75 mm gap. The probe is shielded by brass box and enclosed into boron nitride housing with a 9 mm diameter window for exposing part of cantilever surface to the plasma. When the voltage is applied between the cantilever and the electrode, an attractive electrostatic force is counterbalanced by cantilever restoring spring force. At some threshold (pull-in) voltage the system becomes unstable and the cantilever abruptly pulls toward the fixed electrode until breakdown occurs between them. The threshold voltage is sensitive to an additional externally applied force, while a simple detection of breakdown occurrence can be used to measure that threshold voltage value. The sensitivity to externally applied forces obtained during calibration is 0.28 V/microN (17.8 VPa for pressure). However, the resolution of the measurements is +/-0.014 mN (+/-0.22 Pa) due to the statistical scattering in measured pull-in voltages. The diagnostic temporal resolution is approximately 10 ms, being determined by the dynamics of pull-in process. The probe has been tested in the tokamak ISTTOK edge plasma, and a plasma force of approximately 0.07 mN (plasma pressure approximately 1.1 Pa) has been obtained near the leading edge of the limiter. This value is in a reasonable agreement with the estimations using local plasma parameters measured by electrical probes. The use of the described CFP is limited by a heat flux of Q approximately 10(6) W/m(2) due to uncontrollable rise of the cantilever temperature (DeltaT approximately 20 degrees C) during CFP response time.     

Direct continuous measurements of thermal expansion coefficients of liquids and solids using flow microcalorimetry

A differential heat capacity flow microcalorimeter is used to monitor in a continuous mode the thermal expansion of a sample during a programmed temperature scan. The sample may consist of liquids, suspensions, or bulk solids in a confining liquid and the typical temperature scanning rate is of the order of 1 K/min. The technique has a precision better than 1% and a detection limit of 10(-6) ml s(-1). In contrast to conventional dilatometers, this technique offers variable sensitivity and is not limited by the magnitude of the total volume change during the experiment. Various expansibility data obtained in the temperature range 10-55 degrees C are reported for several systems, namely water, benzene, carbon tetrachloride, and aqueous solutions of sodium chloride. The volume changes for the thermal transition of Teflon and the phase separation of 2-butoxyethanol/water mixtures further illustrate the possibilities of this new technique.     

基于红外锁相法的热波检测技术及缺陷深度测量-1

红外锁相法热波检测技术（Lock-in Thermography）是一种基于热波处理的主动式红外热成像检测技术,适用于复合材料及复杂结构构件的无损检测,已广泛应用于航天航空、汽车、机械、电力等领域。本文着重介绍了阐述了红外锁相法热波检测技术的原理、缺陷深度测量及在蜂窝夹层结构及焊接构件检测中的应用。采用有限差分法计算了强度按正弦规律变化热流引起试件表面温度变化历程,并采用锁相法提取了有缺陷与无缺陷处的稳态温度变化和计算二者相位差,与试验结果接近。建立了热波在试件中传导的热—电等效模型,利用该模型对红外锁相法热波检测技术进行了仿真研究,得到了缺陷深度和反射热波与入射热波相位差之间的关系,该模型计算结果与试验结果基本一致。采用红外锁相法热波检测技术对模拟缺陷的蜂窝夹层结构试件和实际的焊接构件进行了无损检测试验研究,结果表明,采用红外锁相法热波检测技术能够快速、准确的获得缺陷大小、位置等,该技术对具有复杂曲面结构的构件也十分优越。     

Numerical analysis of flow distribution for combined weapon system in environmental tester

Thermal behaviors of combined weapon systems were analyzed by developed computational programs in this study. Also, temperature distributions of the materials of the system were measured according to the experimental conditions. Field tests that reflected the calculated thermal flow characteristics and the measured temperature distributions of the materials were prepared in a large environmental tester for the weapon systems. Boundary conditions of the analysis were the inlet and outlet conditions of the environmental tester and the low temperature limit of ?32°C. The soaking time of the system, including a fuel tank and a battery in the environmental tester, was obtained by the programs developed in this study to carry out the experiment in the predicted conditions.     

The measurement of thermal conductivity variation with temperature for solid materials

An apparatus was designed to routinely measure the thermal conductivity variation with temperature for solid materials. The apparatus was calibrated by measuring the thermal conductivity variations with temperature for aluminum, zinc, tin and indium metals. The variations of thermal conductivity with temperature for the Zn-[x] wt.% Sb alloys (x = 10, 20, 30 and 40) were then measured by using the linear heat flow apparatus designed in present work. From experimental results it can be concluded that the linear heat flow apparatus can be used to measure thermal conductivity variation with temperature for multi component metallic alloys as well as pure metallic materials and for any kind of alloys. Variations of electrical conductivity with temperature for the Zn-[x] wt.% Sb alloys were determined from the Wiedemann–Franz (W–F) equation by using the measured values of thermal conductivity. Dependencies of the thermal and electrical conductivities on composition of Sb in the Zn–Sb alloys were also investigated. According to present experimental results, the thermal conductivity and electrical conductivity for the Zn-[x] wt.% Sb alloys decrease with increasing the temperature and the composition of Sb.     

Local beam heating in metallic electron microscope specimens

A very sensitive method is described to measure the local rise in the temperature of a metal specimen during investigation in the electron microscope. The method is based on the known temperature dependence of the climb rate of Frank dislocation loops in materials with relatively high stacking fault energy. The climb rate of loops subject to the influence of the condensed electron beam is compared to the corresponding rate for loops in an area of the same specimen which is remote from the observation spot. From the difference in the logarithms of these rates the amount of local beam heating is determined. For a typical Al-1.5 wt% Mg specimen under typical normal working conditions an average local rise in temperature of approximately 6°C was determined.     

A simple method for depositing thin films on the surface of transmission electron microscope specimens

Thin-film deposition on already thinned transmission electron microscope (TEM) samples is generally difficult as these samples are often small and fragile. To overcome this difficulty, we have developed a new method for depositing thin films of practically any material onto TEM samples using an ion-milling machine. This principle utilizes the fact that an ion-milling machine can be used not only for removal but also for deposition of materials. Fine-grained thin films were found to grow on TEM samples by this method.     

Sheathed probe thermal gas mass flow meter heat transfer analysis

The thermal gas mass flow meter is an important meter used in industrial measurement. When the environmental temperature changes, the measured gas physical parameters change correspondingly and the thermal gas mass flow meter output signal is affected, causing large measurement error. The influence of gas temperature on the sheathed probe measurements is analyzed in this paper based on experiments and heat transfer theory using a three dimensional probe and gas heat transfer mathematical model based on the heat conduction equation. The probe heat transfer process is analyzed under convection heat transfer coupling conditions. The experimental data were analyzed and compared against the theoretical results, with a maximum average relative error of only 4.56%. The rationality of the theoretical method is thus verified.