PbI2 Confined In The Spaces Of LTA Zeolites

1991 ◽  
Vol 233 ◽  
Author(s):  
O. Terasaki ◽  
Z. K. Tang ◽  
Y. Nozue ◽  
T. Goto

ABSTRACTPbI2 clusters confined in spaces of LTA zeolite are successfully prepared through vapour phase. An HREM image showed that the crystallinity of the zeolite was preserved after preparation and showed directly that the clusters were incorporated into the α-cages. Absorption spectra were measured by diffuse reflection method as a function of loading density of PbI2 molecules. Several absorption bands from different cluster sizes were observed and showed remarkable blue shift. At the maximum loading, extra reflections, which are forbidden for Fm3A of LTA, were observed in electron and X-ray diffraction patterns. The appearence of the extra reflections and the dependence of absorption curve on the loading density suggest that superlattice of clusters was produced. The characteristic feature of zeolites as containers to make an artificial superlattice of clusters is pointed out.

2019 ◽  
Vol 11 (5) ◽  
pp. 678-682
Author(s):  
Ce Liang ◽  
Nian Tao ◽  
Bowen Wang ◽  
Wenjun Liu ◽  
Ke Bi ◽  
...  

In this work, we introduced a facile approach for preparing cadmium gallate (CdGa2 O4 nanoparticles, and we first studied the photocatalytic properties of this ternary spinel oxide. Through a solvothermal process for the formation of precursor and the subsequent calcination process for recrystallization, CdGa2 O4 nanoparticles with diameter of ca. 12 nm were synthesized. They were characterized by using X-ray diffraction patterns and electron microscopy images. UV-visible diffuse absorption spectroscopy was also conducted; its spectra indicate that CdGa2 O4 nanoparticles have strong but small blue-shift absorption relative to that of the bulk samples. Moreover, the CdGa2 O4 nanoparticles could photocatalytically decompose rhodamine B (RhB) molecules with high efficiency in aqueous solution under ultraviolet irradiation. Notably, this novel photocatalyst exhibited outstanding recycling stability, and it retained almost the same capacity in the fourth photocatalytic cycle. We deduce that the high photocatalytic performance results from the large specific surface area, energetic photoinduced carriers, and inherent stability.


2017 ◽  
Vol 50 (6) ◽  
pp. 1716-1724 ◽  
Author(s):  
Mohd. Shkir ◽  
V. Ganesh ◽  
S. AlFaify ◽  
K. K. Maurya ◽  
N. Vijayan

In this work, the growth of large size (∼25 × 29 × 5 mm and ∼25 × 24 × 6 mm) colorful single crystals of zinc (tris) thiourea sulfate (ZTS) in the presence of 0.05–2 wt% phenol red (PR) dye was achieved using a simple and low-cost technique. Powder X-ray diffraction patterns confirm the presence of PR dye, which is indicated by an enhancement of the Raman peak intensities, a shift in their position and the appearance of a few extra peaks. The quality of the grown crystals was assessed by high-resolution X-ray diffraction, which shows that the crystalline perfection of 1 wt% PR-dyed ZTS crystals is better than that of 2 wt% PR-dyed crystals. The measured UV–vis absorbance spectra show two additional, strong absorption bands at ∼430 and 558 nm in the dyed crystals, due to the presence of PR dye, along with a band at ∼276 nm which is present for all crystals but is slightly shifted for the dyed crystals. Photoluminescence spectra were recorded at two excitation wavelengths (λexc= 310 and 385 nm). The luminescence intensity is found to be enriched in dyed crystals, with some extra emission bands. An enhancement in the value of the dielectric constant and a.c. electrical conductivity was also observed in the dyed ZTS crystals.


RSC Advances ◽  
2014 ◽  
Vol 4 (96) ◽  
pp. 53419-53428 ◽  
Author(s):  
N. Pethan Rajan ◽  
Ginjupalli Srinivasa Rao ◽  
Balla Putrakumar ◽  
Komandur V. R. Chary

X-ray diffraction patterns of pure and spent VPO samples.


