Acoustic emissions from spin crossover complexes.

Acoustic emission from the compounds [Fe(HB(tz)3)2] and [Fe(Htrz)(trz)2]BF4 was detected during the thermally induced spin transition and is correlated with simultaneously recorded calorimetric signals. We ascribe this phenomenon to elastic waves produced by microstructural and volume changes accompanying the spin transition. Despite the perfect reversibility of the spin state switching (seen by the calorimeter), the acoustic emission activity decreases for successive thermal cycles, revealing thus irreversible microstructural evolution of the samples. The acoustic emission signal amplitude and energy probability distribution functions followed power-law behavior and the characteristic exponents were found to be similar for the two samples both on heating and cooling, indicating the universal character, which is further substantiated by the well scaled average temporal shapes of the avalanches.

Scaling of Average Avalanche Shapes for Acoustic Emission during Jerky Motion of Single Twin Boundary in Single-Crystalline Ni2MnGa.

Temporal average shapes of crackling noise avalanches, U(t) (U is the detected parameter proportional to the interface velocity), have self-similar behavior, and it is expected that by appropriate normalization, they can be scaled together according to a universal scaling function. There are also universal scaling relations between the avalanche parameters (amplitude, A, energy, E, size (area), S, and duration, T), which in the mean field theory (MFT) have the form E∝A3, S∝A2, S∝T2. Recently, it turned out that normalizing the theoretically predicted average U(t) function at a fixed size, U(t)=atexp-bt2 (a and b are non-universal, material-dependent constants) by A and the rising time, R, a universal function can be obtained for acoustic emission (AE) avalanches emitted during interface motions in martensitic transformations, using the relation R~A1-φ too, where φ is a mechanism-dependent constant. It was shown that φ also appears in the scaling relations E~A3-φ and S~A2-φ, in accordance with the enigma for AE, that the above exponents are close to 2 and 1, respectively (in the MFT limit, i.e., with φ= 0, they are 3 and 2, respectively). In this paper, we analyze these properties for acoustic emission measurements carried out during the jerky motion of a single twin boundary in a Ni50Mn28.5Ga21.5 single crystal during slow compression. We show that calculating from the above-mentioned relations and normalizing the time axis of the average avalanche shapes with A1-φ, and the voltage axis with A, the averaged avalanche shapes for the fixed area are well scaled together for different size ranges. These have similar universal shapes as those obtained for the intermittent motion of austenite/martensite interfaces in two different shape memory alloys. The averaged shapes for a fixed duration, although they could be acceptably scaled together, showed a strong positive asymmetry (the avalanches decelerate much slower than they accelerate) and thus did not show a shape reminiscent of an inverted parabola, predicted by the MFT. For comparison, the above scaling exponents were also calculated from simultaneously measured magnetic emission data. It was obtained that the φ values are in accordance with theoretical predictions going beyond the MFT, but the AE results for φ are characteristically different from these, supporting that the well-known enigma for AE is related to this deviation.

Thermodynamic Analysis of Anomalous Shape of Stress-Strain Curves for Shape Memory Alloys.

In some shape-memory single crystals the stress-strain (σ~ε) curves, belonging to stress induced martensitic transformations from austenite to martensite at fixed temperature, instead of being the usual slightly increasing function or horizontal, have an overall negative slope with sudden stress drops in it. We discuss this phenomenon by using a local equilibrium thermodynamic approach and analysing the sign of the second derivative of the difference of the Gibbs free energy. We show that, considering also the possible nucleation and growth of two martensite structural modifications/variants, the stress-strain loops can be unstable. This means that the overall slope of the uploading branch of the stress-strain curve can be negative for smooth transformation if the second martensite, which is more stable with larger transformation strain, is the final product. We also show that local stress-drops on the stress-strain curve can appear if the nucleation of the second martensite is difficult, and the presence of such local stress-drops alone can also result in an overall negative slope of the stress-strain curves. It is illustrated that the increase of the temperature of the thermal recovery during burst-like transition is a measure of the change of the nucleation energy: the more stable martensite has larger nucleation energy.

Clustering Characterization of Acoustic Emission Signals Belonging to Twinning and Dislocation Slip during Plastic Deformation of Polycrystalline Sn.

Results of acoustic emission (AE) measurements, carried out during plastic deformation of polycrystalline Sn samples, are analyzed by the adaptive sequential k-means method. The acoustic avalanches, originating from different sources, are separated on the basis of their spectral properties, that is, sorted into clusters, presented both on the so-called feature space (energy-median frequency plot) and on the power spectral density (PSD) curves. We found that one cluster in every measurement belongs to background vibrations, while the remaining ones are clearly attributed to twinning as well as dislocation slips at −30 °C and 25 °C, respectively. Interestingly, fingerprints of the well-known "ringing" of AE signals are present in different weights on the PSD curves. The energy and size distributions of the avalanches, corresponding to twinning and dislocation slips, show a bit different power-law exponents from those obtained earlier by fitting all AE signals without cluster separation. The maximum-likelihood estimation of the avalanche energy (ε) and size (τ) exponents provide ε=1.57±0.05 (at −30 °C) and ε=1.35±0.1 (at 25 °C), as well as τ=1.92±0.05 (at −30 °C) and τ= 1.55±0.1 (at 25 °C). The clustering analysis provides not only a manner to eliminate the background noise, but the characteristic avalanche shapes are also different for the two mechanisms, as it is visible on the PSD curves. Thus, we have illustrated that this clustering analysis is very useful in discriminating between different AE sources and can provide more realistic estimates, for example, for the characteristic exponents as compared to the classical hit-based approach where the exponents reflect an average value, containing hits from the low-frequency mechanical vibrations of the test machine, too.

