An efficient fulleride production system

1995 ◽  
Vol 73 (1-2) ◽  
pp. 38-44 ◽  
Author(s):  
W. R. Datars ◽  
S. Galts ◽  
T. Olech ◽  
P. K. Ummat
Keyword(s):  
Complete System ◽  
Continuous Production ◽  
Arc Furnace ◽  
X Ray Diffraction ◽  
High Quality ◽  
X Ray ◽  
Typical Data ◽  
Carbon Soot ◽  
Carbon Rods ◽  
Raman And Infrared Spectroscopy

A complete system for the production of the fullerides C60 and C70 is described. Emphasis is placed on efficient, continuous production of high-quality materials. Carbon soot with a content of 2–5% of a mixture of C60 and C70 is prepared from carbon rods with an arc furnace. The mixture is separated from the carbon by using a Soxhlet extractor. The C60 and C70 are separated with a chromotography column in which the solvent is cycled continuously. The separated C60 is purified by sublimation. The C70 is separated from heavier fullerides with a second chromotography procedure. Single crystals of C60 are prepared from pure C60 powder by slow sublimation. The C60 is characterized by mass spectroscopy, X-ray diffraction, and Raman and infrared spectroscopy. Typical data obtained with these techniques are shown.

X-ray powder diffraction pattern and crystal structure of AlCu4Y ternary compound

2015 ◽  
Vol 30 (4) ◽  
pp. 362-364
Author(s):  
Degui Li ◽  
Ming Qin ◽  
Liuqing Liang ◽  
Changsheng Qin ◽  
Chenzhong Jia ◽  
...  
Keyword(s):  
Diffraction Pattern ◽  
Ternary Compound ◽  
Powder Diffraction ◽  
Hexagonal Structure ◽  
Argon Atmosphere ◽  
Arc Furnace ◽  
Powder Diffraction Data ◽  
X Ray Diffraction ◽  
High Quality ◽  
X Ray

The ternary compound of AlCu4Y was synthesized by melting under argon atmosphere in the arc furnace. High-quality X-ray powder diffraction data of AlCu4Y have been collected using a Rigaku SmartLab X-ray powder diffractometer. The Rietveld refinement results of the X-ray diffraction pattern for the AlCu4Y compound showed that the AlCu4Y is the hexagonal structure, space-group P6/mmm (No. 191) with a = 5.0658(1) Å, c = 4.1569(1) Å, V = 92.38 Å3, Z = 1, and the density is 6.66 g cm−3, and the intensity ratio RIR is 1.96.

Technology of high quality protein crystals’ obtaining aboard the ISS at execution of joint Japanese–Russian experiments

2020 ◽  
pp. 5-25
Author(s):  
Koji INAKA ◽  
Saori ICHIMIZU ◽  
Izumi YOSHIZAKI ◽  
Kiyohito KIHIRA ◽  
Elena G. LAVRENKO ◽  
...  
Keyword(s):  
Drug Design ◽  
International Space Station ◽  
Space Station ◽  
Protein Crystals ◽  
Diffusion Method ◽  
X Ray Diffraction ◽  
High Quality ◽  
International Space ◽  
X Ray ◽  
High Quality Protein

A series of space experiments aboard the International Space Station (ISS) associated with high-quality Protein Crystal Growth (PCG) in microgravity conditions can be considered as a unique and one of the best examples of fruitful collaboration between Japanese and Russian scientists and engineers in space, which includes also other ISS International Partners. X-ray diffraction is still the most powerful tool to determine the protein three dimensional structure necessary for Structure based drug design (SBDD). The major purpose of the experiment is to grow high quality protein crystals in microgravity for X-ray diffraction on Earth. Within one and a half decade, Japan and Russia have established an efficient process over PCG in space to support latest developments over drug design and structural biology. One of the keys for success of the experiment lies in how precisely pre-launch preparations are made. Japanese party provides flight equipment for crystallization and ensures the required environment to support the experiment aboard of the ISS’s Kibo module, and also mainly takes part of the experiment ground support such as protein sample characterization, purification, crystallization screening, and solution optimization for microgravity experiment. Russian party is responsible for integration of the flight items equipped with proteins and precipitants on board Russian transportation space vehicles (Soyuz or Progress), for delivery them at the ISS, transfer to Kibo module, and returning the experiments’ results back on Earth aboard Soyuz manned capsule. Due to close cooperation of the parties and solid organizational structure, samples can be launched at the ISS every half a year if the ground preparation goes smoothly. The samples are crystallized using counter diffusion method at 20 degree C for 1–2.5 months. After samples return, the crystals are carefully taken out from the capillary, and frozen for X-ray diffraction at SPring8 facility in Japan. Extensive support of researchers from both countries is also a part of this process. The paper analyses details of the PCG experiment scheme, unique and reliable technology of its execution, and contains examples of the application. Key words: International Space Station, Protein crystals, Microgravity, International collaboration.

