Improvement of the fracture toughness of adhesively bonded stainless steel joints with aramid fibers at cryogenic temperatures

Adhesives should be reinforced with reinforcing fibers for the bonding of adherends at cryogenic temperatures because all the adhesives become quite brittle at cryogenic temperatures. In this work, the film-type epoxy adhesive was reinforced with randomly oriented aramid fiber mats to decrease the CTE (Coefficient of Thermal Expansion) of the adhesive and to improve the fracture toughness of adhesive joints composed of stainless steel adherends at the cryogenic temperature of −150 °C. The cleavage tests of the DCB (Double Cantilever Beam) adhesive joints were performed to evaluate the fracture toughness and crack resistance of the adhesive joints. Also, the thermal and mechanical properties of the fiber reinforced adhesive layer were measured to investigate the relationship between the fracture toughness of adhesive joints and fiber volume fraction of aramid fibers. From the experiments, it was found that the crack propagated in the adhesive with the stable mode of significantly increased fracture toughness when the film-type epoxy adhesive was reinforced with aramid fiber mats. The optimum volume fraction of aramid fibers was suggested for the film-type epoxy adhesive in the adhesive joint at the cryogenic temperature of −150 °C.     

On the change of fracture mechanism with test temperature

Three point bending (3PB) tests of precracked specimens were carried out for coarse grain C-Mn steel at three low temperatures. Details of fracture surfaces in the specimens were microscopically observed and cleavage initiation sites were located. Calculations of local critical parameters and simulations of fracture behavior were made using finite element method (FEM). The results reveal that at very low temperature (−196 °C), the critical event controlling cleavage fracture is the nucleation of crack at the precrack tip in ferrite. The critical event moves to the initiation and propagation of a second phase particle crack at moderately low temperature (−110 °C). At higher temperature (−30 °C), the critical event for cleavage fracture after a fibrous crack extends is the propagation of a grain-sized crack.     

The influence of subzero temperatures on fatigue behavior of composite sandwich structures

The fatigue lives and failure modes of foam core carbon/epoxy and glass/epoxy composite sandwich beams in 4-point bending were characterized from room temperature (22 °C) down to −60 °C. Similar previous investigations had focused on elevated temperatures only, but the low temperature fatigue behavior must be understood so that these materials may be evaluated for possible use in the hull structures of ships, which operate in cold regions. Core shear was found to be the dominant fatigue failure mode for the test specimens over the entire temperature range from 22 °C down to −60 °C. Significant increases in the useful fatigue life with brittle type core shear failure were observed at low temperatures by comparison with the corresponding room temperature behavior. Fatigue failure at the low temperatures was catastrophic and without any significant early warning, but the corresponding failures at room temperature were preceded by relatively slow but steadily increasing losses of stiffness. Two different approaches were used to investigate stiffness reductions during fatigue tests, and both approaches led to the same conclusions. Experimental observations regarding the location of fatigue crack initiation were confirmed by static finite element analyses for both materials.     

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.     

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.     

Mechanical characterization of steel/CFRP double strap joints at elevated temperatures

This paper examines the mechanical performance of steel/CFRP adhesively-bonded double strap joints at elevated temperatures around the glass transition temperature (T_g, 42 °C) of the adhesive. A series of joints with different bond lengths were tested to failure at temperatures between 20 °C and 60 °C. It was found that the joint failure mode changed from adherend failure to debonding failure as the temperature approached T_g. In addition, the ultimate load and joint stiffness decreased significantly at temperatures near to and greater than T_g, while the effective bond length increased with temperature. Based on the ultimate load prediction model developed by Hart-Smith for double lap joints and kinetic modelling of the mechanical degradation of the adhesive, a mechanism-based model is proposed to describe the change of effective bond length, stiffness and strength degradation for steel/CFRP double strap joints at elevated temperatures. The modelling results were validated by the corresponding experimental measurements.     

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.     

