scholarly journals In-Situ Kinetic Investigation of Calcium Aluminate Formation

Ceramics ◽  
2018 ◽  
Vol 1 (1) ◽  
pp. 175-197 ◽  
Author(s):  
John Salasin ◽  
Claudia Rawn

Rapid in-situ non-ambient X-ray diffraction represents a powerful tool for characterizing the evolution of crystalline materials in real time. The calcium aluminate system and formation of Ca12Al14O33 (C12A7) is particularly sensitive to processing conditions. This report characterizes the kinetic pathways to thermodynamic equilibrium as a function of atmosphere (ambient, dry, and vacuum) and reactant heterogeneity (as-received, milled, and sol-gel reactants). When reactants are heterogenous (as-received and milled), intermediary phases of Ca3Al2O6 (C3A) and CaAl2O4 (CA) are observed as the route to C12A7 formation and Ca5Al6O14 (C5A3) is only observed as a decomposition product of C12A7. When reactants are heterogenous, C12A7 is only thermodynamically favorable under ambient conditions due to the stability provided by hydration. When reactants are homogenous (sol-gel), direct crystallization of C12A7 from an amorphous precursor is observed at low temperature regardless of atmosphere defining C12A7 as the kinetic equilibrium. These findings accurately define the heterogenous formation pathways and report for the first time the formation of C12A7 under a carbon-free vacuum environment.

Nanomaterials ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 1885
Author(s):  
Xinyu Wu ◽  
Feng Yang ◽  
Jian Gan ◽  
Zhangqian Kong ◽  
Yan Wu

The silver particles were grown in situ on the surface of wood by the silver mirror method and modified with stearic acid to acquire a surface with superhydrophobic and antibacterial properties. Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and X-ray energy spectroscopy (XPS) were used to analyze the reaction mechanism of the modification process. Scanning electron microscopy (SEM) and contact angle tests were used to characterize the wettability and surface morphology. A coating with a micro rough structure was successfully constructed by the modification of stearic acid, which imparted superhydrophobicity and antibacterial activity to poplar wood. The stability tests were performed to discuss the stability of its hydrophobic performance. The results showed that it has good mechanical properties, acid and alkali resistance, and UV stability. The durability tests demonstrated that the coating has the function of water resistance and fouling resistance and can maintain the stability of its hydrophobic properties under different temperatures of heat treatment.


2014 ◽  
Vol 70 (a1) ◽  
pp. C94-C94
Author(s):  
Pawel Kuczera ◽  
Walter Steurer

The structure of d(ecagonal)-Al-Cu-Rh has been studied as a function of temperature by in-situ single-crystal X-ray diffraction in order to contribute to the discussion on energy or entropy stabilization of quasicrystals (QC) [1]. The experiments were performed at 293 K, 1223 K, 1153 K, 1083 K, and 1013 K. A common subset of 1460 unique reflections was used for the comparative structure refinements at each temperature. The results obtained for the HT structure refinements of d-Al-Cu-Rh QC seem to contradict a pure phasonic-entropy-based stabilization mechanism [2] for this QC. The trends observed for the ln func(I(T1 )/I(T2 )) vs.|k⊥ |^2 plots indicate that the best on-average quasiperiodic order exists between 1083 K and 1153 K, however, what that actually means is unclear. It could indicate towards a small phasonic contribution to entropy, but such contribution is not seen in the structure refinements. A rough estimation of the hypothetic phason instability temperature shows that it would be kinetically inaccessible and thus the phase transition to a 12 Å low T structure (at ~800 K) is most likely not phason-driven. Except for the obvious increase in the amplitude of the thermal motion, no other significant structural changes, in particular no sources of additional phason-related configurational entropy, were found. All structures are refined to very similar R-values, which proves that the quality of the refinement at each temperature is the same. This suggests, that concerning the stability factors, some QCs could be similar to other HT complex intermetallic phases. The experimental results clearly show that at least the ~4 Å structure of d-Al-Cu-Rh is a HT phase therefore entropy plays an important role in its stabilisation mechanism lowering the free energy. However, the main source of this entropy is probably not related to phason flips, but rather to lattice vibrations, occupational disorder unrelated to phason flips like split positions along the periodic axis.


1996 ◽  
Vol 459 ◽  
Author(s):  
E. Ching-Prado ◽  
W. Pérez ◽  
A. Reynés-Figueroa ◽  
R. S. Katiyar ◽  
D. Ravichandran ◽  
...  

ABSTRACTThin films of SrBi2Nb2O9 (SBN) with thicknesses of 0.1, 0.2, and 0.4 μ were grown by Sol-gel technique on silicon, and annealed at 650°C. The SBN films were investigated by Raman scatering for the first time. Raman spectra in some of the samples present bands around 60, 167, 196, 222, 302, 451, 560, 771, 837, and 863 cm−1, which correspond to the SBN formation. The study indicates that the films are inhomogeneous, and only in samples with thicknesses 0.4 μ the SBN material was found in some places. The prominent Raman band around 870 cm−1, which is the A1g mode of the orthorhombic symmetry, is assigned to the symmetric stretching of the NbO6 octahedrals. The frequency of this band is found to shift in different places in the same sample, as well as from sample to sample. The frequency shifts and the width of the Raman bands are discussed in term of ions in non-equilibrium positions. FT-IR spectra reveal a sharp peak at 1260 cm−1, and two broad bands around 995 and 772 cm−1. The bandwidths of the latter two bands are believed to be associated with the presence of a high degree of defects in the films. The experimental results of the SBN films are compared with those obtained in SBT (T=Ta) films. X-ray diffraction and SEM techniques are also used for the structural characterization.