scholarly journals Crystallographic features of ammonium fluoroelpasolites: dynamic orientational disorder in crystals of (NH4)3HfF7 and (NH4)3Ti(O2)F5

2017 ◽  
Vol 73 (1) ◽  
pp. 1-9 ◽  
Author(s):  
Anatoly A. Udovenko ◽  
Alexander A. Karabtsov ◽  
Natalia M. Laptash
Keyword(s):  
Single Crystal ◽  
Electron Density ◽  
Diffraction Data ◽  
Central Atom ◽  
X Ray Diffraction ◽  
Dynamic Nature ◽  
Orientational Disorder ◽  
High Quality ◽  
Structural Units ◽  
X Ray

A classical elpasolite-type structure is considered with respect to dynamically disordered ammonium fluoro-(oxofluoro-)metallates. Single-crystal X-ray diffraction data from high quality (NH4)3HfF7 and (NH4)3Ti(O2)F5 samples enabled the refinement of the ligand and cationic positions in the cubic Fm \bar 3 m (Z = 4) structure. Electron-density atomic profiles show that the ligand atoms are distributed in a mixed (split) position instead of 24e. One of the ammonium groups is disordered near 8c so that its central atom (N1) forms a tetrahedron with vertexes in 32f. However, a center of another group (N2) remains in the 4b site, whereas its H atoms (H2) occupy the 96k positions instead of 24e and, together with the H3 atom in the 32f position, they form eight spatial orientations of the ammonium group. It is a common feature of all ammonium fluoroelpasolites with orientational disorder of structural units of a dynamic nature.

scholarly journals Redetermination of Sr2PdO3 from single-crystal X-ray data

2019 ◽  
Vol 75 (1) ◽  
pp. 30-32
Author(s):  
Gohil S. Thakur ◽  
Hans Reuter ◽  
Claudia Felser ◽  
Martin Jansen
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Diffraction Data ◽  
Structure Refinement ◽  
Structure Type ◽  
X Ray Diffraction ◽  
High Quality ◽  
X Ray ◽  
Cell Parameters ◽  
Anisotropic Displacement Parameters

The crystal structure redetermination of Sr2PdO3 (distrontium palladium trioxide) was carried out using high-quality single-crystal X-ray data. The Sr2PdO3 structure has been described previously in at least three reports [Wasel-Nielen & Hoppe (1970). Z. Anorg. Allg. Chem. 375, 209–213; Muller & Roy (1971). Adv. Chem. Ser. 98, 28–38; Nagata et al. (2002). J. Alloys Compd. 346, 50–56], all based on powder X-ray diffraction data. The current structure refinement of Sr2PdO3, as compared to previous powder data refinements, leads to more precise cell parameters and fractional coordinates, together with anisotropic displacement parameters for all sites. The compound is confirmed to have the orthorhombic Sr2CuO3 structure type (space group Immm) as reported previously. The structure consists of infinite chains of corner-sharing PdO4 plaquettes interspersed by SrII atoms. A brief comparison of Sr2PdO3 with the related K2NiF4 structure type is given.

scholarly journals Cubic InGaN Grown by MOCVD

1999 ◽  
Vol 4 (S1) ◽  
pp. 239-243
Author(s):  
J.B. Li ◽  
Hui Yang ◽  
L.X. Zheng ◽  
D.P. Xu ◽  
Y.T. Wang
Keyword(s):  
Room Temperature ◽  
Emission Peak ◽  
Buffer Layers ◽  
Cubic Phase ◽  
Yellow Luminescence ◽  
X Ray Diffraction ◽  
High Quality ◽  
X Ray ◽  
Cubic Gan ◽  
Pl Emission

