Anelastic relaxation processes due to hopping of interstitial oxygen in scandium

The anelastic spectrum of the solid solution Sc–O has been investigated on a polycrystalline sample from 360 to 570 K for oxygen concentrations varying between 0.024 and 0.91 at.% O, as estimated by electrical resistivity and intentional doping. Two relaxation processes appear at 430 and 520 K for the vibration frequency of 3.5 kHz; both peaks are stable with thermal cycling and their intensities increase with the oxygen content.

The process at lower temperature has been tentatively interpreted as due to the stress-induced hopping of oxygen atoms between the non equivalent tetrahedral and octahedral interstitial sites. A possible mechanism for the higher temperature process could be the dissolution/formation of interacting O–O pairs.     

Mechanical relaxation in simple molecular liquids from the liquid to the supercooled state

Attenuation and velocity of acoustic waves have been revealed at ultrasonic frequencies (2, 5 and 10 MHz) in some glass-forming liquids. The mechanical response has been studied following continuously the materials from the liquid to the supercooled state, using an experimental set-up developed to this purpose. A peak in the attenuation of longitudinal acoustic waves has been observed in a temperature region in which the liquids are supercooled. Correspondingly, the sound velocity shows a dispersion, increasing from liquid-like to solid-like values for decreasing temperatures. Both features develop above the calorimetric glass transition temperature (T_g). In the deeply supercooled liquids, nearly 10 K above their calorimetric T_g, also the propagation of transverse wave sound (which is a characteristic behaviour of solid-like materials) has been experimentally detected. Shear and longitudinal relaxation times are not decoupled in the time–temperature region investigated. Compared to the mechanical one, the dielectric relaxation studied as a function of temperature at the same frequency of the ultrasonic experiments shows a loss peak centred at the same temperature. Depending on the liquid investigated, the mechanical relaxation spectrum can be broader than the dielectric one, specially in the low temperature flank, suggesting that some dissipative processes at lower energies can contribute to the mechanical loss, even though they do not couple to the electric probe field.     

Approaching the fundamental noise limit in Mo/Au TES bolometers with transverse normal metal bars

Recent efforts in the Transition Edge Sensor (TES) bolometer/calorimeter community have focused on developing detectors whose noise properties are near the fundamental limits. These include the in-band phonon noise, the out-of-band Johnson noise, and the 1/f noise. We have investigated the noise performance of Mo/Au-bilayer TES bolometers designed for infrared detectors. These detectors use normal metal regions for the suppression of excess noise, which are oriented either parallel to (“bars”) or transverse to (“stripes”) the direction of current flow. Two nearly identical detectors, one with stripes and one with bars, were fabricated at the NASA/GSFC detector development facility. Significantly lower noise is found with the normal metal regions oriented transversely. We compare the detailed noise measurement and quantitative analysis of the noise level in each device as a function of the detector resistance. Our preliminary result is that the best detector features only moderate excess noise in both the in-band region and in the out-of-band region. This noise performance is suitable for instruments with multiplexed TES arrays, such as GSFC's FIBRE and SAFIRE.     

Estimation of fatigue crack growth retardation due to crack branching

Quantitative analysis is provided to estimate the reduction of fatigue crack growth rate due to overload crack branching. A recent mixed-mode fatigue crack growth model based on the dilatational component of the accumulated strain energy density near the crack tip is modified to quantify the retardation factor of crack growth rate following an overload. It is found that crack branching due to an overload results in considerable reduction of fatigue crack growth rate. The retardation factor estimated by the proposed methodology is correlated with test results for the 2090-T8E41 aluminum–lithium alloy indicating encouraging agreement.     

Using a microcalorimeter to measure the Lamb shift in hydrogenic gold and uranium on cooled, decelerated ion beams

A precise determination of the Lamb shift from photons emitted by highly charged, one electron ions represents one of the most sensitive tests of QED in strong electromagnetic fields. Recent progress in the production and cooling of intense beams of fully stripped Au and U in the SIS/ESR synchrotron storage ring at GSI, Darmstadt has made it possible to obtain precision spectroscopy of these ions. A fully stripped beam of either Au⁷⁹⁺ or U⁹²⁺ ions is injected, stored and cooled in the ESR and interacts with an internal gas target. The capture of an electron and the subsequent population of a 2p or 3p state will lead to a decay by either Lyman or Balmer X-ray emission. Although measurements of the 1 s Lamb shift in U with Ge ionization detectors accurate to 3% have provided a test of QED for the high Z domain, the experimental errors (±13 eV) are about one order of magnitude larger than the accuracy theoreticians presently claim (±1 eV). We present the results from initial broad band experiments using NTD Ge microcalorimeters to measure the 2 s Lamb Shift in Au and U at the ESR. The broad band coverage of the microcalorimeter makes it possible to reduce the systematic uncertainties in the Doppler corrections while the high-energy resolution reduces the statistical error in the absolute energy calibration.     

