Effects of low and high temperatures on tensile behavior of adhesively-bonded GFRP joints

The tensile behavior of adhesively-bonded double-lap joints composed of pultruded glass fiber-reinforced adherends and an epoxy adhesive was investigated under temperatures ranging between −35 °C and 60 °C. The load–elongation response was influenced primarily by the thermomechanical behavior of the adhesive and much less so by that of the adherends. For temperatures above the adhesive glass transition temperature, strength and stiffness decreased with the former being less affected than the latter. The failure mechanism changed with increasing temperature from fiber-tear to adhesive failure. The crack initiation loads were unaffected as long as the temperature remained below the adhesive glass transition temperature. However, the crack propagation rate was higher at low temperatures. Critical strain energy release rates for crack initiation and propagation consistently rose as temperature increased. Modeling results obtained using existing empirical models and FEA compared well to the experimental data in the examined temperature range.     

Reliability assessment of indium solder for low temperature electronic packaging

Indium is the choice of material for cryogenic joining applications. It is superior under repeated wide temperature excursions including extreme cold temperatures (below −55 °C) because of its excellent electrical conductivity and ductility at cryogenic temperatures. In particular, it is being considered for die/substrate attaches in low temperature SiGe BiCMOS modules for Martian and Lunar exploration. An efficient and systematic assessment was conducted to evaluate the reliability of indium solder under thermal fatigue and extended cold temperature mechanical fatigue conditions encountered in space exploration missions. In addition, fatigue failure sites, modes and mechanisms in indium solder at low temperature were investigated. A fatigue model was also calibrated for indium solder joint at cryogenic temperatures.     

Thermo-mechanical characterisation of AA 6056-T4 and estimation of its material properties using Genetic Algorithm

This paper presents an experimental investigation of thermo-mechanical material properties of AA 6056-T4, which is used extensively in aeronautic applications. Monotonic tensile tests have been carried out on the dog-bone type specimens at temperatures ranging from room temperature (16 °C) to high temperature (450 °C) with two different strain rates; viz. high strain rate (∼0.002 s⁻¹) and low strain rate (∼0.0002 s⁻¹). Specimens were heated with the help of Joule heating system using Gleeble® 3500 machine at a temperature rate of 25 °C/s. Material properties which were investigated include the Young’s modulus, yield strength at 0.1% plastic strain and hardening modulus.     

Delamination and kink-band failure of pultruded GFRP laminates under elevated temperatures and compression

Compression experiments were conducted on slender glass fiber-reinforced polymer (GFRP) laminates at different temperatures in the elevated range. Experimental buckling loads, lateral second-order deformations, and shear strength decreased with increasing temperature until stable values were reached at a much lower level in the leathery material state. The resin-dominated bending stiffness decreased at a higher rate than the fiber-dominated compressive stiffness. Global buckling followed by a delamination failure during the post-buckling process was observed for temperatures below 180 °C, while pre-buckling kink-band failure occurred when the temperature increased to 220 °C. Recently proposed thermomechanical models were further validated and enabled the changing failure mode and associated Tresca and kink-band shear stress and strength conditions to be modeled.     

A study of frequency and temperature effects on fatigue crack growth resistance of CPVC

Excellent corrosion resistance of chlorinated polyvinyl chloride (CPVC) makes it an attractive material for piping systems carrying corrosive materials. The relatively high glass transition temperature of CPVC has increased its use in hot water distribution. Establishing a relationship that describes the effect of test frequency on fatigue crack propagation (FCP) rate of polymers is an interesting challenge. FCP rates can decrease increase or remain constant with increasing test frequency. Moreover, FCP sensitivity to frequency of some polymers is known to be dependent on test temperature. In this study, fatigue crack propagation in a commercial grade chlorinated vinyl chloride (CPVC) over the frequency and temperature ranges of 0.1-10 Hz and −10 °C to 70 °C, respectively, was investigated. FCP tests were conducted on single edge notch (SEN) specimens prepared from 100-mm injection molded CPVC pipefittings. The crack growth rate (da/dN) was correlated with the stress intensity range ΔK. The FCP rate was found to be insensitive to frequency at sub room temperatures. The fatigue crack propagation resistance of CPVC was enhanced with increasing cyclic frequency at 50 and 70 °C. Frequency effect on FCP rate was found to be higher in the low frequency range.Macro-fractographic analysis of fracture surface showed that stepwise crack propagation existed at 0.1 and 1 Hz for all temperatures of interest.     

