scholarly journals Direct refinement of the atomic structure of MoS2layered compounds from PXRD

2014 ◽  
Vol 70 (a1) ◽  
pp. C511-C511
Author(s):  
Ivan Bushmarinov ◽  
Alexander Goloveshkin ◽  
Alexandre Golub
Keyword(s):  
Atomic Structure ◽  
Stoichiometric Composition ◽  
Intercalation Compounds ◽  
Layered Compounds ◽  
Organic Layer ◽  
Published Data ◽  
X Ray Diffraction ◽  
Cell Content ◽  
X Ray ◽  
Diffraction Patterns

The graphene analog MoS2can be exfoliated into single-layer dispersion of MoS2crystals by reduction of starting material to LiMoS2followed by detachment of its layers in aqueous solvents. This dispersion reacts with organic salts in solution, producing precipitates of layered MoS2intercalated with their cations [1]. Most of these compounds have distinct chemical composition and powder X-ray diffraction (PXRD) patterns. The analysis of published data, however, indicates that these diffraction patterns were used only for fingerprinting and estimation of cation size and orientation by checking the positions of the basal (00l) reflections. The low-intensity hkl zone of the diffraction patterns was effectively ignored. In the current work, we report that the diffraction patterns of MoS2intercalation compounds contain enough information to refine their atomic structure directly. We found that the patterns of (NR4)x MoS2(R=alkyl, H) compounds correspond to turbostratic disorder of MoS2-organic layers. The patterns were indexed with a common orthorhombic cell. The cell content was Rietveld refined using a modification of a "supercell approach" [2,3] developed for full-pattern modeling of disordered clays. We determined that the Mo atoms in MoS2layers in the intercalation compounds change the coordination from prismatic to octahedral and that the S atoms form "nanorunnels" containing organic cations. The geometry of the Mo-Mo chains forming in the layer was consistent with the EXAFS data. The ordering of the organic layer depended on the nature of the cation, with (NEt4)x MoS2notably ordered enough to have specific stoichiometric composition (x=1/6) defined by the intralayer packing. The PW-DFT-d calculations based on our model confirmed our results. The developed approach allows determination of previously inaccessible atomic structures of a wide class of MoS2-based layered compounds using commercially available software and laboratory X-ray diffraction data.

Exfoliated single molecular layers of Mn0.8PS3 and Cd0.8PS3

2005 ◽  
Vol 20 (5) ◽  
pp. 1107-1112 ◽  
Author(s):  
R.F. Frindt ◽  
D. Yang ◽  
P. Westreich
Keyword(s):  
Ion Exchange ◽  
Structure Factor ◽  
Single Layer ◽  
Layered Compounds ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Vacancy Ordering ◽  
Diffraction Patterns ◽  
Molecular Layers

The layered compounds MnPS3 and CdPS3 were exfoliated to form single molecular layers of Mn0.8PS3 and Cd0.8PS3 in suspension in water by ion exchange. The x-ray diffraction patterns of the two single-layer suspensions showed profound differences in some of the Bragg peaks, and we demonstrated that the differences are not due to the quality or size of the single layers, but are caused by structure factor modulations of the Warren tail for two-dimensional systems. We also demonstrated that the Cd or Mn vacancies generated in the exfoliation process are not ordered at long range, in contrast to an earlier report of vacancy ordering on intercalated MnPS3.

Solvothermal Growth of Flower-Like Morphology from Nanorods of Copper Sulfides

2008 ◽  
Vol 8 (3) ◽  
pp. 1523-1527 ◽  
Author(s):  
Poulomi Roy ◽  
Suneel Kumar Srivastava
Keyword(s):  
Optical Properties ◽  
Reaction Time ◽  
Copper Sulfide ◽  
Solvothermal Synthesis ◽  
Stoichiometric Composition ◽  
X Ray Diffraction ◽  
Reaction Duration ◽  
X Ray ◽  
Copper Sulfides ◽  
Diffraction Patterns

The present work reports the effect of reaction time on solvothermal synthesis of copper sulfides from CuCl2·2H2O and thiourea with various compositions and morphologies using ethylenediamine as solvent at 120 °C. X-ray diffraction patterns of the products at different durations shows the development of different stoichiometric composition of copper sulfides in where Cu:S ratio increases from 1.39 to 1.79 indicating transformation of Cu39S28 to Cu7S4. As inferred by EDX and XPS studies of the final products. SEM shows the growth of bundles of nanorods of length ≈1 μm and diameter in nanometer range are observed after 6 h. On increasing the reaction duration to 9 h, nanorods tends to combines with each other and growth occurs in six directions and after 12 h leads to the formation of flower-like morphology of copper sulfide. The optical properties of these products also have been studied.