High temperature structural evolution of a CuAlNi alloy studied by in situ X-ray diffraction and isothermal mechanical spectroscopy

The purpose of this work is to study the microstructural mechanisms associated with the eutectoid transition in a ternary Cu–12 wt.% Al–3 wt.% Ni alloy. The samples have been initially annealed at 850 °C, then slowly cooled down to room temperature. The experiments have been carried out both on cooling and on heating above 500 °C using isothermal mechanical spectroscopy and X-ray diffraction (fitted with a temperature camera). On heating, a relaxation peak with a high intensity rises up above 600 °C, then on cooling, the peak totally disappears below 580 °C, the effect being reproducible. The structural analysis, undertaken in the same temperature domain, has clearly evidenced each step of the evolution, particularly the eutectoid transformation. Consequently, the damping effect seems to be associated to the presence of the high temperature β phase.     

Anelastic relaxation processes due oxygen in Nb–3.1 at.% Ti alloys

In the last 50 years several studies have been made to understand the relaxation mechanisms of the heavy interstitial atoms present in transition metals and their alloys. Internal friction measurements have been carried out in a Nb–Ti alloy containing 3.1 at.% of Ti produced by the Materials Department of Chemical Engineering Faculty of Lorena (Brazil), with several quantities of oxygen in solid solution using a torsion pendulum. These measurements have been performed by a torsion pendulum in the temperature range from 300 to 700 K with an oscillation frequency between 0.5 and 10 Hz. The experimental results show complex internal friction spectra that have been resolved, into a series of Debye peaks corresponding to different interactions. For each relaxation process it was possible to obtain the height and temperature of the peak, the activation energy and the relaxation time of the process.     

Amplitude-dependent internal friction in copper thin films on silicon substrates

Internal friction in copper thin films 0.2–1.5 μm thick on silicon substrates has been measured between 180 and 340 K as a function of strain amplitude. Analysis of the amplitude-dependent internal friction in the copper films shows the relation between the plastic strain of the order of 10⁻⁹ and the effective stress on dislocation motion. The stress–strain curves thus obtained for the copper films tend to shift to a higher stress with decreasing film thickness and also with decreasing temperature, both indicating a suppression of microplastic flow. It is concluded that the microflow stress at a constant level of the plastic strain varies inversely with the film thickness at all temperatures examined. The film thickness effect in the microplastic range can be explained on the basis of a dislocation-bowing model.     

Detectors with Ir/Au-thermometers for high count rate tests in the CRESST experiment

With simultaneous measurement of the temperature signal and the scintillation light of a CaWO₄ absorber crystal, it is possible to reject the gamma and electron background in the Cryogenic Rare Event Search with Superconducting Thermometers experiment. In order to understand the different events from various particles correctly a neutron calibration experiment and other tests are necessary. Using an existing accelerator facility these tests will be performed above ground. For such an experiment, a detector with good stability at high count rates is necessary. The detectors used in the Gran Sasso Laboratory are equipped with W-thermometers. They show long decay times and need active stabilisation and therefore are not well suitable for experiments with high count rates. We report on developments and first results on detectors based on Ir/Au-thermometers in electrothermal feedback mode.     

Interaction of dissolved atoms and relaxation due to interstitial atoms in hcp metals

The literature data on the mechanism of internal friction maxima induced by O, N, and C in α-Ti, α-Zr, and α-Hf, are contradictory. They do not answer the question which kind of complexes induces relaxation: interstitial atoms or interstitial atoms with substitutional atoms. To clarify this question, modeling of the short-range order and atomic displacement fields around the solute atom clusters was carried out by the Monte-Carlo technique for typical Ti–O–Zr alloys. The energies of strain-induced (elastic) O–O and O–Zr interactions and displacement fields of host atoms around the solute atoms were calculated and used in modelling. The concentration dependence of relaxation strength due to diffusion under stress of oxygen atoms was evaluated using the values of local displacement around the solute atom complexes. It is shown that the developing short-range order cannot be described by the single O–O or O–Zr pair and the associated relaxation, as simple reorientation of any specific atomic pairs. It seems likely that in many cases the internal friction is caused by more complicated clusters constituted by interstitial and substitutional atoms.     

