Experimental study of room-temperature indentation viscoplastic ‘creep’ in zirconium

In this paper we have studied the mechanisms of so-called ‘indentation creep’ in a zirconium alloy. Nanoindentation was used to obtain strain rate data as the sample was indented at room temperature, at a homologous temperature below that for which creep behaviour would be expected for this material. A high value of strain rate was obtained, consistent with previous work on indentation creep. In order to elucidate the mechanism of time-dependent deformation, a load relaxation experiment was performed by uniaxial loading of a sample of the same alloy. By allowing relaxation of the sample from a peak load in the tensile test machine, a similar stress exponent was obtained to that seen in the nanoindentation creep test. We conclude that for metals, at temperatures below that at which conventional creep will occur, nanoindentation ‘creep’ proceeds through deformation on active slip systems that were initiated by prior loading beyond the plastic limit. It is therefore more appropriate to describe it as a viscoplastic process, and not as creep deformation.     

Creep deformation of single crystals of new Co–Al–W-based alloys with fcc/L12 two-phase microstructures

The creep deformation behaviour of single crystals of Co–Al–W-based alloys with γ?+?γ′ two-phase microstructures has been investigated in tension under a constant stress of 137?MPa in air at 1000°C as a function of the γ′ solvus temperature and the volume fraction of the γ′ phase. When described by the creep strain rate versus time curve, the creep deformation of Co–Al–W-based alloys consists of transition and accelerating regions without a steady-state region, as observed in many modern nickel-based alloys. However, the creep strength of the present Co–Al–W-based alloys is comparable with nickel-based superalloys of the first generation but is much weaker than those of the second and higher generations. Unlike in nickel-based superalloys, the so-called p (parallel)-type raft structure, in which the γ′ phase is elongated along the tensile axis direction, is formed during creep in Co–Al–W-based alloys, being consistent with what is expected from the positive values of lattice misfit between the γ and γ′ phases. As a result, of the alloys investigated, the best creep properties are obtained with the alloy possessing the highest volume fraction (85%) of the γ′ phase, which is far larger than usual for nickel-based superalloys (55–60%).     

Deformation mechanisms of low density polyethylene with parallel lamellar morphology

The mechanical anisotropy of low density polyethylene sheets possessing orthorhombic symmetry and parallel lamellae morphology has been studied by making measurements of the creep behavior in extension and shear at room temperature. The behavior is interpreted in terms of two predominant deformation mechanisms taking place within and between the lamellae, i.e., the c-shear process and interlamellar shear, respectively, the latter involving both simple and pure shear of the interlamellar regions. Some of the creep compliances have unusually high time dependence and it is shown that this is related with intralamellar processes.

The determination of the three shear compliances involves the application of the St. Venant relations for torsion of rectangular prisms. This aspect has been thoroughly explored and is described in detail.     

Creep of multidirectionally fibre-reinforced composites

A model for the creep of metal matrix composites multidirectionally reinforced by short fibres is proposed. The reinforcement is described by the effective stiffness tensor of a multidirectional arrangement of continuous fibres and the internal damage of the composite during creep due to fibre fragmentation is introduced by assigning a heuristic nonlinear stress–strain relationship to the fibres. Based on the model, the load partitioning between matrix and fibres is computed. The macroscopic creep behaviour is simulated for composites exhibiting different fibre orientation distributions and different heuristic nonlinear stress–strain functions. The computational results rationalize the creep behaviour of multidirectional fibre-reinforced composites. For a two-dimensional random orientation distribution, a good qualitative match between simulation and experimental results is obtained for compressive loading and for in-plane tensile loading. For loading normal to the reinforcement plane, the model overestimates the creep resistance. In this case, the formation and growth of cavities seems to govern the creep deformation of the composite.     

Elastic stiffness of the nuclear-spin system in tetragonal U2D2 nuclear-ordered solid (3)He

We have measured temperature dependences of sound velocity for both longitudinal and transverse sound in nuclear-ordered U2D2 solid 3He with several crystal orientations along the melting curve. The sound velocity change was proportional to T4 for all sound modes and crystal orientations and was attributed to the nuclear-spin part of the internal energy. We extracted six-independent elastic stiffness of the nuclear-spin part and obtained Grüneisen constants of the spin wave velocity for four-independent strains. Grüneisen constants for compressional strain were larger than those for shear strain. Using the multiple-spin-exchange model, we explain the anisotropy of Grüneisen constants in tetragonal symmetry.     

