Failure of thin films: Optical shearography versus electrochemical impedance spectroscopy

In the present work, the temperature versus thermal deformation (strain) with respect to time, of different coating films, was studied by a non-destructive technique (NDT) known as shearography. An organic coating, i.e., ACE Premium Enamel, on a metallic alloy, i.e., a carbon steel, was investigated at a temperature range simulating the severe weather temperatures in Kuwait, especially between the daylight and the nighttime temperatures, 20-60 °C. The investigation focused on determining the in-plane displacement of the coating, which amounts to the thermal deformation (strain) with respect to the applied temperature range. Furthermore, the investigation focused on determining the thermal expansion coefficients of coatings, the slope of the plot of the thermal deformation (strain) versus the applied temperature range. In other words, one could determine, from the decreasing value of the thermal expansion coefficients of coatings, a critical (steady state) value of the thermal expansion coefficients of coatings, in which the integrity of the coatings can be assessed with respect to time. In fact, determination of the critical (steady state) value of the thermal expansion coefficients of coatings could be accomplished independent of parameters, i.e., ultraviolet (UV) exposure, humidity, and exposure to chemical species, which normally are considered in conventional methods of assessing the integrity of coatings. Furthermore, results of shearography indicate that the technique is a very useful NDT method not only to determine the critical value of the thermal expansion coefficients of different coatings but also to be used as a 2D-microscope for monitoring the deformation of the coatings in real time at a submicroscopic scale. Also, the obtained data of the shearography technique were compared with data obtained by electrochemical impedance spectroscopy (EIS) in an aqueous solution of 3% NaCl.     

Thermally induced deformations measured by shearography

In the present work, the thermo-mechanical behavior, temperature versus thermal deformation with respect to time, of different coating films were studied by a non-destructive technique (NDT) known as shearography. Organic coatings, i.e., Epoxy on metallic alloys, i.e., carbon steels, were investigated at a temperature range simulating the severe weather temperatures in Kuwait especially between the day-time and the night-time temperatures. The investigation focused on determining the in-plane displacement of the coatings, which amounts to the thermal deformation and stress with respect to temperature and time. Along with the experimental data, a mathematical relationship was derived describing the thermal deformation and stress of a coating film as a function of temperature. Furthermore, results of shearography indicate that the technique is a very useful NDT method not only for determining the thermo-mechanical behavior of different coatings but also can be used as a 2D microscope for monitoring the deformation of the coatings in real-time at a microscopic scale.     

Surface resistivity/conductivity of different organic-thin films by a combination of optical shearography and electrochemical impedance spectroscopy

Optical shearography and electrochemical impedance spectroscopy (EIS) were used for the first time to measure the surface resistivity/conductivity of different organic-thin films. Different organic coatings i.e., ACE Premium-gray, white, and beige Enamels (spray coatings), on a metallic alloy, i.e., a carbon steel, were investigated at a temperature range between 20–60 °C. The investigation focused on determining the in-plane displacement of the coatings with respect to the applied temperature range by optical shearography. Then, the AC impedance (resistance) of the same coated samples was determined by the technique of EIS in 3.5% NaCl solution at room temperature. In addition, a mathematical model was developed in order to obtain a proportionality constant (surface resistivity = ρ or conductivity = 1/ρ) between the determined AC impedance and the in-plane displacement. The obtained values of ρ of all investigated coatings, 0:25 × 10⁸–0:27 × 10¹⁰ Ωcm was found in the insulator range.     

Thermal stresses in box-type laser packages

The effect of Au coating on thermally induced stresses in box-type semiconductor laser packages was investigated by a finite-element method (FEM). The simulated results showed that Invar–Invar joints with Au coating have maximum stresses two times higher than joints without Au coating. This is due to the different coefficients of the thermal expansion (CTE) between dissimilar materials of Invar and Au, resulting in higher stresses. Maximum stresses were also found to be increased as the Au thickness increased. This effect is attributed to the increase in the thermal gradient in the welded region provided by the increased thermal conduction of the thicker Au coating layer. These results suggest that both the difference in CTE between dissimilar materials and higher thermal conduction of Au coating layer have an important impact on thermally induced stresses for optoelectronic packages having laser-welded Au coated materials.     

Microstructure and selected properties of hot-work tool steel with PVD coatings after laser surface treatment

The paper presents the effect of HPD laser treatment on the microstructure and selected properties of the PVD CrN, (Ti,Al) and Ti(C,N) coatings deposited onto hot-work tool steel substrates. The microstructure and surface topography of the investigated samples are characteristic of the diversified morphology connected with the applied laser beam power. Employment of laser beam at 0.7 kW power to the laser treatment of samples with Ti(C,N) coatings causes clear coating adhesion growth because of the diffusive processes induced by heat release. Because of the higher value of the (Ti,Al)N absorption coefficient one can state that the observed substrate materials change and finally coatings destruction in case of those samples is the most noticeable. The moderate effect of the laser beam treatment of the hot-work tool steel with the PVD coating was observed for CrN coatings. However, for laser beam power above 0.5 kW differences in the thermal expansion coefficients of the substrate materials and coatings generate coating crackings.     