The preparation and performance of a novel room-temperature-cured heat-resistant adhesive for ceramic bonding

A novel adhesive for joining ceramic materials was made using silicon-epoxy interpenetrating polymer networks (IPNs) as matrix (based on silicon resin (SR) and diglycidyl ether of bisphenol A (DGEBA) epoxy resin (EP)), γ-glycidoxypropyltrimethoxysilane (γ-GPS) as cross-linking agent, dibutyltin dilaurate (DBTDL) as catalyst, Al, low melting point glass (GP) and B₄C powders as inorganic fillers, low molecular polyamide (LMPA 650) as curing agent. The character and heat-resistance property of the IPNs and adhesive were tested by FT-IR, DSC and TG. The compressive shear strength of ceramic joints was investigated at different temperatures in atmosphere surroundings. The modification mechanism of inorganic fillers was studied using XRD. Results showed that the IPNs were a homogeneous morphology of inter-crosslinked network structure with single T_g. The adhesive could be cured at room temperature with good heat-resistance property due to the chemical bond of epoxy group and Si-O-Si. The optimum compressive shear strength (9.44 MPa at 1000 °C) occurred at SR/EP ratio: 9/1, content of KH560: 2%, Al/GP/B₄C ratio: 3.2/4/3, fillers/IPNs ratio: 6/4. The adhesive had good heat-resistance property with 10% weight loss at 435 °C. Failure mode of joint was mixing failure due to the high chemical bonding force.     

Effect of temperature and hold time on internal hardening behavior of a near α titanium alloy under cyclic deformation

In the present work, the study of dynamic strain aging (DSA) in near α titanium alloy Timetal 834 is reported in terms of internal hardening variables (kinematic and isotropic hardening variable). Total strain controlled low cycle fatigue tests have been conducted in air at 300 °C and from 400 °C to 500 °C at a temperature interval of 25 °C at nominal strain rates of 6.67 × 10⁻³ s⁻¹. The alloy exhibits gradual cyclic softening till failure at 300 °C, whereas, it exhibits initial cyclic softening followed by marked cyclic hardening from 400 °C to 500 °C. The cyclic hardening is attributed to DSA phenomena, resulting due to increase in isotropic stress component. The observed maximum peak stress ratio, lower fatigue life and minimum half-life plastic strain range at 450 °C indicates the maximum effect of DSA at that temperature. The fatigue life of tensile and compressive hold at 450 °C was observed to be inferior as compared to pure fatigue tests.     

The influence of dynamic strain aging on resistance to strain reversal as assessed through the Bauschinger effect

The Bauschinger effect of three commercially produced medium carbon bar steels representing different microstructural classes with similar tensile strengths and substantially different yielding and work-hardening behaviors at low-strain was evaluated at room temperature and in situ at temperatures up to 361 °C. The influence of deformation at dynamic strain aging temperatures as a means to produce a more stable dislocation structure was evaluated by measuring the resistance to strain reversal during in situ Bauschinger effect tests. It was shown that the three medium carbon steels exhibited substantial increases in strength at dynamic strain aging temperatures with the peak in flow stress occurring at a test temperature of 260 °C for an engineering strain rate of 10⁻⁴ s⁻¹. Compressive flow stress data following tensile plastic prestrain levels of 0.01, 0.02 and 0.03 increased with an increase in temperature to a range between 260 °C and 309 °C, the temperature range where dynamic strain aging was shown to be most effective. The increased resistance to flow on strain reversal at elevated temperature was attributed to the generation of more stable dislocation structures during prestrain. It is suggested that Bauschinger effect measurements can be used to assess the potential performance of materials in fatigue loading conditions and to identify temperature ranges for processing in applications that utilize non-uniform plastic deformation (e.g. shot peening, deep rolling, etc.) to induce controlled residual stress fields stabilized by the processing at temperatures where dynamic strain aging is active.     

Damage modeling of carbon-fiber reinforced polymer composite pin-joints at extreme temperatures

A novel finite element based framework was developed to study the effect of extreme temperatures on damage progression in carbon-fiber reinforced composite pin-joints. A progressive damage method that incorporated Hashin-type damage criteria was implemented in the model. Temperature dependent material properties were used to create three material models with properties corresponding to ambient temperatures −55 °C, 20 °C and 82 °C. At −55 °C ambient temperature, joint strength was reduced 8.6% as the relaxation temperature was varied from 20 °C to 100 °C. At 82 °C ambient temperature, joint strength was reduced 3.6% as the relaxation temperature was varied from 20 °C to 100 °C. The model showed that increasing the relaxation temperature decreased the joint strength and increased the matrix tensile damage rate but did not greatly affect other failure modes.     