scholarly journals THE ICOSAHEDRAL PHASE OF Al63Cu25Fe12 SYSTEM

2019 ◽  
Vol 28 (1) ◽  
pp. 51-56
Author(s):  
Anastazia Melnik ◽  
Luciano Nascimento
Keyword(s):  
Chemical Elements ◽  
Stoichiometric Composition ◽  
Icosahedral Phase ◽  
Quasicrystalline Phase ◽  
Nominal Composition ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ideal Composition ◽  
Diffraction Patterns

The present work aimed to characterize the microstructure of the icosahedral phase (quasicrystalline phase-ϕ) of the system with stoichiometric composition of the quasicrystal Al63Cu25Fe12. The ternary alloy with nominal composition of Al63Cu25Fe12 was processed by mechanical alloying (MA) as a viable solid state processing method for producing various metastable and stable quasicrystalline phases. The structural characterization of the obtained samples was performed by X-ray diffraction (XRD) and Scanning Electron Microscopy (SEM), while the elemental composition of the chemical elements Al, Fe and Cu were determined by X-ray spectroscopy technique of dispersive energy (EDS). According to the results of XRD, the diffraction patterns of Al63Cu25Fe12 showed the presence of β-Al(Fe, Cu) and λ-Al13Fe4 phases coexist with the thermodynamic ϕ-phase quasicrystalline. Finally, elemental analysis indicates that during alloy synthesis there is little variation of the ideal composition. The results indicate that alloys with high percentage of icosahedral phase can be obtained by casting in the air.

X-ray powder diffraction studies of (BaxSr1−x)2Co2Fe12O22 and (BaxSr1−x)Co2Fe16O27

2015 ◽  
Vol 30 (2) ◽  
pp. 139-148 ◽  
Author(s):  
W. Wong-Ng ◽  
G. Liu ◽  
Y. Yan ◽  
K. R. Talley ◽  
J. A. Kaduk
Keyword(s):  
Seebeck Coefficient ◽  
Powder Diffraction ◽  
Lattice Parameters ◽  
Hexagonal Ferrite ◽  
Layered Compounds ◽  
X Ray Diffraction ◽  
Powder Diffraction File ◽  
Space Group ◽  
X Ray ◽  
Diffraction Patterns

X-ray structural characterization and X-ray reference powder patterns have been determined for two series of iron- and cobalt-containing layered compounds (BaxSr1−x)2Co2Fe12O22 (x = 0.2, 0.4, 0.6, 0.8) and (BaxSr1−x)Co2Fe16O27 (x = 0.2, 0.4, 0.6, 0.8). The (BaxSr1−x)2Co2Fe12O22 series of compounds crystallized in the space group R$\bar 3$m (No. 166), with Z = 3. The structure is essentially that of the Y-type hexagonal ferrite, BaM2+Fe63+O11. The lattice parameters range from a = 5.859 15(8) to 5.843 72(8) Å, and c = 43.4975(9) to 43.3516(9) Å for x = 0.2 to 0.8, respectively. The (BaxSr1−x)Co2Fe16O27 series (W-type hexagonal ferrite) crystallized in the space group P63/mmc (No. 194) and Z = 2. The lattice parameters range from a = 5.902 05(12) to 5.8979(2) Å and c = 32.9002(10) to 32.8110(13) Å for x = 0.2 to 0.8. Results of measurements of the Seebeck coefficient and resistivity of these two sets of samples indicated that they are insulators. Powder X-ray diffraction patterns of these two series of compounds have been submitted to be included in the Powder Diffraction File.

Preparation of FeCl3–IBr–H2SO4–graphite multi-intercalation compounds

1994 ◽  
Vol 9 (2) ◽  
pp. 377-382 ◽  
Author(s):  
Takeshi Abe ◽  
Yasuo Mizutani ◽  
Eiji Ihara ◽  
Mitsuru Asano ◽  
Toshio Harada
Keyword(s):  
Saturated Vapor ◽  
Intercalation Compound ◽  
Intercalation Compounds ◽  
Stacking Sequence ◽  
X Ray Diffraction ◽  
Graphite Intercalation Compounds ◽  
X Ray ◽  
Graphite Intercalation ◽  
Diffraction Patterns