2017 ◽  
Vol 727 ◽  
pp. 327-334
Author(s):  
Yan Wang ◽  
Jun Wang ◽  
Xiao Fei Zhang ◽  
Ya Qing Liu

La-Nd co-doped barium hexaferrites, Ba0.7(LamNdn)0.3Fe12O19 (D-BaM), were successfully prepared by sol-gel method. PANI / D-BaM composites were synthesized by in-situ polymerization in solution. The structure, morphology and properties of samples have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), vibrating sample magnetometer (VSM), four-probe conductivity tester and vector network analyzer. The XRD patterns showed that the crystal structure of all the samples exist as M-type phases. The SEM images revealed that the particles presented a hexagonal platelet-like morphology. The magnetic properties could be improved by substitutions of La and Nd ions. The saturation magnetization (Ms) and coercive force (Hc) increased with the change of La / Nd ratio to the maximum at La / Nd = 3:1. The doped particles have also been embedded in conductive PANI to prepare electromagnetic materials, and the conductivity kept on the order of 10-2. The microwave absorbing properties of composites at 30 MHz-6 GHz improved obviously, the peak value of reflection loss could reach-7.5 dB.


2007 ◽  
Vol 130 ◽  
pp. 7-14 ◽  
Author(s):  
Andrew N. Fitch

The highly-collimated, intense X-rays produced by a synchrotron radiation source can be harnessed to build high-resolution powder diffraction instruments with a wide variety of applications. The general advantages of using synchrotron radiation for powder diffraction are discussed and illustrated with reference to the structural characterisation of crystalline materials, atomic PDF analysis, in-situ and high-throughput studies where the structure is evolving between successive scans, and the measurement of residual strain in engineering components.


2019 ◽  
Vol 117 (1) ◽  
pp. 184-189 ◽  
Author(s):  
Yanhao Lin ◽  
Qingyang Hu ◽  
Yue Meng ◽  
Michael Walter ◽  
Ho-Kwang Mao

The distribution and transportation of water in Earth’s interior depends on the stability of water-bearing phases. The transition zone in Earth’s mantle is generally accepted as an important potential water reservoir because its main constituents, wadsleyite and ringwoodite, can incorporate weight percent levels of H2O in their structures at mantle temperatures. The extent to which water can be transported beyond the transition zone deeper into the mantle depends on the water carrying capacity of minerals stable in subducted lithosphere. Stishovite is one of the major mineral components in subducting oceanic crust, yet the capacity of stishovite to incorporate water beyond at lower mantle conditions remains speculative. In this study, we combine in situ laser heating with synchrotron X-ray diffraction to show that the unit cell volume of stishovite synthesized under hydrous conditions is ∼2.3 to 5.0% greater than that of anhydrous stishovite at pressures of ∼27 to 58 GPa and temperatures of 1,240 to 1,835 K. Our results indicate that stishovite, even at temperatures along a mantle geotherm, can potentially incorporate weight percent levels of H2O in its crystal structure and has the potential to be a key phase for transporting and storing water in the lower mantle.


2004 ◽  
Vol 19 (3) ◽  
pp. 827-833 ◽  
Author(s):  
N. Maffei ◽  
G.A. Rossetti

Lead titanate (PbTiO3) is a ferroelectric/piezoelectric material widely used in medical ultrasound transducers and infrared detectors. It is also important as an end member of morphotropic solid-solution systems such as Pb(Zn1/3Nb2/3)–PbTiO3 (PZN–PT) and Pb(Mg1/3Nb2/3)–PT (PMN–PT) that exhibit exceptional electromechanical properties as oriented single crystals. The float-zone technique has been used to grow pure crystals of lead titanate. To the best of the authors’ knowledge, this is the first time that the growth of this compound by the float-zone technique has been reported. The principal advantage of the float-zone technique is that no container is required so that a uniform distribution of chemical constituents can be obtained while eliminating problems of heterogeneous nucleation and metal contamination at the container wall. Although large single crystals were not obtained in the current study primarily due to instabilities of the molten liquid zone, the combined results of characterization by electron probe microanalysis, x-ray diffraction, specific heat, and dielectric permittivity measurements show that the float-zone crystal growth technique can produce lead titanate crystals of high chemical and phase purity. However, the results show that to obtain large single crystals, the stability of the molten zone at low cooling rates must be improved.


1997 ◽  
Vol 12 (4) ◽  
pp. 1131-1140 ◽  
Author(s):  
Kui Yao ◽  
Weiguang Zhu ◽  
Liangying Zhang ◽  
Xi Yao

Several ABO3perovskite ferroelectric crystals, PbTiO3, Pb(Zr, Ti)O3, and BaTiO3have beenin situgrown from amorphous gels with glass elements, and the structural evolution has been systematically investigated using x-ray diffraction (XRD), infrared spectra (IR), differential thermal analysis (DTA), thermogravimetric analysis (TGA), and dielectric measurements. It is found that in the Si-contained glass-ceramic systems, Si and B glass elements are incorporated into the crystalline structures, resulting in the variation of the crystallization process, change of lattice constant, and dielectric properties. Some metastable phases expressed by a general formula AxByGzOw(A = Pb and Ba; B = Zr and Ti; G for glass elements, especially for Si) have been observed and discussed.


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