Mechanisms of high-temperature creep of nickel-based superalloys under low applied stresses

[001] single-crystal specimens of the superalloys CMSX-4 and CMSX-10 were tested for creep at 1100°C under tensile stresses between 105 and 135?MPa, where they show pronounced steady creep. The deformed superalloys were analysed by density measurements, scanning electron microscopy and transmission electron microscopy which supplied information about porosity growth, evolution of the γ–γ′ microstructure, dislocation mobility and reactions during creep deformation. It is shown that, under the testing conditions used, steady creep strain mostly results from transverse glide–climb of (a/2) ?011? interfacial dislocations. A by-product of the interfacial glide–climb are vacancies which diffuse along the interfaces to growing pores or to a ?100? edge dislocations climbing in the γ′ phase. Climb of a ?100? dislocations in the γ′ phase is a recovery mechanism which reduces the constraining of the γ phase by the γ′ phase, thus enabling further glide of (a/2) ?011? dislocations in the matrix. Moreover the γ′ dislocations act as vacancy sinks facilitating interfacial glide–climb. The creep rate increases when the γ–γ′ microstructure becomes topologically inverted; connection of the γ′ rafts results in extensive transverse climb and an increase of the number of a?100? dislocation segments in the γ′ phase.     

Phonon dispersion in aluminium arsenide and antimonide

The phonon dispersion curves for aluminium arsenide and antimonide have been investigated by using a deformation bond approximation model. The results obtained from this model are compared with the experimental values wherever it is available. Since there is no complete experimental phonon dispersion curves for AlAs, we could not compare our calculated results, but the results of AlSb have been compared with the inelastic neutron scattering measurements at 15 K. However, we compare the phonon frequencies of AlAs and AlSb at critical points of the Brillouin zone obtained by our calculations and Raman spectroscopy measurements. This model predicts the phonon modes satisfactorily in all the symmetry directions of the Brillouin zone (BZ). The spectrum has similar features as observed in other III–V compound semiconductors.     

蠕变镍基单晶高温合金微观结构与界面特征的X射线小角散射研究

利用SAXS技术对蠕变过程中不同尺度范围的微观结构变化分析表明X射线小角散射(SAXS)与中子小角散射(SANS)测量的二维散射图具有明显的差异,由散射强度曲线的变化说明了蠕变过程中二次析出γ'相形貌和不同区域尺寸特征的改变情况.分析结果表明二次析出γ'相存在两类特征尺寸,在蠕变过程中沿[100]或[010]方向的变化趋势类似,均是在第一和第二阶段有所减小,在第三阶段又有所增大,相较而言,特征尺寸较大的γ'相变化也较为显著.二次析出γ'相在蠕变第二阶段元素扩散最严重,相表面最粗糙,在第三阶段两相界面又进一 关键词： 单晶高温合金 二次析出γ'相 X射线小角散射 微观结构     

Small-angle X-ray scattering investigation of deformation-induced nanovoids in AA6063 aluminium alloy

Abstract

Small-angle X-ray scattering studies of microstructure in metallic systems are prone to contamination by double Bragg scattering from the crystalline matrix. This is particularly problematic to the study of fracture in ductile metals via the nucleation and growth of nanovoids in response to plastic deformation. We show clear evidence of the presence of these scattering artefacts in the scattering data from representative Al systems and describe a simple method of numerically isolating and removing potentially misleading information to reveal the true small angle scattering response of the sample. This data correction process is used to obtain quantitative measurements of the nanovoid volume fraction in deformed AA6063. The SAXS results yield values comparable to existing predictions of the total vacancy volume fraction obtained from the mechanical stress–strain data.     

In-situ SAXS study on PET/ PMMT composites during tensile tests

The nanostructures during the tensile drawing of poly(ethylene terephthalate)(PET)/hexadecyl triphenyl phosphonium bromide montmorillonite(PMMT) nanocomposites were studied by in-situ small angle x-ray scattering. For strain higher than the yield point, the scattering intensity increases dramatically due to the nucleation and growth of nanovoids and crystals. The nanovoids and crystals are significantly dependent on the heating temperature. The effective filling of PMMT in the PET matrix provokes a strong restriction to the long period. The peaks of the long period disappear gradually with the deformation strain increasing from 0% to 34%.     

Nanoscale deformation irregularities of γ-irradiated poly(methyl methacrylate)

Development of deformation jumps in the creep of poly(methyl methacrylate) (PMMA) has been studied. The structural levels of deformation have been determined from the creep rate oscillation periods (deformation jumps) measured by the interferometric method. Special attention is given to a new method of data processing, which enables one to reveal previously undetectable nanoscale deformation jumps. By the example of PMMA specimens preliminarily exposed to γ radiation with doses D=55–330 kGy and unexposed specimens, the presence of nanoscale deformation jumps with the values dependent on the dose D and time of creep has been shown. The obtained results confirm the existence of 10–20-nm domains in amorphous polymers and make it possible to study the multilevel organization of the deformation process, starting from the nanoscale.     

