The Growth and the Reaction Mechanism of Si3N4 Powder from Silica

2007 ◽  
Vol 554 ◽  
pp. 157-162 ◽  
Author(s):  
Ahmet Atasoy
Keyword(s):  
Gas Phase ◽  
Carbothermal Reduction ◽  
Nitrogen Flow ◽  
X Ray Diffraction ◽  
One Dimensional ◽  
X Ray ◽  
The Third ◽  
Third Stage ◽  
Electron Microscope Analysis ◽  
Experimental Runs

The behaviour of silica during the carbothermal reduction nitriding process at temperatures between 1300-1500°C was studied by means of X-ray diffraction and scanning electron microscope analysis. The experimental runs were allowed to proceed up to 1 h in presence of nitrogen flow. The following mechanism of reduction nitriding of silica which was based on the experimental observation was proposed. Initially the impurity of the starting material is reduced before 1300°C. SiO2 was reduced into SiO gas phase by active carbon and it was vaporised out of the mixture. The nucleation of α-Si3N4 was formed vapour-gas reaction took place and deposited on the surface of the mixture as well as around the reaction crucible. In the third stage, α-Si3N4 transforms to one dimensional direction which was β-Si3N4 particle. This was followed by the formation of SiC at temperature above 1450°C.

Cd and Hg coordination complexes based on a heterocyclic multidentate ligand: Synthesis, structures and photoluminescence properties

2017 ◽  
Vol 41 (5) ◽  
pp. 275-279
Author(s):  
Jiyong Hu ◽  
Fan Yang ◽  
Jin'an Zhao
Keyword(s):  
Single Crystal ◽  
Coordination Complexes ◽  
Chain Structure ◽  
Photoluminescence Properties ◽  
X Ray Diffraction ◽  
One Dimensional ◽  
X Ray ◽  
Multidentate Ligand ◽  
The Third ◽  
Binuclear Structure

The complexes [Cd(cpbi)Cl2]·(H2O), [Hg2(cpbi)2Cl4] and [Hg(cpbi)Br2] (cpbi = [5-chloro-2-(pyrazin-2-yl)-1H-benzoimidazole]) have been synthesised using solvent evaporation reactions and structurally characterised by single-crystal X-ray diffraction. The first complex displays a one-dimensional (1-D) chain structure, the second has a binuclear structure, while the third is mononuclear. The complexes show different luminescence properties.

Investigation of the products of carbothermal reduction of yttrium oxide by the hydrolysis method

1984 ◽  
Vol 49 (4) ◽  
pp. 936-943 ◽  
Author(s):  
Bohumil Hájek ◽  
Pavel Karen ◽  
Vlastimil Brožek
Keyword(s):  
Yttrium Oxide ◽  
Carbothermal Reduction ◽  
Stoichiometric Ratio ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hydrolysis Method ◽  
Sample Decomposition ◽  
Products Of Reaction ◽  
Hydrolysis Of ◽  
Lower Carbon

For the investigation of the products of reaction of yttrium oxide with carbon mixed in various proportions, the chemical and X-ray diffraction methods of analysis were combined with the gas chromatographic analysis of the mixture of hydrocarbons and hydrogen formed on the sample decomposition with water. The carboreduction of Y2O3 was examined at relatively low temperatures, convenient for obtaining the reaction intermediates in higher yields. At 1 600 °C and pressures of 10-3 Pa the reduction of a mixture of Y2O3 with carbon in a stoichiometric ratio of 1 : 7 yields YC2 in equilibrium with 20% of Y2OC phase. At lower carbon contents (down to the Y2O3 : C ratio of 1 : 2) tha fraction of the Y2OC phase increases up to approximately 30%. In addition to Y2O3, the reaction mixture contains also Y2C, Y2OC and a phase giving propyne on hydrolysis. The presence of traces of C3 hydrocarbons and small amounts of methane in the product of hydrolysis of the carbide sample prepared by the carbothermal reduction of the oxide can be explained in terms of the occurrence of the Y15C19 phase, probably substituted in part by oxygen, and of the Y2OC phase. The results are compared with those obtained previously for the Sc2O3 + C system.

Effect of Calcinations on Characterizations of Fabricated Nano Manganese Ferrite

2013 ◽  
Vol 634-638 ◽  
pp. 2150-2154 ◽  
Author(s):  
Rita Sundari ◽  
Tang Ing Hua ◽  
M. Rusli Yosfiah
Keyword(s):  
Sol Gel ◽  
Volatile Components ◽  
Manganese Ferrite ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Reflectance Analysis ◽  
Transmission Electron Microscope Analysis ◽  
Electron Microscope Analysis ◽  
Nano Size