Adhesive-free bonding of Zerodur glass to silicon

This work demonstrates anodic bonding of Zerodur glass having very low co-efficient of thermal expansion (CTE) to Si, Zerodur glass to thermally grown silicon dioxide on silicon and Pyrex glass to Ge. Bonding results, using point cathode contact and plate cathode contact configurations, are discussed. Bonding parameters, i.e. applied dc voltage, temperature and bonding time were determined. Heating and cooling rates for crack-free bonding of Zerodur glass were also determined.     

Control of the structure and stress state of thin films and coatings in the process of their preparation by ion-plasma methods

A system analysis of the influence of the substrate temperature during deposition on two main factors (nanodimensionality of structural aggregates and high stresses) responsible for the nonequilibrium state of the materials of ion-plasma-deposited films and coatings has been performed. It has been shown that an increase in the temperature during deposition leads to a preferred growth of nanocrystallites in the direction of incidence of film-forming particles, which, in turn, results in the formation of an anisometric crystal structure. The main causes of the generation of high elastic stresses in ion-plasma condensates are the ion/atom bombardment in the process of deposition (which stimulates the development of compressive stresses) and the difference in the thermal expansion coefficients of the condensate and substrate materials (which initiates the development of thermal stresses; the sign is determined by the difference between the thermal expansion coefficients of the condensate and substrate materials). An increase in the temperature during deposition results in the relaxation of compressive stresses stimulated by the ion/atom bombardment and in an enhancement of the influence of thermal stresses on the state of the ion-plasma condensate. This makes it possible to control the stress state of ion-plasma films and coatings by purposefully varying the substrate temperature during deposition.     

Antibacterial polymeric coatings grown by matrix assisted pulsed laser evaporation

We report on a simple and environmental friendly method to produce composite biocompatible antibacterial coatings consisting of silver nanoparticles (AgNPs, size 40 nm) combined with polymer blends (polyethylene glycol/poly(lactide-co-glycolide), PEG/PLGA blends). The PEG/PLGA&AgNPs coatings were produced by Matrix Assisted Pulsed Laser Evaporation, using a Nd:YAG laser with λ=266 nm. The AgNPs were deposited either on top of a PEG/PLGA layer (i.e., bilayered coating), or simultaneously with the polymers (i.e., blended coating). In both cases, chemical analysis indicated that the polymers preserved their integrity, with no evidence of chemical interaction with the AgNPs. Morphological investigations evidenced homogenous distribution of individual AgNPs on the surface of the coatings, with no signs of aggregation. The size of the AgNPs was ～40 nm, consistent with size of the as-received ones. The presence of AgNPs in the coatings was confirmed by the absorption band at ～420 nm and their stability was checked by monitoring this absorption versus time. After exposure to air, the AgNPs from the bilayered coating showed signs of oxidation. In the blended coating, the oxidation of the AgNPs was prevented by the neighboring polymer molecules. Finally, preliminary investigations confirmed the bacterial killing activity of the coatings against Escherichia coli.     

Temperature-dependent thermal expansion of cast and hot-pressed LAST (Pb–Sb–Ag–Te) thermoelectric materials

The thermal expansion for two compositions of cast and hot-pressed LAST (Pb–Sb–Ag–Te) n-type thermoelectric materials has been measured between room temperature and 673 K via thermomechanical analysis (TMA). In addition, using high-temperature X-ray diffraction (HT-XRD), the thermal expansion for both cast and hot-pressed LAST materials was determined from the temperature-dependent lattice parameters measured between room temperature and 623 K. The TMA and HT-XRD determined values of the coefficient of thermal expansion (CTE) for the LAST compositions ranged between 20 × 10^?6 K^?1 and 24 × 10^?6 K^?1, which is comparable to the CTE values for other thermoelectric materials including PbTe and Bi₂Te₃. The CTE of the LAST specimens with a higher Ag content (Ag_0.86Pb₁₉Sb_1.0Te₂₀) exhibited a higher CTE value than that of the LAST material with a lower Ag content (Ag_0.43Pb₁₈Sb_1.2Te₂₀). In addition, a peak in the temperature-dependent CTE was observed between room temperature and approximately 450 K for both the cast and hot-pressed LAST with the Ag_0.86Pb₁₉Sb_1.0Te₂₀ composition, whereas the CTE of the Ag_0.43Pb₁₈Sb_1.2Te₂₀ specimen increased monotonically with temperature.     