Synthesis and dielectric characterization of Ba0.6Sr0.4TiO3 ferroelectric ceramics

Ferroelectric ceramics Ba_0.6Sr_0.4TiO₃ (BST 40) were prepared, by solid-state reaction in the temperature range 1210-1450 °C. Maximum values of the ceramic densities were around 94% of their theoretical value. X-ray diffraction techniques (XRD) and scanning electron spectroscopy (SEM) were used to analyze the structure and the surface morphology of ceramics. Rounded, well defined or abnormal granular growth was observed in the SEM images, vs. sintering conditions and purity of the raw materials. In all samples, BST 40 ceramic is the major phase, but there are also present small amounts of secondary phases, as revealed in XRD diffraction patterns. Permittivity and dielectric loss measurements were performed in the temperature range − 150 to + 150 °C, and 150 Hz-5 MHz frequency values. Permittivity values rising from 1200 to 12,500, with increasing sintering temperatures, were recorded. Narrow and well defined transition peaks were noticed at higher sintering temperatures. Curie temperature was around 2 °C, for samples with the mentioned composition. Permittivity and losses vs. frequency show different behavior whether BST ceramics are in polar or non-polar state and with the distance toward phase transition. Microwave measurements performed at room temperature have shown lower values of permittivity, compared with similar data at low frequency, and dielectric losses lower than 1% at 0.7 GHz. The sintering conditions (temperatures, sintering time, etc.) and purity of the raw materials lead to important changes of transition temperatures in the polymorphic diagram, which we have built—for the other Ba1−xSrxTiO3 compositions (x = 0.25-0.90) sintered at 1260 °C for 2 h.     

Damage evolution and characterisation of crack types in CF/EP laminates loaded at low temperatures

Tensile testing of CF/EP AS4/8552 cross-ply laminates at room (RT) and cryogenic (around −150 °C) temperatures has been performed to study the effect of temperature on damage (intralaminar cracking) evolution. Microscopy studies of the specimen edges showed a significant difference in damage pattern for the two different temperatures. At the low temperature (LT), more complex crack types were obtained that could not be found in specimens tested at the RT. The effect of these crack types on the laminate tensile modulus was studied by FEM. In analytical stiffness modelling complex shape crack was replaced by an “effective” normal (straight) crack with an “effective” crack opening displacement (COD) that leads to the same reduction in laminate stiffness. A crack efficiency factor was introduced to characterize the significance of complex crack shapes for stiffness reduction. The reduction of tensile modulus for a laminate damaged at low temperature was measured and compared with model predictions.     

On the fatigue small crack behaviors of directionally solidified superalloy DZ4 by in situ SEM observations

Small fatigue crack behaviors in a nickel-based directionally solidified superalloy DZ4 were studied by in situ Scanning Electron Microscopy. The crack initiation and propagation manners were identified under different temperatures, i.e. 25 °C, 350 °C, 700 °C. Fatigue crack growth occurred preferentially along slip bands at 25 °C and 350 °C but by Mode-I type at 700 °C. The crack growth rate generally increased with temperature, especially between room temperature and 350 °C. The anomalous small crack growth was analyzed by in situ examining the effect of microstructure. The small cracks were found to be primarily microstructurally small and secondly mechanically small.     

Delamination failure of multilaminated adhesively bonded joints at low temperatures

A series of experimental investigations of multilaminated joints adhesively bonded by epoxy/polyurethane (PU) glue were conducted in order to examine the delamination failure characteristics under in-plane shear loading at low temperatures. In order to observe these phenomena, a series of lap-shear tests were carried out at various low temperatures (20 °C, −110 °C and −163 °C) and various adhesion areas (15 mm × 50 mm, 30 mm × 50 mm, 50 mm × 50 mm, 75 mm × 50 mm and 100 mm × 50 mm). The test results were used to investigate the delamination and material characteristics, as well as the material properties, e.g., ultimate shear stress and shear elongation. Furthermore, the dependencies of the characteristics of multilaminated adhesively bonded joints (MABJs) on temperature and adhesion area was analyzed using the stress–strain relationship, and closed form formulas that are functions of the dependent parameters are proposed.     

