A series of reduced-charge montmorillonites with cation exchange capacities of 89, 73, 49 and 29% of the starting mineral was prepared from a Li-saturated smectite (Kriva Palanka, Republic of Macedonia) by heating at 110, 130, 160 and 300°C for 24 h (samples KP110 – KP300, respectively). Hydration properties of this series were investigated gravimetrically and by in situ XRD at different relative humidities (RHs). In the gravimetric experiments, higher water contents were observed for desorption than for sorption and hysteresis was present over the whole range of RHs for all the samples. The parent montmorillonite and the samples KP110 and KP130 retained similar amounts of water under the same conditions, thus showing that the decreased negative charge on the layers had minor effect on the water uptake at all investigated RHs. Significantly decreased water content was retained by KP160 while KP300 contained only 8% water at 100% RH. The d001 values of the parent montmorillonite and the samples KP110 and KP130 increased with RH, while those of KP160 and KP300 were independent of RH and remained at ∼10.4 and ∼9.6 Å, respectively.

Mastery of strengthening strategies to achieve high-capacity anodes for lithium-ion batteries can shed light on understanding the nature of diffusion-induced stress and offer an approach to use submicro-sized materials with an ultrahigh capacity for large-scale batteries. Here, we report solute strengthening in a series of silicon (Si)–germanium (Ge) alloys. When the larger solute atom (Ge) is added to the solvent atoms (Si), a compressive stress is generated in the vicinity of Ge atoms. This local stress field interacts with resident dislocations and subsequently impedes their motion to increase the yield stress in the alloys. The addition of Ge into Si substantially improves the capacity retention, particularly in Si0.50Ge0.50, aligning with literature reports that the Si/Ge alloy showed a maximum yield stress in Si0.50Ge0.50. In situ X-ray diffraction studies on the Si0.50Ge0.50 electrode show that the phase change undergoes three subsequent steps during the lithiation process: removal of surface oxide layer, formation of cluster-size Lix(Si,Ge), and formation of crystalline Li15(Si,Ge)4. Furthermore, the lithiation process starts from higher index facets, i.e., (220) and (311), then through the low index facet (111), suggesting the orientation-dependence of the lithiation process in the Si0.50Ge0.50 electrode.

Organo-kenyaites were prepared from a cetyltrimethylammonium hydroxide (C16TMAOH) solution and solid sodium kenyaite (Na2Si22O45.10H2O) mixture. The effect of the initial cetyltrimethylammonium solution on the structure of the intercalated materials was investigated by CHN analyses, X-ray diffraction (XRD), thermogravimetric analysis, SEM, and 29Si and 13C solid NMR techniques. For C16TMAOH concentration 0.25 mM, the Na+ cations were fully exchanged. Initial C16TMAOH concentrations higher than 0.25 mM had little effect on the intercalated amount of C16TMA+ cations. The organic cations content reached a plateau of 0.66 mmol/g. The arrangement model of C16TMA+ cations corresponded to a tilt of the organic cations to the silicate layers with an angle of 42° as deduced by XRD studies. The C16TMA+ cations exhibited mainly trans-configuration of the methyl chains, as was shown by solid 13C NMR. The thermal stability of the organo-silicates was studied using in situ FTIR and in situ XRD in the range 25–450°C. The C16TMA-kenyaites were stable at temperatures below 200°C. They collapsed at higher temperatures due to the decomposition of the intercalated surfactants. These organo-kenyaites were used to remove the acidic dye molecule, eosin. The removal tests were performed at varying conditions of initial dye concentrations, organic content in the organo-kenyaites and heating temperatures. In general, the organic modification improved the removal capacity of the Na-kenyaite from 2 mg of eosin/g to 60 mg of eosin/g, and this capacity was related to the organic contents and the calcination temperatures of the organo-kenyaites.