Thermodynamic and structural properties of polystyrene/C_(60) composites: A molecular dynamics study

To tailor properties of polymer composites are very important for their applications.Very small concentrations of nanoparticles can significantly alter their physical characteristics.In this work,molecular dynamics simulations are performed to study the thermodynamic and structural properties of polystyrene/C_(60)(PS/C_(60)) composites.The calculated densities,glass transition temperatures,and coefficient of thermal expansion of the bulk PS are in agreement with the experimental data available,implying that our calculations are reasonable.We find that the glass transition temperature Tg increases accordingly with an added concentration of C_(60) for PS/C_(60) composites.However,the self-diffusion coefficient D decreases with increase of addition of C_(60.)For the volumetric coefficients of thermal expansion(CTE) of bulk PS and ps/C_(60) composites,it can be seen that the CTE increases with increasing content of C_(60) above Tg(rubbery region).However,the CTE decreases with increasing content of C_(60) below Tg(glassy region).     

Graded finite element simulation of thermal stress in inhomogeneous high-Tc superconductor

YBa₂Cu₃O_y is an orthotropic material with different material properties in a, b and c directions, such as Young’s modulus, coefficient of thermal expansion (CTE), and thermal conductivity. It is assumed that the material properties of inhomogeneous high temperature superconductor (HTS) vary with different height coordinate and temperature. A model is presented in this paper to calculate the thermal stress of inhomogeneous HTS when temperature decreases from ambient to operating conditions (cryogenic temperatures). By fitting a second order polynomial to the experimental data, value of the material properties of inhomogeneous HTS can be obtained. Then, through the proposed graded finite element method, the coupled thermo-mechanical equations were solved numerically. The numerical results show that the temperature profiles distribute the function of time after soaking. It is notable that the temperature profile reaches steady in a very short period of time, so the thermal stress suddenly increases to a very high level for a bulk superconductor. It is also shown that the closer to the sample internal region it is, the larger the heat fluxes are. Besides, the maximum tensile stresses, i.e. the peeling stresses, occur near bottom corner of inhomogeneous HTS. It is intended that the model presented in this paper could be useful to researchers who are interested in mechanical properties of inhomogeneous HTS.     

Fe2-xYxMo3O12系列材料的相变及负膨胀性研究

本文对Fe2-xYx(MoO4)3(x=0.0,0.2,0.4,0.5,0.6,0.8,1.0,1.2,1.4,1.6,1.8,2.0)系列材料的相变及负膨胀性能进行了研究.通过对Fe2-xYx( MoO4)3系列材料的XRD和拉曼谱的分析发现,当x≤0.4时Fe2-xYxMo3O12在常温下是单斜结构;当x≥0.5时...     

Study of the multilayer PCB CTEs by moiré interferometry

Microelectronics packaging has been developing rapidly due to the demands for faster, lighter and smaller products. Printed circuit boards (PCBs) provide mechanical support and electrical interconnection for electronic devices. Many types of composite PCBs have been developed to meet various needs. Recent trends in reliability analysis of PCBs have involved development of the structural integrity models for predicting lifetime under thermal environmental exposure; however the theoretical models need verification by the experiment.

The objective of the current work is the development of an optical system and testing procedure for evaluation of the thermal deformation of PCBs in the wide temperature range. Due to the special requirements of the specimen and test condition, the existing technologies and setups were updated and modified. The discussions on optical methods, thermal loading chambers, and image data processing are presented. The proposed technique and specially designed test bench were employed successfully to measure the thermal deformations of PCB in the −40°C to +160°C temperature range. The video-based moiré interferometry was used for generating, capturing and analysis of the fringe patterns. The obtained information yields the needed coefficients of thermal expansion (CTE) for tested PCBs.     

Thermal Expansion and Deformation of Graphene

Taking into consideration short-atomic-range interactions and anharmonic effects,we calculate the thermal expansion coefficients,Gruneisen parameters,the elastic modulus of graphene varying with temperature and the phonon frequency.The anharmonic effects associated with the graphene deformation are also discussed.The results show that the value of thermal expansion coefficient is negative in the moderate temperature range,and it becomes positive when the temperature grows to be higher than a certain value.The change rate of elastic modulus with respect to temperature and pressure are calculated,and phonon frequencies are estimated.In the process of graphene thermal expansion,it is accompanied with the change of bond length and the rotation around the axis normal to the plane.Our results indicate that the effects due to the bond change are more significant than that of the rotation.We also show that if anharmonic effects are ignored,the thermal expansion coefficient and the Gruneisen parameters are zero,and the elastic modulus and the phonon frequency are constant.If anharmonic effects are considered up to the second term,these values will vary with temperature,and become closer to the experimental value.The higher the temperature is,the more significant the anharmonic effects become.     