Numerical analysis of fracture in ceramic coatings subjected to thermal loading

In this paper the general purpose finite element code ANSYS has been employed to analyse fracture in ceramic coatings subjected to thermal loading. An approach is developed in which hypothetical material properties have been considered as material data for coupled (thermal and structure) finite element analysis. These properties were chosen by assumed changes in some functional properties of ZrO₂-G.G. coatings. The aim was to evaluate the stress intensity factors in different coatings. Furthermore, to demonstrate the influence of crack length and coating geometry on the stress intensity in coatings, finite element analyses were carried out for various cases. The normalized stress intensity factors were obtained. The results showed that the shorter the crack length and the thinner the coating, the sounder the coatings. Furthermore, coatings representing a wide range of thermal and mechanical properties have a close normalized stress intensity factor values. It is also concluded that the finite element technique can be used to optimize the design and the processing of ceramic coatings.     

Contribution to the comprehension of dissipation phenomena in lead zirconate titanate: aliovalent doping effect

By the solid reaction method, undoped, potassium doped and niobium doped lead zirconate titanate (PZT) are elaborated. The mechanical losses measured in the range of the Hz as a function of temperature shows two peaks R₁ and R₂, and a ferroelectric transition peak P₁ between ferroelectric and para-electric states on the undoped PZT—Pb(Zr_0.54Ti_0.46)O₃—noted PZT54/46. Potassium doped PZT—Pb_1−xK_x(Zr_0.54Ti_0.46)O₃—shortly called PKZT 100x/54/46 shows an increase in the height of both the peaks at a doping content, x, less than 0.5 at.% but an opposite effect is observed above this value. Niobium doped PZT—Pb[(Zr_0.54Ti_0.46)_1−yNb_y]O₃—shortly called PNZT 100y/54/46, shows the vanish of the R₂ peak and the decrease of the height of the R₁ peak when the doping content increases.     

Comparative study of mechanical and dielectric relaxations in polymers

The state-of-the-art concerning the comparison and interconversion of mechanical and dielectric relaxational data of polymers is revisited. Different methods and strategies referred to the analysis of normal and segmental modes as well as secondary absorptions, are discussed. Current theories are illustrated with examples taken from the current literature.     

Multi-objective optimisation of composite absorber shape under crashworthiness requirements

The dynamic fracture behavior of a functionally graded coating–substrate system with an internal crack perpendicular to the interface is studied under an in-plane impact load. The structure consists of a functionally graded coating and a semi-infinite homogeneous substrate. The crack is located in the functionally graded coating. The mixed boundary value problem is formulated analytically by use of integral transform techniques and singular integral equation. The influences of material constants and the geometry parameters on the dynamic stress intensity factors (SIFs) are studied.     

Relaxation processes in a glassy polymer containing methanol molecules

The interaction of small guest molecules with the molecular degrees of freedom of a glassy polymer matrix is investigated, i.e. (i) the dynamics of these guest molecules and (ii) their effect on the secondary ‘β’ and main ‘’ relaxations of the host polymeric matrix. The system considered here is the glassy poly(methyl metacrylate) modified by introduction and desorption of methanol. The dynamics of the system is observed by means of low-frequency mechanical and wide band dielectric spectroscopies. The presence of small molecules in the PMMA glassy matrix induces several effects, namely (i) a strong relaxation peak develops at low temperature (near 120 K at 1 Hz and called _m in the following), (ii) the strength of the β relaxation is increased while the temperature of the maximum shifts towards the low temperatures, (iii) a sharp peak appears superimposed on the β peak, and finally (iv) the relaxation shifts towards the low temperatures. Dielectric and mechanical spectroscopies results are in agreement and make it possible to capture the dynamical behavior in a wide frequency range (eight decades). The experimental results are explained on the basis of physical concepts recently introduced in the physics of glassy matter: cooperativity and nanoheterogeneity. In particular, the low-temperature relaxation process _m is attributed to cooperative motions in methanol clusters which form in the nanoheterogeneous polymeric matrix, in agreement with small angle X-rays scattering and low-frequency Raman scattering observations recently reported.     

