scholarly journals THE SYNTHESIS AND PROPERTIES OF THE ANHYDROUS HEXACHLOROZIRCONATES OF SODIUM AND POTASSIUM

1964 ◽  
Vol 42 (5) ◽  
pp. 1102-1105 ◽  
Author(s):  
R. L. Lister ◽  
S. N. Flengas
Keyword(s):  
Alkali Metal ◽  
Closed System ◽  
Metal Chloride ◽  
X Ray Diffraction ◽  
Zirconium Tetrachloride ◽  
Melting Points ◽  
Alkali Metal Chloride ◽  
X Ray ◽  
Diffraction Patterns ◽  
Sodium And Potassium

The hexachlorozirconates of sodium and potassium have been produced in a closed system following the reaction:[Formula: see text]where M is Na and K, respectively. The zirconium tetrachloride was reacted at approximately 1 atm. pressure, and at temperatures of the alkali metal chloride between 425 °C and 525 °C. The densities, melting points, and the corresponding X-ray diffraction patterns for both compounds have been determined.

The synthesis and properties of the hexachloroniobates and hexachlorotantalates of Na, K, Rb, and Cs

1978 ◽  
Vol 56 (15) ◽  
pp. 2013-2018 ◽  
Author(s):  
Donald R. Sadoway ◽  
S. N. Flengas
Keyword(s):  
Alkali Metal ◽  
Phase Transformations ◽  
Powder Diffraction ◽  
Closed System ◽  
Metal Chloride ◽  
Alkali Metal Chloride ◽  
X Ray ◽  
Diffraction Patterns

The compounds NaNbCl6, NaTaCl6, KNbCl6, KTaCl6, RbNbCl6, RbTaCl6, CsNbCl6, and CsTaCl6, were synthesized in a closed system by the reaction of NbCl5 or TaCl5 vapour with solid alkali-metal chloride as follows[Formula: see text]where M is Nb or Ta, and A is Na, K, Rb, or Cs. The X-ray powder diffraction patterns of these compounds were obtained. Temperatures of various phase transformations were determined cryoscopically.

scholarly journals An Experimental Study on High Temperature Corrosion of TP347H Stainless Steel in Molten Chloride and Sulfate

2021 ◽  
Vol 2101 (1) ◽  
pp. 012064
Author(s):  
Weixin Yu ◽  
Xi Chu ◽  
Huihui Zhang ◽  
Yue Shen ◽  
Kangning Tao ◽  
...  
Keyword(s):  
Stainless Steel ◽  
Corrosion Resistance ◽  
Alkali Metal ◽  
Energy Dispersive Spectrometer ◽  
Decisive Role ◽  
Metal Chloride ◽  
Corrosion Mechanism ◽  
X Ray Diffraction ◽  
Alkali Metal Chloride ◽  
Molten Chloride

Abstract The corrosion resistance of TP347H stainless steel was evaluated by measuring mass loss in molten salt at 500-650°C. The corrosion mechanism was characterized by scanning electron microscope (SEM), energy dispersive spectrometer (EDS) and X-ray diffraction (XRD). The results show that the corrosion resistance of TP347H stainless steel increases with the increase of corrosion temperature. When the temperature is below 600°C, TP347H mainly generate low-stable FexOy, and the oxides such as Fe2O3, Fe3O4, Ni1.43Fe1.7O4 and NiFe2O4 are dissolved with the increase of temperature. NbO with higher stability is formed on the surface at 650 °C, which help Cr2O3 and NiO retain for a longer time. Mn-containing compounds on the surface further improve corrosion resistance of TP347H. The corrosion of TP347H stainless steel is mainly intergranular corrosion, and the temperature range of corrosion is consistent with the melting range of alkali metal chloride. Therefore, the molten alkali metal chloride plays a decisive role in the corrosion of TP347H stainless steel.

scholarly journals Sodium and Potassium tert-Butyl Peroxide Hydrates: Crystal Structure and Properties