We report on the growth of high-quality cubic phase InGaN on GaAs by MOCVD. The cubic InGaN layers are grown on cubic GaN buffer layers on GaAs (001) substrates. The surface morphology of the films are mirror-like. The cubic nature of the InGaN films is obtained by X-ray diffraction (XRD) measurements. The InGaN layers show strong photoluminescence (PL) at room temperature. Neither emission peak from wurtzite GaN nor yellow luminescence is observed in our films. The highest In content as determined by XRD is about 17% with an PL emission wavelength of 450 nm. The FWHM of the cubic InGaN PL peak are 153 meV and 216 meV for 427 nm and 450 nm emissions, respectively. It is found that the In compositions determined from XRD are not in agreement with those estimated from PL measurements. The reasons for this disagreement are discussed.

Synthèse et caractérisation des oxypentafluorouranates(VI) NH4UOF5, KUOF5, RbUOF5 et CsUOF5

1978 ◽  
Vol 56 (14) ◽  
pp. 1874-1880 ◽  
Author(s):  
Philippe Joubert ◽  
Roland Bougon ◽  
Bernard Gaudreau
Keyword(s):  
Infrared Spectroscopy ◽  
Solid State ◽  
Alkali Metal ◽  
Vibrational Spectroscopy ◽  
Uranium Atom ◽  
The Other ◽  
Metal Fluoride ◽  
X Ray Diffraction ◽  
X Ray ◽  
Raman And Infrared Spectroscopy

The oxypentafluorouranates(VI) MUOF5, where M = NH4, K, Rb, Cs, have been synthetized from reaction of UOF4 with the ammonium or corresponding alkali metal fluoride in liquid SO2. According to X-ray diffraction, Raman and infrared spectroscopy, and from an isomorphism with the corresponding hexafluorouranates(V) MUF6, two different environments around the uranium atom are observed. In CsUOF5 the five fluorine atoms and the oxygen around the uranium result in a pseudo-octahedral surrounding whereas for the other complexes (M = NH4, K, Rb) each uranium is surrounded by eight light atoms forming a dodecahedron. In this structure the dodecahedra are linked together by fluorine atoms to form infinite chains. The UOF5− ion has been characterized by vibrational spectroscopy in the solid state. The proposed assignment, which was made with the assumption of a C4v symmetry of the UOF5− ion, was confirmed by a force constant calculation. From these data and contrary to the values reported for comparable oxypentafluoroanions, the axial fluorine is found to be less ionic than the equatorial ones.

The X-Ray Powder Diffraction Patterns and Crystal Structure for Al2M3Y(M=Cu, Ni)

2014 ◽  
Vol 950 ◽  
pp. 48-52
Author(s):  
De Gui Li ◽  
Ming Qin ◽  
Liu Qing Liang ◽  
Zhao Lu ◽  
Shu Hui Liu ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Hexagonal Structure ◽  
Argon Atmosphere ◽  
X Ray Diffraction ◽  
High Quality ◽  
X Ray ◽  
Arc Melting ◽  
Diffraction Patterns

The Al2M3Y(M=Cu, Ni) compound was synthesized by arc melting under argon atmosphere. The high-quality powder X-ray diffraction data of Al2M3Y have been presented. The refinement of the X-ray diffraction patterns for the Al2M3Y compound show that the Al2M3Y has hexagonal structure, space groupP6/mmm(No.191), with a = b = 5.1618(2) Å, c = 4.1434(1) Å,V= 95.6 Å3,Z= 1,ڑx= 5.7922 g/cm3,F30= 155.5(0.0057, 34), RIR = 2.31 for Al2Cu3Y, and with a = b = 5.0399(1) Å, c = 4.0726(1) Å,V= 89.59 Å3,Z= 1,ڑx= 5.9118 g/cm3,F30= 135.7(0.0072, 30), RIR = 2.54 for Al2Ni3Y.

