The impact of low-pressure treatment on the crystal structure, morphology, and chemical composition of ettringite, due to their major importance with respect to processability (i.a., drying conditions) and to the analysis of ettringite-containing samples, is examined utilizing X-ray diffraction, thermogravimetric analysis, Raman spectroscopy, and environmental scanning electron microscopy. Synthetic ettringite was treated for various durations (5 min up to 72 h) and at two different levels of low-pressure (4.0 mbar and 60 µbar). Evaluation showed a correlation between the procedural parameters (time and pressure), the chemical composition, and the morphology of ettringite. The experiments reveal that, when exposed to 4 mbar pressure, nearly no changes occur in the ettringite’s morphology, whereas the crystals undergo swelling and slight deformations at very low pressures (60 µbar and 35.3 nbar), which is attributed to the loss of bound water and the partial transformation from ettringite to quicklime, anhydrite, and calcium aluminate. Furthermore, the strongly dehydrated ettringite shows the same morphology.
La2NiO4+δ particles with a plate-like morphology were prepared from a NaOH melt by molten-flux synthesis. For this purpose, the intermediates from a sol–gel process were used as reactants. Using powder X-ray diffraction, the sol–gel intermediates were identified as a mixture of tetragonal La2O2CO3 and cubic NiO. The existence of NiO was also confirmed by transmission electron microscopy in combination with electron-energy loss spectroscopy. The ultrafine mixed sol–gel intermediates were then mixed with NaOH powder and additional water in a nickel crucible and heated to 673 K for 8 h. The chemical reactions in the air during the molten-flux synthesis and the influence of the salt on the formation of La2NiO4+δ were examined by thermogravimetric analysis. The powder X-ray diffraction indicated a K2NiF4-type tetragonal structure with the I4/mmm space group for the reaction product. The scanning electron microscopy showed plate-like La2NiO4+δ crystals with a length and thickness of approximately 9 µm and 2 µm, respectively, while the energy-dispersive X-ray spectroscopy revealed a homogeneous distribution of lanthanum and nickel in the product powder. The influence of the processing parameters on the product generation, as well as on the size and morphology of the La2NiO4+δ particles, was systematically studied.
16 December 2021 in Journal of Electronic Materials
Ceramic composites composed of oxide materials have been synthesized by reaction sintering of Ca3Co4O9 with BiCuSeO nanosheets. In situ x-ray diffraction and thermogravimetric analyses of the compound powders were conducted to understand the phase transformations during heating up to 1173 K. Further thermogravimetric analyses investigated the thermal stability of the composites and the completion of reaction sintering. The microstructure of the formed phases after reaction sintering and the composition of the composites were investigated for varying mixtures. Depending on the amount of BiCuSeO used, the phases present and their composition differed, having a significant impact on the thermoelectric properties. The increase of the electrical conductivity at a simultaneously high Seebeck coefficient resulted in a large power factor of 5.4 $$\mu $$ W cm−1 K−2, more than twice that of pristine Ca3Co4O9.
18 December 2023 in Angewandte Chemie International Edition
Ruddlesden‐Popper‐type oxides exhibit remarkable chemical stability in comparison to perovskite oxides. However, they display lower oxygen permeability. We present an approach to overcome this trade‐off by leveraging the anisotropic properties of Nd2NiO4+δ. Its (a,b)‐plane, having oxygen diffusion coefficient and surface exchange coefficient several orders of magnitude higher than its c‐axis, can be aligned perpendicular to the gradient of oxygen partial pressure by a magnetic field (0.81 T). A stable and high oxygen flux of 1.40 mL min−1 cm−2 was achieved for at least 120 h at 1223 K by a textured asymmetric disk membrane with 1.0 mm thickness under the pure CO2 sweeping. Its excellent operational stability was also verified even at 1023 K in pure CO2. These findings highlight the significant enhancement in oxygen permeation membrane performance achievable by adjusting the grain orientation. Consequently, Nd2NiO4+δ emerges as a promising candidate for industrial applications in air separation, syngas production, and CO2 capture under harsh conditions.