2021 ◽  
Vol 47 (10) ◽  
pp. 670-678
Author(s):  
A. G. Medvedev ◽  
M. Yu. Sharipov ◽  
A. A. Mikhaylov ◽  
D. A. Grishanov ◽  
A. V. Churakov ◽  
...  
Keyword(s):  
Alkali Metal ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Metal Atoms ◽  
Butyl Peroxide ◽  
Crystal Packings ◽  
Sodium And Potassium ◽  
C Nmr

Abstract Sodium and potassium tert-butyl peroxide hydrates 2Na+·2C4H9$${\text{O}}_{2}^{ - }$$·7H2O (I) and 2K+· 2C4H9$${\text{O}}_{2}^{ - }$$·4H2O (II) were prepared. According to X-ray diffraction data (CIF files CCDC no. 2081025 (I) and no. 2081024 (II)), the compounds are coordination polymers in which alkali metal atoms have C.N.(Na) of 6 or C.N.(K) of 6 and 8. The crystal packings comprise layers with clearly defined hydrophobic surfaces consisting of hydrocarbon groups and hydrophilic inner areas including water molecules, alkali metal cations, and peroxy groups of the tert-butyl peroxide anions. Compounds were characterized by vibrational spectroscopy, 1H, 13C NMR spectroscopy, thermogravimetry, and differential scanning calorimetry.

Evaluation of Freezing Methods by Low Temperature X-Ray Diffraction

1977 ◽  
Vol 35 ◽  
pp. 330-333
Author(s):  
T. Gulik-Krzywicki ◽  
M.J. Costello
Keyword(s):  
Biological Materials ◽  
Molecular Organization ◽  
X Ray Diffraction ◽  
Glass Capillary ◽  
X Ray ◽  
Rate Dependent ◽  
Before And After ◽  
Freeze Etching ◽  
Diffraction Patterns ◽  
Set Up

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.

Examination of Rabbit Fc Crystals

1968 ◽  
Vol 26 ◽  
pp. 140-141
Author(s):  
J. P. Robinson ◽  
P. G. Lenhert
Keyword(s):  
Molecular Weight ◽  
Flat Plate ◽  
Phosphate Buffer ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
X Ray ◽  
Neutral Ph ◽  
Small Crystals ◽  
Carbon Coated ◽  
Diffraction Patterns

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.

Control of the phase composition of advanced calcium phosphates using an x-ray diffractometer with a curved position-sensitive detector

2020 ◽  
Vol 86 (6) ◽  
pp. 29-35
Author(s):  
V. P. Sirotinkin ◽  
O. V. Baranov ◽  
A. Yu. Fedotov ◽  
S. M. Barinov
Keyword(s):  
Phase Composition ◽  
Calcium Phosphates ◽  
Position Sensitive Detector ◽  
Sensitive Detector ◽  
X Ray Diffraction ◽  
X Ray ◽  
Impurity Phases ◽  
Position Sensitive ◽  
Diffraction Peaks ◽  
Diffraction Patterns

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.

Infrared spectroscopic study of the YPO4-YCrO4 system

1985 ◽  
Vol 50 (10) ◽  
pp. 2139-2145
Author(s):  
Alexander Muck ◽  
Eva Šantavá ◽  
Bohumil Hájek
Keyword(s):  
Spectroscopic Study ◽  
Infrared Spectra ◽  
Point Of View ◽  
Mixed Crystals ◽  
Crystal Symmetry ◽  
Infrared Spectroscopic Study ◽  
X Ray Diffraction ◽  
X Ray ◽  
Infrared Spectroscopic ◽  
Diffraction Patterns

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.

scholarly journals Deep learning for visualization and novelty detection in large X-ray diffraction datasets

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Lars Banko ◽  
Phillip M. Maffettone ◽  
Dennis Naujoks ◽  
Daniel Olds ◽  
Alfred Ludwig
Keyword(s):  
Thin Film ◽  
Crystal Structure ◽  
Artificial Intelligence ◽  
Deep Learning ◽  
Novelty Detection ◽  
Structural Similarity ◽  
X Ray Diffraction ◽  
X Ray ◽  
Diffraction Patterns ◽  
Post Hoc

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.

Sign in / Sign up

Export Citation Format

Share Document