Epitaxial Growth of Aluminum Nitride on Sapphire and Silicon

1994 ◽  
Vol 358 ◽  
Author(s):  
K. Dovidenko ◽  
S. Oktyabrsky ◽  
J. Narayan ◽  
M. Razeghi
Keyword(s):  
Epitaxial Growth ◽  
Substrate Surface ◽  
Wide Band ◽  
X Ray Diffraction ◽  
Wide Band Gap ◽  
High Quality ◽  
Microstructural Characteristics ◽  
X Ray ◽  
Si Substrates ◽  
Transmission Electron

ABSTRACTThe microstructural characteristics of wide band gap semiconductor, hexagonal A1N thin films on Si(100), (111), and sapphire (0001) and (10ī2) were studied by transmission electron microscopy (TEM) and x-ray diffraction. The films were grown by MOCVD from TMA1 + NH3 + N2 gas mixtures. Different degrees of film crystallinity were observed for films grown on α-A12O3 and Si substrates in different orientations. The epitaxial growth of high quality single crystalline A1N film on (0001) α-Al2O3 was demonstrated with a dislocation density of about 2*10 10cm−2 . The films on Si(111) and Si(100) substrates were textured with the c-axis of A1N being perpendicular to the substrate surface.

On the problem of overlapping ω scans measured on thin films deposited on monocrystal substrates

1999 ◽  
Vol 32 (4) ◽  
pp. 736-743 ◽  
Author(s):  
D. Machajdík ◽  
A. Pevala ◽  
A. Rosová ◽  
K. Fröhlich ◽  
J. Šouc ◽  
...  
Keyword(s):  
Thin Film ◽  
Thin Films ◽  
Spectral Characteristics ◽  
Full Width ◽  
X Ray Diffraction ◽  
Resolution Function ◽  
High Quality ◽  
Experimental Procedure ◽  
X Ray ◽  
Crystallographic Planes

CeO2thin films deposited on sapphire monocrystal substrates were used for an experimental study of the nature of extremely narrow overlapped maxima on X-ray diffraction ω scans. Full width at half-maximum (FWHM) values of such maxima typically reached the resolution function of the diffractometer. A comparative study of the influence of various diffractometer set-ups on the spectral characteristics of the X-ray beam in relation to the above-mentioned phenomenon was carried out. A surrounding (λmin− λmax) or (2θmin− 2θmax) of the strong substrate reflection was obtained, where a substrate contribution to an ω scan measured on thin-film reflection can be expected. Two possible origins of the narrow maxima are discussed: (a) a contribution of a part of the X-ray beam having λ ≠ λKαthat diffracts on a set of substrate crystallographic planes parallel to the thin-film crystallographic planes used for the ω-scan measurement; and (b) the presence in part of the thin film of a perfect monocrystal-like quality with practically no mosaicity. The principles of this approach and experimental procedure are reported, and on this basis it is possible to distinguish between the two possible origins of the narrow overlapped maxima. It is shown that under appropriate conditions, an extremely high quality CeO2thin film can be grown. The FWHM value of its ω scan can reach the value of diffractometer instrumental broadening obtained for a perfect monocrystal.

scholarly journals Preparation of BaZrO3 powders by a spray-drying process

2003 ◽  
Vol 18 (6) ◽  
pp. 1325-1332 ◽  
Author(s):  
B. Robertz ◽  
F. Boschini ◽  
A. Rulmont ◽  
R. Cloots ◽  
I. Vandriessche ◽  
...  
Keyword(s):  
Spray Drying ◽  
Precursor Solution ◽  
Barium Zirconate ◽  
Drying Process ◽  
X Ray Diffraction ◽  
High Quality ◽  
Corrosion Resistant ◽  
X Ray ◽  
Potential Use ◽  
Scanning Electron

The potential use of barium zirconate for the manufacture of corrosion-resistant substrates emphasizes the need for a simple, inexpensive, and easily scalable process to produce high-quality powders with well-controlled composition and properties. However, the classical solid-state preparation of barium zirconate leads to an inhomogeneous powder unsuitable for applications in highly corrosive environment. For this paper, the possibility to use the spray-drying technique for the preparation of BaZrO3 powders with a controlled size distribution and morphology was investigated. The influence of the nature and concentration of the precursor solution and the influence of the spray-drying step are discussed on the basis of x-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, and dilatometric measurements.

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