In this work, the reduction mechanism of potassium chromate (K2CrO4) was investigated via in situ high-temperature X-ray diffraction coupled with Fourier transform infrared spectroscopy. During the hydrogen reduction of K2CrO4, the formation of K3CrO4, KCrO2, and KxCrO2 were detected for the first time. The study discovered that K2CrO4 was firstly reduced to K3CrO4 and an amorphous Cr(III) intermediate product at low temperature (400–500 °C). Moreover, the K3CrO4 was the only crystalline material at this stage. As the temperature increased, a stabilized amorphous CrOOH was formed. At a high temperature (550–700 °C), KCrO2 was generated. Interestingly, a portion of KCrO2 was spontaneously decomposed during the hydrogen reduction, accompanying by the formation of K0.7CrO2. Finally, the results clearly illustrated the reduction mechanism of K2CrO4: K2CrO4 → K3CrO4 → amorphous intermediate → KCrO2.

In situ laboratory-based and in situ synchrotron X-ray diffraction techniques were employed to study quantitatively the strain-induced austenite-to-martensite (A–M) transformation in thermally cycled (TC) superelastic NiTi alloys. The propagation of the A–M interfaces and the evolution of the microstructure were traced during uniaxial tensile loading. It was shown that the TC material exhibits localized transformation via the propagation of transformation bands. The amount of the martensite phase depends approximately linearly on the applied strain. Analysis of the broadening of the austenite diffraction lines indicates the presence of highly deformed austenite grains within the transformation bands. Analysis of the austenite diffraction-line shifts indicates that the overall lattice strain in the (retained) austenite in the transformation bands differs from that of the austenite in the adjacent untransformed regions.

Investigation into the early hydration of Portland cement was performed by in situ X-ray diffraction (XRD). Technical white cement was used for the XRD analysis on a D5000 diffractometer (Siemens). All diffraction patterns of the in situ measurement which were recorded up to 22 h of hydration at defined temperatures were analyzed by Rietveld refinement. The resulting phase composition was transformed with respect to free water and C-S-H leading to the total composition of the cement paste. The hydration reactions can be observed by dissolution of clinker phases as well as by the formation of the hydrate phases ettringite and portlandite. With increasing temperatures the reactions proceed faster. The formation of ettringite is directly influenced by the rate of dissolution of anhydrite and tricalcium aluminate (C3A). The beginning of the main period of hydration is marked by the start of portlandite formation. The experiments point out that a quantitative phase analysis of the cement hydration is feasible with standard laboratory diffractometers.

The two-dimensional XRD (GADDS) was used to characterize the microstructure of an applied self-leveling compound (SLC). A calcium aluminate cement based SLC was prepared on two different substrates (water absorbent and nonwater absorbent) to determine the vertical distribution of the crystalline phases. The application of the GADDS enables the detection of the phase composition of the hydrating mortar in horizontal slices. Thus the analysis could be carried out in position-sensitive mode at three different areas: near the bottom, in the center, and at the top of the mortar. For investigation of SLCs from the very early hydration stage up to 10 h of hydration, a custom-made in situ sample holder for the measurements was designed and constructed. The combination of the GADDS and the custom-made in situ sample holder provides the possibility to characterize additionally the time-dependent phase composition within the SLC. The nonabsorbent substrate has no effect on the hydration of the binder phases but the absorbent substrate influences the formation of ettringite. In the top layer of the SLC the ettringite content is reduced during the first hours of hydration. The absorbing forces of the substrate lead to migration of the mix water to the substrate. This lack of water results in the reduced formation of ettringite.

We report on the size relationship of Au and Au-Pt nanoparticles that were synthesised on silica and anatase phase titania supports. Deposition-precipitation (DP) of metal chlorides with the addition of urea and ammonium hydroxide was used to produce the nanoparticles. The relative particle size relationship of the Au and Au-Pt nano particles (NP's) was investigated, relating the Pt concentration and the support polymorph over a temperature range. It was found, with the use of in-situ variable temperature powder X-ray diffraction (VT-PXRD) and transmission electron microscopy (TEM), that the addition of Pt to the Au system corresponded to a reduction in particle size over a broad temperature range.