Author(s):  
T. Gulik-Krzywicki ◽  
M.J. Costello

Freeze-etching electron microscopy is currently one of the best methods for studying molecular organization of biological materials. Its application, however, is still limited by our imprecise knowledge about the perturbations of the original organization which may occur during quenching and fracturing of the samples and during the replication of fractured surfaces. Although it is well known that the preservation of the molecular organization of biological materials is critically dependent on the rate of freezing of the samples, little information is presently available concerning the nature and the extent of freezing-rate dependent perturbations of the original organizations. In order to obtain this information, we have developed a method based on the comparison of x-ray diffraction patterns of samples before and after freezing, prior to fracturing and replication.Our experimental set-up is shown in Fig. 1. The sample to be quenched is placed on its holder which is then mounted on a small metal holder (O) fixed on a glass capillary (p), whose position is controlled by a micromanipulator.


Author(s):  
J. P. Robinson ◽  
P. G. Lenhert

Crystallographic studies of rabbit Fc using X-ray diffraction patterns were recently reported. The unit cell constants were reported to be a = 69. 2 A°, b = 73. 1 A°, c = 60. 6 A°, B = 104° 30', space group P21, monoclinic, volume of asymmetric unit V = 148, 000 A°3. The molecular weight of the fragment was determined to be 55, 000 ± 2000 which is in agreement with earlier determinations by other methods.Fc crystals were formed in water or dilute phosphate buffer at neutral pH. The resulting crystal was a flat plate as previously described. Preparations of small crystals were negatively stained by mixing the suspension with equal volumes of 2% silicotungstate at neutral pH. A drop of the mixture was placed on a carbon coated grid and allowed to stand for a few minutes. The excess liquid was removed and the grid was immediately put in the microscope.


2020 ◽  
Vol 86 (6) ◽  
pp. 29-35
Author(s):  
V. P. Sirotinkin ◽  
O. V. Baranov ◽  
A. Yu. Fedotov ◽  
S. M. Barinov

The results of studying the phase composition of advanced calcium phosphates Ca10(PO4)6(OH)2, β-Ca3(PO4)2, α-Ca3(PO4)2, CaHPO4 · 2H2O, Ca8(HPO4)2(PO4)4 · 5H2O using an x-ray diffractometer with a curved position-sensitive detector are presented. Optimal experimental conditions (angular positions of the x-ray tube and detector, size of the slits, exposure time) were determined with allowance for possible formation of the impurity phases during synthesis. The construction features of diffractometers with a position-sensitive detector affecting the profile characteristics of x-ray diffraction peaks are considered. The composition for calibration of the diffractometer (a mixture of sodium acetate and yttrium oxide) was determined. Theoretical x-ray diffraction patterns for corresponding calcium phosphates are constructed on the basis of the literature data. These x-ray diffraction patterns were used to determine the phase composition of the advanced calcium phosphates. The features of advanced calcium phosphates, which should be taken into account during the phase analysis, are indicated. The powder of high-temperature form of tricalcium phosphate strongly adsorbs water from the environment. A strong texture is observed on the x-ray diffraction spectra of dicalcium phosphate dihydrate. A rather specific x-ray diffraction pattern of octacalcium phosphate pentahydrate revealed the only one strong peak at small angles. In all cases, significant deviations are observed for the recorded angular positions and relative intensity of the diffraction peaks. The results of the study of experimentally obtained mixtures of calcium phosphate are presented. It is shown that the graphic comparison of experimental x-ray diffraction spectra and pre-recorded spectra of the reference calcium phosphates and possible impurity phases is the most effective method. In this case, there is no need for calibration. When using this method, the total time for analysis of one sample is no more than 10 min.