Stages 4-6 FeCl3-graphite intercalation compounds (GIC's) have been prepared by an ordinary two-bulb method, and FeCl3-IBr-graphite bi-intercalation compounds (GBC's) are synthesized by holding the FeCl3-GIC's in the saturated vapor of IBr. The x-ray diffraction patterns of the FeCl3-IBr-GBC's obtained from stages 4, 5, and 6 FeCl3-GIC's give the stacking sequences as G(FeCl3)GG(IBr)GG(FeCl3)G, G(FeCl3)GG(IBr)GGG(FeCl3)G, and G(FeCl3)GG(IBr)GG(IBr)GG(FeCl3)G, respectively, where G, (FeCl3), and (IBr) refer to the graphite, FeCl3, and IBr layers, respectively. The multi-intercalation of H2SO4 into the FeCl3-IBr-GBC's synthesized from stages 4 and 6 FeCl3-GIC's occurs at all the vacant galleries of the GBC's at the same time. In contrast, the multi-intercalation of H2SO4 into the FeCl3-IBr-GBC obtained from the stage 5 FeCl3-GIC takes place in two processes. The first multi-intercalation occurs at the gallery adjacent to the bi-intercalated IBr layer, and the stacking sequence of the resulting graphite multi-intercalation compound is determined to be G(FeCl3)GG(IBr)G(H2SO4)GG(FeCl3)G, where (H2SO4) refers to the H2SO4 layer. The second multi-intercalation occurs at all the rest of the vacant galleries.

scholarly journals Characterization in the icosahedral phase of the system Al63Cu25Fe12

2021 ◽  
Vol 24 (3) ◽  
pp. 1-5
Author(s):  
Luciano Nascimento ◽  
Anastasia Melnyk
Keyword(s):  
Chemical Elements ◽  
Stoichiometric Composition ◽  
Icosahedral Phase ◽  
Quasicrystalline Phase ◽  
Nominal Composition ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ideal Composition ◽  
Diffraction Patterns

The present work aimed to characterize the microstructure of the icosahedral phase (ɸ-quasicrystalline phase) of the system with stoichiometric composition of the quasicrystal Al63Cu25Fe12. The ternary alloy with nominal composition of Al63Cu25Fe12 was processed by Mechanical Alloying (MA) as a viable solid state processing method for producing various metastable and stable quasicrystalline phases. The structural characterization of the obtained samples was performed by X-ray diffraction (XRD) and Scanning Electron Microscopy (SEM), while the elemental composition of the chemical elements Al, Fe and Cu were determined by the technique of X-ray spectroscopy by dispersive energy (EDS). According to the results of XRD, the diffraction patterns of Al63Cu25Fe12 showed the presence of β-Al (Fe, Cu) and λ-Al13Fe4 phases coexist with the thermodynamic ɸ-phase quasicrystalline. Finally, elemental analysis indicates that during alloy synthesis there is little variation of the ideal composition. The results indicate that alloys with high percentage of icosahedral phase can be obtained by casting in the air.

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.

TEM studies of solid-state reactions in sputter-deposited Nb/Al multilayer thin films

1996 ◽  
Vol 54 ◽  
pp. 1020-1021
Author(s):  
F. Ma ◽  
S. Vivekanand ◽  
K. Barmak ◽  
C. Michaelsen
Keyword(s):  
Thin Films ◽  
Solid State ◽  
Stoichiometric Composition ◽  
Analytical Electron Microscopy ◽  
Grain Structure ◽  
Solid State Reactions ◽  
Multilayer Thin Films ◽  
X Ray Diffraction ◽  
X Ray ◽  
Sputter Deposited

Solid state reactions in sputter-deposited Nb/Al multilayer thin films have been studied by transmission and analytical electron microscopy (TEM/AEM), differential scanning calorimetry (DSC) and X-ray diffraction (XRD). The Nb/Al multilayer thin films for TEM studies were sputter-deposited on (1102)sapphire substrates. The periodicity of the films is in the range 10-500 nm. The overall composition of the films are 1/3, 2/1, and 3/1 Nb/Al, corresponding to the stoichiometric composition of the three intermetallic phases in this system.Figure 1 is a TEM micrograph of an as-deposited film with periodicity A = dA1 + dNb = 72 nm, where d's are layer thicknesses. The polycrystalline nature of the Al and Nb layers with their columnar grain structure is evident in the figure. Both Nb and Al layers exhibit crystallographic texture, with the electron diffraction pattern for this film showing stronger diffraction spots in the direction normal to the multilayer. The X-ray diffraction patterns of all films are dominated by the Al(l 11) and Nb(l 10) peaks and show a merging of these two peaks with decreasing periodicity.

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.

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