Crack arrest testing of high strength structural steels for naval applications

The crack arrest fracture toughness of two high strength steel alloys used in naval construction, HSLA-100, Composition 3 and HY-100, was characterized in this investigation. A greatly scaled-down version of the wide-plate crack arrest test was developed to characterize the crack arrest performance of these tough steel alloys in the upper region of the ductile-brittle transition. The specimen is a single edge-notched, 152 mm wide by 19 mm thick by 910 mm long plate subjected to a strong thermal gradient and a tensile loading. The thermal gradient is required to arrest the crack at temperatures high in the transition region, close to the expected service temperature for crack arrest applications in surface ships. Strain gages were placed along the crack path to obtain crack position and crack velocity data, and this data, along with the applied loading is combined in a “generation mode” analysis using finite element analysis to obtain a dynamic analysis of the crack arrest event. Detailed finite element analyses were conducted to understand the effect of various modeling assumptions on the results and to validate the methodology compared with more conventional crack arrest tests.Brittle cracks initiation, significant cleavage crack propagation and subsequent crack arrest was achieved in all 15 of the tests conducted in this investigation. A crack arrest master curve approach was used to characterize and compare the crack arrest fracture toughness. The HSLA-100, Comp. 3 steel alloy had superior performance to the HY-100 steel alloy. The crack arrest reference temperature was T_KIA = −136 °C for the HSLA-100 plate and T_KIA = −64 °C for the HY-100 plate.     

Statistical scatter of fracture toughness in the ductile-brittle transition of a structural steel

The statistical scatter of fracture toughness in the ductile-brittle transition temperature range was experimentally examined on a 500 MPa class low carbon steel. Fracture toughness tests were replicatedly performed at −60 °C, −20 °C and −10 °C. The tests at −60 °C resulted in a single modal Weibull distribution with a shape parameter of 4 for the critical stress intensity factor converted from J-integral, whereas the Weibull distributions of the critical stress intensity factor at −20 °C and −10 °C showed a bilinear pattern with an elbow point, which caused a wider scatter than that at −60 °C. Such scatter transition behavior was discussed with reference to stable crack initiation. A model of the statistical scatter transition has been proposed in this work and the model reasonably explains the experimental results.     

Low temperature crack propagation in an epoxide resin

The effects of temperature and testing rate on the fracture energies and modes of crack propagation of an epoxide resin cured with a range of amine curing agents have been determined. The simplest behaviour observed consisted of unstable crack propagation at high temperatures with a transition to stable crack growth at lower temperatures (~ 0° C) followed by a further transition (at ~ –150° C) back to unstable crack growth at the lowest temperatures. More complicated series of transitions were also observed. The variation of the upper transition temperature with testing rate and cross-linking density is qualitatively what would be expected from a model of limited crack tip plasticity but the reasons for the lower temperature transition are unknown. Some observations of the effects on crack propagation mode of curing conditions and water are also reported.     

Cryogenic reliability of composite insulation panels for liquefied natural gas (LNG) ships

The major carrier of liquefied natural gas (LNG) is LNG ships, whose containment system is composed of dual barriers and composite insulation panels. The LNG containment system should have cryogenic reliability and high thermal insulation performance for safe and efficient transportation of LNG. The secondary barrier composed of adhesive bonded aluminum strips should keep tightness for 15 days, when the welded stainless primary barrier fails. However, cracks are generated in the composite insulation panels due to the local stress concentration and the brittleness of insulation materials at the cryogenic temperature of −163 °C. If cracks generated in the insulation panel propagate into the secondary barrier, LNG leakage problem might occur, which is a remaining concern in ship building industries.In this study, crack retardation capability in the composite insulation panel was investigated with glass fabric reinforcement. Finite element analysis was conducted to estimate the thermal stress at the cryogenic temperature and a new experimental method was developed to investigate the failure of secondary barrier of composite insulation panel. From the experimental results, it was found that the glass fabric reinforcement was effective to retard the crack propagation into the aluminum secondary barrier from the polyurethane insulation foam at the cryogenic temperature.     