Internal friction in martensitic, ferritic and bainitic carbon steel; cold work effects

We present the comparative analysis of the temperature dependent internal friction (IF) spectra for 1.23 wt.% carbon steel with martensitic, bainitic or ferritic structure as well as cold-work effects. Samples that have a martensitic structure at room temperature show a characteristic spectrum consisting of five peaks and an exponential background. Tempering at 800 K transforms the sample structure to a completely ferritic one. All peaks are erased upon tempering, except the peak P5 identified as a Snoek–Köster (S-K) relaxation, the amplitude of which is however drastically reduced. The Snoek–Köster peak is also present in the bainitic structure as well as in initial ferrite, but with an amplitude much lower than in martensitic samples. Cold work performed on tempered samples at room temperature either by bending or roll milling is followed by the formation of a very broad double peak between 200 and 300 K. A similar peak is also found in initial ferrite, which has been subjected to heavy machining. A local minimum in the IF spectrum is found at the temperature of cold work and post-aging. This minimum is the effect of dislocation pinning by carbon precipitates.     

Interaction between substitutional and interstitial solute atoms in α iron studied by isothermal mechanical spectroscopy

The interaction of interstitial nitrogen with substitutional alloying elements has been studied by measuring the Snoek relaxation in very dilute Fe–X–N ternary alloys (X: V, Cr, Mn, Mo). Isothermal measurements by the sub-resonance forced-vibration technique have revealed characteristic influence of substitutional solutes on the Snoek relaxation, which can be understood as trapping of N atoms at neighbouring sites of X atoms. The interaction energy has been evaluated by comparing the relaxation profiles observed experimentally with those calculated theoretically. The values thus obtained are of the order of 0.1 eV, with the magnitude being larger for elements of smaller group numbers, and are similar to those in the γ and liquid phases.     

Flat coil-based tunnel diode oscillator enabling to detect the real shape of the superconductive transition curve and capable of imaging the properties of HTSC films with high spatial resolution

Owing to a pick-up coil's flat design, relatively low MHz-range operation frequency, and six orders relative resolution a flat coil-based tunnel diode oscillator has advantages, compared to all other methods. They become crucial in studies with thin high-T_c superconductivity (HTSC) materials (with small signals), especially at the start of the Cooper pairs’ formation. Due to this the superconductivity precursor ‘paramagnetic’ effect was detected recently in YBaCuO films at N/S transition. It precedes Meissner ejection and specifies details of the shape of the transition curve. We discuss the influence of the currents on this effect, and the relationship between the quality of the material and the shape of the effect. A new imaging device has also been created based on this test method (using a focused He–Ne laser beam as a probing signal), capable of imaging the properties of HTSC films with 3 μm spatial resolution. The method is based on detection of the inductance and Q-factor value changes of a single-layer flat coil, placed at the face of the sample. This leads to frequency and/or amplitude changes of the stable oscillator. The test device enabled 2D-mapping of the grain structure of a bridge-shaped YBaCuO film. Basically, the method is capable of imaging 2D-current distribution in thin HTS with sub-μm spatial-resolution, using non-bolometric response. However, the achieved resolution 3 μm of a bolometric nature (in a given device with 3.5 mm-size coil) by no means is limited by the abilities of the method, but mainly, it depends on how narrowly it is possible to focus the probing beam, while the own resolution of a present flat coil-based technique is better than 0.1 μm, and can be improved essentially by reducing the coil size.     

Quantitative determination of the volume fraction of intergranular amorphous phase in sintered silicon nitride

In this paper, a commercial liquid phase sintered silicon nitride with Y₂O₃ and Al₂O₃ additives is investigated. The material is characterised by a large, and stable, internal friction peak near 1150 °C. The peak is linked with the glass transition in intergranular amorphous volumes, whose presence is confirmed with transmission electron microscopy. An estimate of the volume fraction of the amorphous phase is calculated from the difference in stiffness below and above the glass transition temperature. The procedure relies on accurate Young’s modulus data, which were obtained with the impulse excitation technique (IET). The amount of amorphous pocket phase was estimated at 12.4 vol.%. For the first time, microstructural evidence supporting this estimate is obtained, using analysis of scanning electron microscopy (SEM) images. The rather large amount of amorphous matter explains the limited high temperature potential of the material, which was primarily and successfully developed for wear applications.     

Maximum mass flow ratio due to secondary flow choking in an ejector refrigeration system

The occurrence of flow choking in an ejector of an ejector refrigeration system (ERS) was analysed and a model for predicting the maximum flow ratio of the ejector was developed. The multi-parameter equation to calculate the mass flow ratio takes into account the performance of the primary nozzle, the flow entrainment and mixing relating to ejector geometry and operating conditions. We validated the model using the reported experimental data of refrigerant R113, R141b and steam ERS. The present model was shown to provide better accuracy compared with results obtained by applying the existing 1-D ejector theory. We discussed the application of the model and highlighted the significance of the parameters for future work.