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Copper sulfide shows some unique physico-chemical properties that make it appealing as a cathode active material (CAM) for solid-state batteries (SSBs). The most peculiar feature of the electrode reaction is the reversible formation of μm-sized Cu crystals during cycling, despite its large theoretical volume change (75%). Here, the dynamic microstructural evolution of CuS cathodes in SSBs is studied using in situ synchrotron X-ray tomography. The formation of μm-sized Cu within the CAM particles can be clearly followed. This process is accompanied by crack formation that can be prevented by increasing the stack pressure from 26 to 40 MPa. Both the Cu inclusions and cracks show a preferential orientation perpendicular to the cell stack pressure, which can be a result of a z-oriented expansion of the CAM particles during lithiation. In addition, cycling leads to a z-oriented reversible displacement of the cathode
pellet, which is linked to the plating/stripping of the Li counter electrode. The pronounced structural changes cause pressure changes of up to 6 MPa within the cell, as determined by operando stack pressure measurements. Reasons for the reversibility of the electrode reaction are discussed and are attributed to the favorable combination of soft materials.
An extensive set of information about the diffracting volume is carried by EBSD patterns: the crystal lattice, the reciprocal lattice, the crystal structure, the crystal symmetry, the mean periodic number of the diffracting phase, the source point from where it has been projected (projection centre), the crystal orientation, the sample topography (local tilt), the (preparation) quality of defect density of the crystal, and possible pattern overlaps. Some of this information is used regularly in conventional EBSD analyses software while others are still waiting for a more widespread application. Despite the wealth of information available, the accuracy and precision of the data that are presently extracted from conventional EBSD patterns are often well below the actual physical limits. Using a selection of example applications, we will demonstrate the gain in angular resolution possible using relatively low-resolution patterns of approximately 20k pixels in combination with pattern matching (PM) approaches. In this way, fine details in a microstructure can be revealed which would otherwise be hidden in the orientation noise.
Calcium alkali phosphates Ca(Na,K)PO4 are main constituents of bioceramics and thermochemically produced phosphorus fertilizers because of their bioavailability. Sparse thermodynamic data are available for the endmembers CaNaPO4 and CaKPO4. In this work, the missing data were determined for the low-temperature phase modifications of the endmembers CaNaPO4 and CaKPO4 and three intermediate Ca(Na,K)PO4 compositions. Standard enthalpy of formation ranges from - 2018.3 ± 2.2 kJ mol-1 to - 2030.5 ± 2.1 kJ mol-1 and standard entropy from 137.2 ± 1.0 J mol-1 K-1 to 148.6 ± 1.0 J mol-1 K-1 from sodium endmember b-CaNaPO4 to potassium endmember b0-CaKPO4.
Thermodynamic functions are calculated up to 1400 K for endmembers and the sodium-rich intermediate phase b-Ca(Na0.93K0.07)PO4. Functions above 640 K are extrapolated because of the phase transition from low- to high-temperature phase. Impurities in the synthesized intermediate phases c-Ca(Na0.4K0.6)PO4 and c-Ca Na0.35K0.65)PO4 and one additional phase transition around 500 K impeded the determination of high-temperature thermodynamic functions. In general, data for phase transition temperatures agree with the previously reported phase diagrams.
The current paper presents residual stress analyses of large scale LTT (Low Transformation Temperature) welds. LTT filler materials are specially designed for residual stress engineering by means of an adjusted martensite phase transformation. Controlling the level of mostly detrimental residual stresses already during the welding process would be highly attractive as time and cost consuming post processing may be prevented. In large scale welds the residual stress state is influenced by the heat control (e.g. interpass temperature) during welding. Therefore, welding residual stresses are studied here putting the focus on the influence of welding process parameters while joining heavy steel sections with a thickness of 25 mm. The residual stress state was determined at the top surface using X-ray diffraction as well as in the bulk by neutron diffraction. The results show that control of the interpass temperature is vital for the residual stresses present in the joints. This accounts for the top surface but is most pronounced for the bulk of the welds. While high interpass temperatures are appropriate to induce compressive residual stresses in the weld metal, low interpass temperatures favor unwanted tensile residual stresses instead.
A combined experimental numerical approach is applied to determine the transformation induced plasticity (TRIP)-parameter K for different strength low-alloy steels of grade S355J2+N and S960QL as well as the super martensitic filler CN13-4-IG containing 13 wt% chromium and 4 wt% nickel. The thermo-physical analyses were conducted using a Gleeble® 3500 facility. The thermal histories of the specimens to be tested were extracted from corresponding simulations of a real gas metal arc weldment. In contrast to common TRIP-experiments which are based on complex specimens a simple flat specimen was utilized together with an engineering evaluation method. The evaluation method was validated with literature values for the TRIP-parameter. It could be shown that the proposed approach enables a correct description of the TRIP behavior.
Cold cracking resistance is a relevant evaluation criterion for welded joints and affected by residual stresses which result from the welding procedure. Compressive residual stresses can thereby have a positive influence on preventing cracking. A unique possibility of generating compressive residual stresses already during the welding procedure is offered by the so-called Low Transformation Temperature (LTT) filler wires. Compared to conventional wires, these materials show decreased phase transformation temperatures which can work against the cooling-specific contraction. In consequence, distinct compressive residual stresses can be observed within the weld and adjacent areas. The strength of these fillers makes them potentially applicable to high-strength steel welding. Investigations were carried out to determine the phase transformation behaviour of different LTT-filler materials. Transformation temperatures were identified using Single Sensor Differential Thermal Analysis (SS-DTA). Additionally Synchrotron radiation was used to measure the transformation kinetics of all involved crystalline phases during heating and cooling of a simulated weld thermal cycle.
For the safety and cost efficiency of welded high-strength steel structures, precise knowledge of the level and distribution of welding- and cooling-specific stresses and residual stresses is essential, since they exert a decisive influence on strength, crack resistance, and finally on the bearable service load. This paper presents innovative filler materials, of which the phase transformation temperature was deliberately adjusted via the chemical composition. The transformation behaviour of these martensitic Low Transformation Temperature (LTT-) filler materials shows direct effects on the local residual stresses in the weld and the HAZ. These effects can purposefully be exploited to counteract the thermally induced shrinkage of the material and to produce significant compressive residual stresses in the weld. Comparative welding experiments were carried out on 690 MPa high-strength base materials using various LTT-filler materials. High energy synchrotron radiation was used for residual stress measurement. Particularly the use of high energy synchrotron radiation makes it possible to detect the residual stress condition fast without destruction of material. Thereby, residual stress depth gradients can be determined simultaneously without removing material. In steel, gradients of up to 150 µm can be resolved in such a way. Furthermore, the application of high energy radiation permits determination of residual stresses of any available residual austenite contents. Results show significant dependence of transformation temperatures on the resulting residual stress level and distribution.