Initiation and propagation of fatigue cracks in cast IN 713LC superalloy

Fatigue life, initiation and propagation of cracks at 800 °C in a cast Ni-base superalloy IN 713LC were experimentally studied in high-cycle fatigue region. Load symmetrical cycling and cycling with high tensile mean load were applied. Both crystallographic crack initiation resulting in long Stage I crack growth and non-crystallographic Stage II propagation were observed. High scatter of fatigue life data was explained by: (i) variability in microstructural conditions for crystallographic crack initiation and propagation and by (ii) influence of casting defect size distribution. The fractographic observation supports the slip band decohesion mechanism of crack initiation and an important role of cyclic slip localization in persistent slip bands.     

Environmental effects on fatigue behavior of adhesively-bonded pultruded structural joints

The fatigue response of adhesively-bonded pultruded GFRP double-lap joints has been investigated under different environmental conditions. Tests were performed at ?35 °C, 23 °C and 40 °C. A fourth set of fatigue data was collected from tests on preconditioned specimens in warm (40 °C) water. The tests were performed at 40 °C and at 90% relative humidity. Specimens were instrumented with strain and crack gages to record fatigue data. In addition to the S–N curves, stiffness fluctuations and crack initiation and propagation during fatigue were monitored. The dominant failure mode was a fiber-tear failure that occurred in the mat layers of the GFRP laminates. In the presence of high humidity, the failure shifted to the adhesive/composite interface. Although the testing temperature was lower than the glass transition temperature of the adhesive, its influence on the fatigue life and fracture behavior of the examined joints was apparent and was aggravated by the presence of humidity.     

Some recent results on crack healing of poly(methyl methacrylate)

The solvent healing and void growth of poly(methyl methacrylate) (PMMA) at elevated temperatures were studied. In addition to entanglement between two or more broken polymeric chains, the chemical bonds between two polymeric broken chains were produced during healing in methanol or d₁-methanol. Cracks in PMMA were induced either by Nd-YAG laser irradiation or by acetone immersion. The solvents occupied the voids enclosed by polymeric chains. The chemical bonds and structure were analyzed with FTIR and NMR spectroscopy. The results show that in addition to mechanical lock of broken chains, hydrogen bond increases with uptake of solvent which enhances the crack healing. The cylindrical crack in PMMA was healed at temperatures 110-160 °C and spherical void was grown at temperatures 170-190 °C. This suggests that annealing above the glass transition temperature of polymer is a necessary condition for thermal healing, but not for the sufficient condition.     

Effect of temperature and strain rate on the strength of a PET/glass fibre composite

Constant strain-rate mechanical testing and surface fractography were used to characterize the failure behaviour of a PET/glass injection-moulding compound and of its unfilled matrix material. Parameters for this investigation were temperature and strain rate. The matrix material exhibited a viscous-brittle transition between room temperature and 60° C. Low temperature failure occurred by craze growth, followed by slow and rapid crack propagation. The composite material likewise behaved as a viscous solid at superambient temperatures. Failure at low temperatures and/or high deformation rates occurred by brittle matrix fracture and fibre pull-out. Under these conditions, mechanical properties improved, relative to those at room temperatures. At intermediate temperatures and/or low strain rates, failure occurred via matrix crazing and crack propagation near the fibre ends. An observed serration of the fracture path at high strain rates is suggested to be due to the need for high shear stresses at the fibre-matrix interface.On leave from the Center for Composite Materials and Department of Chemical Engineering, University of Delaware, Newark, Delaware 19711, USA.     