Denouement of the Energy-Amplitude and Size-Amplitude Enigma for Acoustic-Emission Investigations of Materials.

There are many systems producing crackling noise (avalanches) in materials. Temporal shapes of avalanches, U(t) (U is the detected voltage signal, t is the time), have self-similar behaviour and the normalized U(t) function (e.g., dividing both the values of U and t by S1/2, where S is the avalanche area), averaged for fixed S, should be the same, independently of the type of materials or avalanche mechanisms. However, there are experimental evidences that the temporal shapes of avalanches do not scale completely in a universal way. The self-similarity also leads to universal power-law-scaling relations, e.g., between the energy, E, and the peak amplitude, Am, or between S and Am. There are well-known enigmas, where the above exponents in acoustic emission measurements are rather close to 2 and 1, respectively, instead of E~Am3 and S~Am2, obtained from the mean field theory, MFT. We show, using a theoretically predicted averaged function for the fixed avalanche area, U(t)=atexp(-bt2) (where a and b are non-universal, material-dependent constants), that the scaling exponents can be different from the MFT values. Normalizing U by Am and t by tm (the time belonging to the Am: rise time), we obtain tm~Am1-φ (the MFT values can be obtained only if φ would be zero). Here, φ is expected to be material-independent and to be the same for the same mechanism. Using experimental results on martensitic transformations in two different shape-memory single-crystals, φ = 0.8 ± 0.1 was obtained (φ is the same for both alloys). Thus, dividing U by Am as well as t by Am1-φ (~tm) leads to the same common, normalized temporal shape for different, fixed values of S. This normalization can also be used in general for other experimental results (not only for acoustic emission), which provide information about jerky noises in materials.

Acoustic Emission Characteristics and Change the Transformation Entropy after Stress-Induced Martensite Stabilization in Shape Memory Ni53Mn25Ga22 Single Crystal.

Measurements have been carried out to compare stress-induced martensite stabilization aged (SIM-aged) and as grown shape memory Ni53Mn25Ga22 single crystals with the means of simultaneous differential scanning calorimetry (DSC) and acoustic emission (AE). Contrary to expectations, the position of the hysteresis practically did not change, whilst the width of the hysteresis increased, and the forward and reverse transitions became sharper in the SIM-aged sample. The energy distributions of acoustic hits showed regular power law behaviour and the energy exponents were slightly different for heating and cooling; this asymmetry had different signs for the SIM-aged and as grown samples. During heating, in accordance with the sharper transitions observed in the DSC runs, two well-marked jumps could be seen on the plot of cumulative number of the acoustic emission events. Therefore, these were attributed to high sudden jumps in the phase transition during heating observed in the DSC. The effect of the SIM-aging on the transformation entropy was also investigated and it was found that it was about 36% less in the case of the SIM-aged sample.

Determination of the compositions of the DIGM zone in nanocrystalline Ag/Au and Ag/Pd thin films by secondary neutral mass spectrometry.

Alloying by grain boundary diffusion-induced grain boundary migration is investigated by secondary neutral mass spectrometry depth profiling in Ag/Au and Ag/Pd nanocrystalline thin film systems. It is shown that the compositions in zones left behind the moving boundaries can be determined by this technique if the process takes place at low temperatures where solely the grain boundary transport is the contributing mechanism and the gain size is less than the half of the grain boundary migration distance. The results in Ag/Au system are in good accordance with the predictions given by the step mechanism of grain boundary migration, i.e., the saturation compositions are higher in the slower component (i.e., in Au or Pd). It is shown that the homogenization process stops after reaching the saturation values and further intermixing can take place only if fresh samples with initial compositions, according to the saturation values, are produced and heat treated at the same temperature. The reversal of the film sequence resulted in the reversal of the inequality of the compositions in the alloyed zones, which is in contrast to the above theoretical model, and explained by possible effects of the stress gradients developed by the diffusion processes itself.

Formation of Cu x Au1- x phases by cold homogenization of Au/Cu nanocrystalline thin films.

It is shown, by using depth profiling with a secondary neutral mass spectrometer and structure investigations by XRD and TEM, that at low temperatures, at which the bulk diffusion is frozen, a complete homogenization can take place in the Cu/Au thin film system, which leads to formation of intermetallic phases. Different compounds can be formed depending on the initial thickness ratio. The process starts with grain boundary interdiffusion, which is followed by a formation of reaction layers at the grain boundaries that leads to the motion of the newly formed interfaces perpendicular to the grain boundary plane. Finally, the homogenization finishes when all the pure components have been consumed. The process is asymmetric: It is faster in the Au layer. In Au(25nm)/Cu(50nm) samples the final state is the ordered AuCu3 phase. Decrease of the film thicknesses, as expected, results in the acceleration of the process. It is also illustrated that changing the thickness ratio either a mixture of Cu-rich AuCu and AuCu3 phases (in Au(25nm)/Cu(25nm) sample), or a mixture of disordered Cu- as well as Au-rich solid solutions (in Au(25nm)/Cu(12nm) sample) can be produced. By using a simple model the interface velocity in both the Cu and Au layers were estimated from the linear increase of the average composition and its value is about two orders of magnitude larger in Au (ca. 10(-11) m/s) than in Cu (ca. 10(-13) m/s).