Analysis of slip activity and heterogeneous deformation in tension and tension-creep of Ti–5Al–2.5Sn (wt %) using in-situ SEM experiments

The deformation behavior of a Ti–5Al–2.5Sn (wt %) near-α alloy was investigated during in-situ deformation inside a scanning electron microscope. Tensile experiments were performed at 296?K and 728?K (≈0.4?T _m), while tensile-creep experiments were performed at 728?K and 763?K. Active deformation systems were identified using electron backscattered diffraction-based slip trace analysis. Both basal and prismatic slip systems were active during the tensile experiments. Basal slip was observed for grains clustered around high Schmid factor orientations, while prismatic slip exhibited less dependence on the crystallographic orientation. The tension-creep experiments revealed less slip but more development of grain boundary ledges than in the higher strain rate tensile experiments. Some of the grain boundary ledges evolved into grain boundary cracks, and grain boundaries oriented nearly perpendicular to the tensile axis formed ledges earlier in the deformation process. Grain boundaries with high misorientations also tended to form ledges earlier than those with lower misorientations. Most of the grain boundary cracks formed in association with grains displaying hard orientations, where the c-axis was nearly perpendicular to the tensile direction. For the tension-creep experiments, pronounced basal slip was observed in the lower-stress creep regime and the activity of prismatic slip increased with increasing creep stress and temperature.     

Dislocation-mediated creep process in nanocrystalline Cu

Nanocrystalline Cu with average grain sizes ranging from ～ 24.4 to 131.3 nm were prepared by the electric brushplating technique.Nanoindentation tests were performed within a wide strain rate range,and the creep process of nanocrystalline Cu during the holding period and its relationship to dislocation and twin structures were examined.It was demonstrated that creep strain and creep strain rate are considerably significant for smaller grain sizes and higher loading strain rates,and are far higher than those predicted by the models of Cobble creep and grain boundary sliding.The analysis based on the calculations and experiments reveals that the significant creep deformation arises from the rapid absorption of high density dislocations stored in the loading regime.Our experiments imply that stored dislocations during loading are highly unstable and dislocation activity can proceed and lead to significant post-loading plasticity.     

Automatic measurement of the creep behavior of linear polymers in the course of homogeneous drawing

An automatic device was built, enabling the creep behavior of fibers of linear semicrystalline polymers to be studied during various stages of homogeneous drawing. The device first deforms the sample at constant speed up to a certain draw ratio; then, without interrupting the stress, the character of deformation is changed from deformation at constant speed to that caused by constant load (creep). It was verified that the method described supplies more detailed information on the changes of the mechanical behavior of polymers at various stages of orientation than does the more conventional stress-strain curve.     

非线性电磁超声对铝合金拉伸变形评价研究

非线性系数是描述材料中微纳尺度损伤的特征参量,非线性系数常通过接触式压电超声进行检测,但耦合剂引起的非线性一般是未知的,针对这一问题,提出了一种非接触式电磁超声非线性纵波检测方法。该方法基于洛伦兹力机理在试件表面产生的振动弹性波,利用不同拉伸载荷下所制备的损伤试件,分别利用压电超声、电磁超声进行非线性超声系数测量。实验结果表明:利用两种非线性超声检测的相对非线性系数与铝合金的拉伸形变呈单调关系,同时也论证了电磁超声纵波基于非线性理论对塑性变形评估的可行性。      

Statistical analysis of the strength of ultra-oriented ultra-high-molecular-weight polyethylene film filaments in the framework of the Weibull model

A statistical analysis of the distribution of the tensile strength σ of ultra-oriented ultra-high-molecular-weight polyethylene (UHMWPE) film filaments has been performed in the framework of the Weibull model using the results obtained from a large number (50) of measurements. The UHMWPE film filaments have been produced by means of high-temperature multistage zone drawing of xerogels prepared from 1.5% UHMWPE solutions in decalin. The Weibull modulus has been determined for this type of materials. It has been shown that, for the ultimate draw ratio λ = 120, the average tensile strength is equal to 4.7 GPa, which is significantly higher than the tensile strength σ = 3.5 GPa for commercial gel-spun UHMWPE fibers manufactured by the DSM Company (The Netherlands) and the Honeywell International Incorporation (United States). It has been demonstrated that, for 20% of the specimens thus prepared, the tensile strength reaches record-high values σ = 5.2–5.9 GPa.     