Two-Point Correlations and Critical Line of the Driven Ising Lattice Gas in a High-Temperature Expansion

Based on a high-temperature expansion, we compute the two-point correlation function and the critical line of an Ising lattice gas driven into a nonequilibrium steady state by a uniform bias E. The lowest nontrivial order already reproduces the key features, i.e., the discontinuity singularity of the structure factor and the (qualitative) E dependence of the critical line. Our approach is easily generalized to other nonequilibrium lattice models and provides a simple analytic tool for the study of the high-temperature phase and its boundaries.     

Measurement of surface resistivity/conductivity of different organic thin films by a combination of optical shearography and electrochemical impedance spectroscopy

Shearography techniques were applied again to measure the surface resistivity/conductivity of different organic thin films on a metallic substrate. The coatings were ACE premium-grey enamel (spray coating), a yellow Acrylic lacquer, and a gold nail polish on a carbon steel substrate. The investigation was focused on determining the in-plane displacement of the coatings by shearography between 20 and 60 °C. Then, the alternating current (AC) impedance (resistance) of the same coated samples was determined by electrochemical impedance spectroscopy (EIS) in 3.0% NaCl solution at room temperature. As a result, the proportionality constant (resistivity or conductivity = 1/surface resistivity) between the determined AC impedance and the in-plane displacement was obtained. The obtained resistivity of all investigated coatings, 40:15 × 106–24:6 × 109Ωcm, was found in the insulator range.     

Near-zero thermal expansion of In_(2(1-x))(HfMg)_xMo_3O_(12) with tailored phase transition

Solid solutions of In_(2(1-x)(HfMg)_xMo_3O_(12) are synthesized by solid state reaction with the aim to reduce the phase transition temperature of In_2Mo_3O_(12) and improve its thermal expansion property.The effects of(HfMg)~(6+) incorporation on the phase transition and thermal expansion are investigated.It is shown that the monoclinic-to-orthorhombic phase transition temperature obviously decreases and the coefficient of thermal expansion(CTE) of the orthorhombic becomes less negative and approaches to zero with increasing the content of(HfMg)~(6+).A near zero thermal expansion covering the case at room temperature(RT) is achieved for the solid solutions with x ≥ 0.85,implying potential applications of this material in many fields.     

Critical Heat Flux for Downward Facing Boiling on a Coated Hemispherical Surface

An experimental study was performed to investigate the effect of surface coating on the critical heat flux for downward facing boiling on the outer surface of a hemispherical vessel. Steady-state boiling experiments were conducted in the subscale boundary layer boiling (SBLB) facility using test vessels with metallic microporous coatings to obtain the local boiling curves and the local critical heat flux (CHF) limits. Similar heat transfer performance was observed for microporous aluminum and microporous copper coatings. When compared to the corresponding data without coatings, the boiling curves for the coated vessels were found to shift upward and to the right. This meant that the CHF limit was higher with surface coating and that the minimum film boiling temperatures were located at higher wall superheats. In particular, the microporous coatings were found to enhance the local CHF values appreciably at all angular locations explored in the experiments. Results of the present study showed that the microporous aluminum coating was very durable. Even after many cycles of steady state boiling, the vessel coating remained rather intact, with no apparent changes in color or structure. Although similar heat transfer performance was observed for microporous copper coatings, the latter were found to be much less durable and tended to degrade after several cycles of boiling.     

A study of thermal parameters of Ag50Pd50 alloy using X-ray diffraction

Thermal parameters of Ag₅₀Pd₅₀ alloy were studied using the in-situ X-ray diffraction (XRD) technique. Diffraction experiments in the temperature range 308-1178 K showed that the alloy forms a face centered cubic (fcc; A1-type) structure. Temperature dependence of the lattice parameter was investigated using the Bragg line displacement method. Results show that the lattice parameter for the alloy increases with increase in temperature. The temperature dependent XRD data was utilized to determine the mean linear thermal expansion (MLTE (%)) and coefficient of thermal expansion (CTE) ‘α’ in the mentioned temperature range. It was observed that the values of CTE vary between 9.3 and 14.6 [K⁻¹][10⁻⁶]. The same data was also utilized to determine the Debye temperatures Θ_D and mean square amplitude of vibration (MSAV) (u²(T)) for this alloy. Values of thermal parameters as determined in this investigation are in good agreement with the estimated values as well as with those for other alloys of noble metals.     

光学薄膜样品的温度场和形变场分析

通过积分变换理论上求解了光学薄膜样品在脉冲或方波调制激励光作用下的热传导方程和热弹方程,从而获得了样品在瞬态和稳态情况下对应的温度场和形变场.为验证所求解,将理论解析解的计算机模拟结果与有限元的分析结果在时域和空间域进行了比较,两结果获得了较好的一致性;同时讨论了温度,热变形随激励光的调制频率、光斑半径等参数的变化.讨论了此模型在测量光学薄膜样品吸收损耗和表面热变形中的应用. 关键词： 温度场 形变场 表面热透镜 有限元