1985 ◽  
Vol 50 (10) ◽  
pp. 2139-2145
Author(s):  
Alexander Muck ◽  
Eva Šantavá ◽  
Bohumil Hájek

The infrared spectra and powder X-ray diffraction patterns of polycrystalline YPO4-YCrO4 samples are studied from the point of view of their crystal symmetry. Mixed crystals of the D4h19 symmetry are formed over the region of 0-30 mol.% YPO4 in YCrO4. The Td → D2d → D2 or C2v(GS eff) correlation is appropriate for both PO43- and CrO43- anions.


Catalysts ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 899
Author(s):  
Murendeni P. Ravele ◽  
Opeyemi A. Oyewo ◽  
Damian C. Onwudiwe

Pure-phase Cu2−xS (x = 1, 0.2) nanoparticles have been synthesized by the thermal decomposition of copper(II) dithiocarbamate as a single-source precursor in oleylamine as a capping agent. The compositions of the Cu2−xS nanocrystals varied from CuS (covellite) through the mixture of phases (CuS and Cu7.2S4) to Cu9S5 (digenite) by simply varying the temperature of synthesis. The crystallinity and morphology of the copper sulfides were studied using X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM), which showed pure phases at low (120 °C) and high (220 °C) temperatures and a mixture of phases at intermediate temperatures (150 and 180 °C). Covellite was of a spherical morphology, while digenite was rod shaped. The optical properties of these nanocrystals were characterized by UV−vis–NIR and photoluminescence spectroscopies. Both samples had very similar absorption spectra but distinguishable fluorescence properties and exhibited a blue shift in their band gap energies compared to bulk Cu2−xS. The pure phases were used as catalysts for the photocatalytic degradation of tetracycline (TC) under visible-light irradiation. The results demonstrated that the photocatalytic activity of the digenite phase exhibited higher catalytic degradation of 98.5% compared to the covellite phase, which showed 88% degradation within the 120 min reaction time using 80 mg of the catalysts. The higher degradation efficiency achieved with the digenite phase was attributed to its higher absorption of the visible light compared to covellite.


2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Lars Banko ◽  
Phillip M. Maffettone ◽  
Dennis Naujoks ◽  
Daniel Olds ◽  
Alfred Ludwig

AbstractWe apply variational autoencoders (VAE) to X-ray diffraction (XRD) data analysis on both simulated and experimental thin-film data. We show that crystal structure representations learned by a VAE reveal latent information, such as the structural similarity of textured diffraction patterns. While other artificial intelligence (AI) agents are effective at classifying XRD data into known phases, a similarly conditioned VAE is uniquely effective at knowing what it doesn’t know: it can rapidly identify data outside the distribution it was trained on, such as novel phases and mixtures. These capabilities demonstrate that a VAE is a valuable AI agent for aiding materials discovery and understanding XRD measurements both ‘on-the-fly’ and during post hoc analysis.


Crystals ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 312
Author(s):  
Florian Lauraux ◽  
Stéphane Labat ◽  
Sarah Yehya ◽  
Marie-Ingrid Richard ◽  
Steven J. Leake ◽  
...  

The simultaneous measurement of two Bragg reflections by Bragg coherent X-ray diffraction is demonstrated on a twinned Au crystal, which was prepared by the solid-state dewetting of a 30 nm thin gold film on a sapphire substrate. The crystal was oriented on a goniometer so that two lattice planes fulfill the Bragg condition at the same time. The Au 111 and Au 200 Bragg peaks were measured simultaneously by scanning the energy of the incident X-ray beam and recording the diffraction patterns with two two-dimensional detectors. While the former Bragg reflection is not sensitive to the twin boundary, which is oriented parallel to the crystal–substrate interface, the latter reflection is only sensitive to one part of the crystal. The volume ratio between the two parts of the twinned crystal is about 1:9, which is also confirmed by Laue microdiffraction of the same crystal. The parallel measurement of multiple Bragg reflections is essential for future in situ and operando studies, which are so far limited to either a single Bragg reflection or several in series, to facilitate the precise monitoring of both the strain field and defects during the application of external stimuli.


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