Time-dependent behaviour of steel/CFRP double strap joints subjected to combined thermal and mechanical loading

Degradation of structural adhesives at elevated temperatures makes the time-dependent behaviour of adhesively-bonded steel/CFRP joints a critical issue for safety considerations of CFRP strengthened steel structures. This paper reports the examination of specimens at different load levels (i.e. 80%, 50%, and 20% of their ultimate load measured at room temperature) and constant temperatures from 35 °C to 50 °C (i.e. temperatures below and above the glass transition temperature T_g, 42 °C of the adhesive). Furthermore, a scenario of cyclic thermal loading between 20 °C and 50 °C was included to represent more realistic exposure. Joint time-dependent behaviour was demonstrated by the stiffness and strength degradation as a function of not only temperature but also time. At the same temperature level close to or above T_g, a higher load level corresponded to a shorter time-to-failure. In addition, up to 47% of strength recovery was found for the specimens subjected to cyclic temperatures compared with those under constant 50 °C which failed at the same load level. Based on the proposed temperature and time-dependent material property models, the time-dependent failure time of steel/CFRP double strap joints was well described and validated by the experimental results.     

Microwave dielectric properties and microstructures of CuO- and ZnO-doped LaAlO3 ceramics

The microwave dielectric properties and the microstructures of 0.25 wt.% CuO-doped LaAlO₃ ceramics with ZnO additions have been investigated. The sintered LaAlO₃ ceramics are characterized by X-ray diffraction spectra and scanning electron microscopy (SEM). Tremendous reduction in sintering temperature can be achieved with the addition of sintering aids CuO and ZnO. The ceramic samples show that dielectric constants (ε_r) of 22−24 and Q×f values of 33,000−57,000 (at 9.7 GHz) can be obtained at low sintering temperatures 1340−1460°C. The temperature coefficient of resonant frequency varies from −24 to −48 ppm/°C. At the level of 0.25 wt.% CuO and 1 wt.% ZnO additions, LaAlO₃ ceramics possesses a dielectric constant (ε_r) of 23.4, a Q×f value of 57,000 (at 9.7 GHz) and a τ_f value of −38 ppm/°C at 1400°C for 2 h.     

3D damage characterisation and the role of voids in the fatigue of wind turbine blade materials

The fatigue mechanisms of Glass Fibre Reinforced Polymer (GFRP) used in wind turbine blades were examined using computed tomography (CT). Prior to mechanical testing, as-manufactured [+45/−45/0]_3,s glass/epoxy specimens were CT scanned to provide 3-dimensional images of their internal microstructure, including voids. Voids were segmented and extracted, and individual characteristics and volumetric distributions were quantified. The coupons were then fatigue tested in uniaxial loading at R = −1% to 40% of the nominal tensile failure stress. Some tests were conducted to failure for correlation with the initial void analysis and to establish failure modes. Other tests were stopped at various life fractions and examined using CT to identify key damage mechanisms. These scans revealed transverse matrix cracking in the surface layer, occurring predominantly at free edges. These free-edge cracks then appeared to facilitate edge delamination at the 45/−45° interface. Propagation from sub-critical, surface ply damage to critical, inner ply damage was identified with either a −45/0° delamination, or a 0° fibre tow failure allowing a crack to propagate into the specimen bulk. Final failure occurred in compression and was characterised by total delamination between all the 45/−45° plies. A quantitative void analysis, taken from the pre-test CT scans, was also performed and compared against the specimens’ fatigue lives. This analysis, to the authors’ knowledge the first of its kind, measured and plotted approximately 10,000 voids within the gauge length of each specimen. The global void measurement parameters and distributions showed no correlation with fatigue life. A local ply-level investigation revealed a significant correlation between the largest void and fatigue life in the region of the laminate associated with the crack propagation from sub-critical to critical damage.     

Elaboration, by tape casting, and thermal characterization of a solid oxide fuel half-cell for low temperature applications

In the past years, a major interest has been devoted to decrease the working temperature of solid oxide fuel cell (SOFC) down to about 700 °C. In this respect, materials with a high ionic conduction at intermediate temperature have to be found and the processes to elaborate fuel cells, using these new materials, have to be developed.Apatite materials (La_10−xSr_x(SiO₄)₆O_2±δ) are attractive candidates for solid electrolyte working at intermediate temperature. The ceramic powder was produced by solid state reaction and was tape cast to obtain green sheets.Concerning the cathode, a perovskite oxide (La_1−xSr_xMn_1−yCo_yO_3−δ) has been chosen. The perovskite powder was also shaped by tape casting with the introduction of a pore forming agent (corn-starch) to obtain the required porosity in the sintered cathode.The co-firing of the electrolyte/cathode half-cell in air at 1400 °C-2 h gives a flat sample with a dense apatite (98.2%), a 42.7% porous cathode and neither delamination nor chemical reactivity between electrolyte and cathode materials.The dimensional behaviour of the electrolyte material is stable for an oxygen partial pressure ranging from 10⁻¹⁰ to 0.21 atmosphere, from room temperature to 700 °C. The thermal expansion coefficients of the electrolyte and cathode materials are rather close (Δα = 2.8 × 10⁻⁶ K⁻¹) under air.     