Modeling nonlinear thermo-elastic response for glassy polycarbonate using ultrasonic results under compression in a confined cell

We develop a nonlinear thermo-elastic model for polycarbonate (PC) using ultrasonic longitudinal and shear waves applied on a sample under confined compression. The model is a thermodynamically consistent model developed based on data obtained from a modified pressure-volume-temperature measurement system that also provides the longitudinal and shear wave moduli (Masubuchi et al., 1998. Materials Science Research International 4(3), 223-226). The heat capacity data was obtained by using a differential scanning calorimeter. The resulting model reproduces the ultrasonic behavior of the PC over the temperature range of 35 °C to 150 °C and under pressures from 0 to 70 MPa. Since the response at constant pressure is close to linear below the glass transition temperature of 147 °C, one may extend the use of the model to temperatures below 35 °C, possibly covering most of the range of use for most applications.     

Effect of NiCrAlY platelets inclusion on the mechanical and thermal shock properties of glass matrix composites

NiCrAlY platelets modified glass matrix composites were prepared. Their microstructures were characterized, their Young's modulus, fracture strength in bending, Vickers hardness, and indentation toughness were measured, and their thermal shock resistance was studied using quenching-strength and indentation-quench methods. With increasing NiCrAlY content, evident enhancements of the Young's modulus and indentation toughness were obtained. The NiCrAlY alloy inclusion could exert significant influences on the retained bending strength of the samples after quench tests, from 9.6 MPa for NiCrAlY-free glass to 32.0 MPa for 30 wt.% NiCrAlY-containing composites. The indentation-quench tests showed that NiCrAlY alloy inclusion elevated the critical quenching temperatures for propagation of pre-crack, from 150 °C for NiCrAlY-free glass to 225 °C for 30 wt.% NiCrAlY-containing composites. Inclusion debonding and intersection, crack deflection and bridging were observed, and are likely the micromechanisms accounted for the improvement of fracture resistance.     

Yield and fracture behaviour of cross-linked epoxies

The yield stress and fracture energies of a series of cross-linked epoxy resins were studied in order to correlate the macroscopic mechanical properties with the polymer microstructure. Five networks with varying cross-link densities were synthesized by reacting a homologous series of epoxy resins with stoichiometric quantities ofm-phenylenediamine. For all the networks, the yield stress decreased with increasing temperatures in accordance with the predictions of the Eyring theory of viscosity. At constant temperatures, the yield stress decreased with increasing molecular weight between cross-links. The fracture studies revealed two distinct types of crack propagation behaviour above and below approximately 0 °C. Below 0 °C the cracks propagated in a stable and continuous manner, while the crack propagation behaviour changed to an unstable stick-slip mode as the test temperature was increased above 0 °C. For unstable crack growth, the fracture energies for crack initiation increased with increasing temperature, while the fracture energies for crack arrest were, within the limits of experimental error, independent of temperature. The crack arrest fracture energies were similar in magnitude to the fracture energies for stable crack propagation. An empirical power-law type correlation was observed between the glassy arrest fracture energies and the average molecular weight between cross-links. Micrographs of specimens which failed by the unstable, stick-slip mode revealed characteristic plastic deformation zones which highlighted the positions of crack initiation and arrest along the crack path. The deformation zone widths were observed to increase with increasing test temperatures, providing evidence of greater localized plastic deformations and higher fracture initiation energies at higher temperatures.     

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.     

Mechanical properties of pulse discharge sintered Cr2AlC at 25-1000 °C

Ternary compound Cr₂AlC was synthesized by a reactive sintering process and its mechanical properties in the 25-1000 °C temperature range were studied by 4-point bending tests. The flexural strength of Cr₂AlC decreases continuously from 555 ± 11 MPa at room temperature down to 100 ± 4 MPa at 1000 °C and this strength decreasing tendency is more obvious as the testing temperature is higher than 900 °C. The ductile-to-brittle transition temperature of Cr₂AlC locates in the range of 800-900 °C. The macro-plastic deformation of Cr₂AlC is mainly attributed to the initiation and propagation of large number of microcracks.