Strain mapping analysis of textile composites

The focus of the work is meso-scale analysis (scale level of the fabric unit cell) of textile composite deformation and failure. The surface strain measurement is used for: (1) experimental investigation, which includes study of strain distribution at various stages of deformation, plasticity detection, damage initiation; (2) numerical validation of the correspondent finite element (FE) models. Two examples are considered: carbon-epoxy triaxial-braided and glass polypropylene-woven composite. The surface strain measurement (by digital image correlation technique) accompanies the tensile tests, aiming at: (1) elastic anisotropic constants characterisation, (2) study of non-linear material behaviour (for the thermoplastic composite), (3) control of homogeneity of the macro-strain distribution, and (4) analysis of damage initiation in brittle composites. Validation of meso-FE models by strain measurements encounters difficulties arising from (1) resolution of the strain measurements, (2) irregularities of the initial structure such as random layer nesting, ply interaction, and deviation of yarns from their theoretical position, which affects the measured strain fields. The paper discusses these difficulties and demonstrates a qualitative agreement with the FE analysis of idealised composite configurations.     

Solid-state 13C NMR and synchrotron SAXS/WAXS studies of uniaxially-oriented polyethylene

We report solid-state ¹³C NMR and synchrotron wide-and small-angle X-ray scattering experiments (WAXS, SAXS) on metallocene linear low density polyethylene films (e.g., Exceed™ 1018 mLLDPE; nominally 1 MI, 0.918 density ethylene-hexene metallocene copolymer) as a function of uniaxial draw ratio, λ. Combined, these experiments provide an unambiguous, quantitative molecular view of the orientation of both the crystalline and amorphous phases in the samples as a function of draw. Together with previously reported differential scanning calorimetry (DSC), gas transport measurements, transmission electron microscopy (TEM), optical birefringence, small angle X-ray scattering (SAXS) as well as other characterization techniques, this study of the state of orientation in both phases provides insight concerning the development of unusually high barrier properties of the most oriented samples (λ=10). In this work, static (non-spinning) solid-state NMR measurements indicate that in the drawn Exceed^TM films both the crystalline and amorphous regions are highly oriented. In particular, chemical shift data show the amorphous phase is comprised increasingly of so-called “taut tie chains” (or tie chains under any state of tautness) in the mLLDPE with increasing draw ratio – the resonance lines associated with the amorphous phase shift to where the crystalline peaks are observed. In the sample with highest total draw (λ=10), virtually all of the chains in the non-crystalline region have responded and aligned in the machine (draw) direction. Both monoclinic and orthorhombic crystalline peaks are observed in high-resolution, solid-state magic-angle spinning (MAS) NMR measurements of the oriented PE films. The orientation is comparable to that obtained for ultra-high molecular weight HDPE fibers described as “ultra-oriented” in the literature. Furthermore, the presence of a monoclinic peak in cold-drawn samples suggests that there is an appreciable internal stress associated with the LLDPE. The results are confirmed and independently quantified by Herman's Orientation Function values derived from the WAXS measurements. The degree of orientation approaches theoretically perfect alignment of chains along the draw direction. We deduce from this observation that a high fraction of the non-crystalline chains are either tie chains that directly connect adjacent lamellae or are interlocking loops from adjacent lamellae. In either case, the chains are load-bearing and are consistent with the idea of “taut tie chains”. We note that transmission electron micrographs recorded for the ultra-oriented Exceed showed the lamellae are often appreciably thinner and shorter than they are for cast or blown Exceed 1018. Combined with higher crystallinity, the thinner lamellae statistically favor more tie chains. Finally, the remarkably large decrease in permeability of the λ=10 film is primarily attributed to the high degree of orientation (and loss of entropy) of the amorphous phase.     

Creep and physical aging in a polyamideimide carbon fiber composite

The creep properties of an amorphous thermoplastic polyamideimide and its continuous carbon fiber composite have been investigated. Creep behavior in the viscoelastic (low stress) and viscoplastic (high stress) ranges was examined. The interaction of physical aging with the creep behavior of the material was found to be significant in both stress regimens. Physical aging shifted creep curves to longer times in the viscoelastic range, reducing the total amount of creep strain in both the viscoelastic and viscoplastic ranges. The amount of nonrecoverable strain produced during viscoplastic creep was highly dependent upon the amount of time a sample was held under load due to concurrent physical aging. Specimens aged significantly prior to testing showed no undue time dependence in the amount of nonrecoverable creep strain produced. The viscoplastic creep behavior was shown to be composed of instantaneous localized plastic deformation, viscous strain, stiffening due to aging, and densification due to aging.