Processing, dielectric properties and impedance characteristics of Na0.5Bi0.5Cu3Ti4O12 ceramics

Na_0.5Bi_0.5Cu₃Ti₄O₁₂ (NBCTO) ceramics were prepared by conventional solid-state reaction method. The phase structure, microstructure and dielectric properties of NBCTO ceramics sintered at various temperatures with different soaking time were investigated. Pure NBCTO phase could be obtained with increasing the temperature and prolonging the soaking time. High dielectric permittivity (13,495) and low dielectric loss (0.031) could be obtained when the ceramics were sintered at 1000 °C for 7.5 h. The ceramics sintered at 1000 °C for 7.5 h also showed good temperature stability (−4.00 to −0.69%) over a large temperature range from −50 to 150 °C. Complex impedances results revealed that the grain was semiconducting and the grain boundaries was insulating. The grain resistance (R_g) was 12.10 Ω cm and the grain boundary resistance (R_gb) was 2.009 × 10⁵ Ω cm when the ceramics were sintered at 1000 °C for 7.5 h.     

Development of carbon—Low alloy steel grades for low temperature applications

Low alloy steels are processed to fulfill the requirements of low temperature applications. Besides the chemical composition, the steel should receive a suitable heat treatment to ensure the targeted mechanical properties at low temperature. In other words, the steels are designed to delay the ductile to brittle transition temperature to resist dynamic loading at subzero temperatures. Steel alloys processed for liquefied gas pipeline fittings are examples for applications that need deep subzero impact transition temperature (ITT).The main purpose of the present work was to find a suitable heat treatment sequence for alloys LC2 and LC2-1. Further, it aimed to correlate the impact toughness with the microstructure and the fracture surface at different sub-zero temperatures.The steels under investigation are carbon-low alloy grades alloyed with Ni, Cr and Mo. LC2 steel alloy has been successfully processed and then modified to LC2-1 alloy by addition of Cr and Mo. Oil quenching from 900 °C followed by tempering at 595 °C was used for toughness improvements. Hardness, tensile and impact tests at room temperature have been carried out. Further impact tests at subzero temperatures were conducted to characterize alloys behavior. Metallographic as well as SEM fractographic coupled with XRD qualitative analysis are also carried out.Non-homogenous martensite-ferrite cast structure in LC2 was altered to homogeneous tempered martensite structure using quenching-tempering treatment, which is leading to shift the ITT down to −73 °C. Addition of Cr and Mo creates a very fine martensitic structure in LC2-1 alloy. Quenching-tempering of LC2-1 accelerates ITT to −30 °C. It is expected that the steel was subjected to temper embrittlement as a result of phosphorus segregation on the grain boundary due to Cr and Mo alloying, as it was concluded in reference no. [6].     

Growth and characterization of Bi2Se3 thin films by pulsed laser deposition using alloy target

Bi₂Se₃ thin films were deposited on the (100) oriented Si substrates by pulsed laser deposition technique at different substrate temperatures (room temperature −400 °C). The effects of the substrate temperature on the structural and electrical properties of the Bi₂Se₃ films were studied. The film prepared at room temperature showed a very poor polycrystalline structure with the mainly orthorhombic phase. The crystallinity of the films was improved by heating the substrate during the deposition and the crystal phase of the film changed to the rhombohedral phase as the substrate temperature was higher than 200 °C. The stoichiometry of the films and the chemical state of Bi and Se elements in the films were studied by fitting the Se 3d and the Bi 4d5/2 peaks of the X-ray photoelectron spectra. The hexagonal structure was seen clearly for the film prepared at the substrate temperature of 400 °C. The surface roughness of the film increased as the substrate temperature was increased. The electrical resistivity of the film decreased from 1 × 10⁻³ to 3 × 10⁻⁴ Ω cm as the substrate temperature was increased from room temperature to 400 °C.