A citric acid anionic surfactant has been applied for nano manganese ferrite (MnFeO3) fabrication using sol gel method. The calcinations have been varied for 300, 600 and 800oC. The UVDR (UV-Vis Diffused Reflectance) analysis shows a high absorptive band gap after 400 nm for the 600oC calcinated MnFeO3. The DTA (Differential Thermal Analysis) profiles exhibit remarkably trapped volatile matters (H2O, CO2, and NO2) in the fabricated MnFeO3 under sol gel heat treatment at 100oC and the peaks disappeared as the calcination increased to 600oC. As the temperature elevated from 100 to 300oC, the absorption peaks of volatile components are disappeared as demonstrated clearly by the FTIR (Fourier Transform Infrared) spectra of the fabricated material, which 3393 cm-1 corresponded to OH group, 1624 cm-1 to CO group, and 1384 cm-1 to NO group. The XRD (X-Ray Diffraction) spectra show clearly the alteration process from amorphous to crystalline structure as the calcinations increased from 300 to 600oC. In addition, the TEM (Transmission Electron Microscope) analysis exhibits parts of the fabricated MnFeO3 found in cubic nano size of 15-40 nm under interested calcinations and the result is in agreement with that obtained by XRD investigation.

scholarly journals Dislocation Arrangement in a Thick LEO GaN Film on Sapphire

2000 ◽  
Vol 5 (S1) ◽  
pp. 97-103
Author(s):  
Kathleen A. Dunn ◽  
Susan E. Babcock ◽  
Donald S. Stone ◽  
Richard J. Matyi ◽  
Ling Zhang ◽  
...  
Keyword(s):  
High Resolution ◽  
Electron Diffraction ◽  
Threading Dislocations ◽  
X Ray Diffraction ◽  
Burgers Vector ◽  
X Ray ◽  
The Third ◽  
Dislocation Arrangement ◽  
Image Position ◽  
Gan Film

Diffraction-contrast TEM, focused probe electron diffraction, and high-resolution X-ray diffraction were used to characterize the dislocation arrangements in a 16µm thick coalesced GaN film grown by MOVPE LEO. As is commonly observed, the threading dislocations that are duplicated from the template above the window bend toward (0001). At the coalescence plane they bend back to lie along [0001] and thread to the surface. In addition, three other sets of dislocations were observed. The first set consists of a wall of parallel dislocations lying in the coalescence plane and nearly parallel to the substrate, with Burgers vector (b) in the (0001) plane. The second set is comprised of rectangular loops with b = 1/3 [110] (perpendicular to the coalescence boundary) which originate in the coalescence boundary and extend laterally into the film on the (100). The third set of dislocations threads laterally through the film along the [100] bar axis with 1/3<110>-type Burgers vectors These sets result in a dislocation density of ∼109 cm−2. High resolution X-ray reciprocal space maps indicate wing tilt of ∼0.5º.

Formalism for the determination of intermediate stress gradients using X-ray diffraction

2009 ◽  
Vol 42 (2) ◽  
pp. 192-197 ◽  
Author(s):  
Thomas Gnäupel-Herold
Keyword(s):  
Lattice Strain ◽  
Narrow Line ◽  
X Ray Diffraction ◽  
Beam Spot ◽  
Strain Measurements ◽  
One Dimensional ◽  
X Ray ◽  
Stress Gradients ◽  
Shaped Beam

A method is outlined that allows the determination of one-dimensional stress gradients at length scales greater than 0.2 mm. By using standard four-circle X-ray diffractometer equipment and simple aperture components, length resolutions down to 0.05 mm in one direction can be achieved through constant orientation of a narrow, line-shaped beam spot. Angle calculations are given for the adjustment of goniometer angles, and for the effective azimuth and tilt of the scattering vector for general angle settings in a four-circle goniometer. The latter is necessary for the computation of stresses from lattice strain measurements.

Die Kristallstrukturen der isotypen Verbindungen Ba3[MoN4] und Ba3[WN4] / The Crystal Structures of the Isotypic Compounds Ba3[MoN4] and Ba3[WN4]

1991 ◽  
Vol 46 (5) ◽  
pp. 566-572 ◽  
Author(s):  
Axel Gudat ◽  
Peter Höhn ◽  
Rüdiger Kniep ◽  
Albrecht Rabenau
Keyword(s):  
Transition Metals ◽  
Single Crystal ◽  
Crystal Structures ◽  
Structure Type ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ternary Compounds ◽  
The Third

The isotypic ternary compounds Ba3[MoN4] and Ba3[WN4] were prepared by reaction of the transition metals with barium (Ba3N2, resp.) under nitrogen. The crystal structures were determined by single crystal X-ray diffraction: Ba3[MoN4] (Ba3[WN4]): Pbca; Z = 8; a = 1083.9(3) pm (1091.8(3) pm), b = 1030.3(3) pm (1037.5(3) pm), c = 1202.9(3) pm (1209.2(4) pm). The structures contain isolated tetrahedral anions [MN4]6- (M = Mo, W) which are arranged in form of slightly distorted hexagonal layers and which are stacked along [010] with the sequence (···AB···). Two of the three Ba atoms are situated between, the third one is placed within the layers of [MN4]-groups. In this way the structures can be derived from the Na3As structure type.

The Roman Ceramics of Salobrena (Granada-Spain) and their Raw Materials

1992 ◽  
Vol 267 ◽  
Author(s):  
Ana M De Andres ◽  
Isabel MuÑOZ
Keyword(s):  
Thermal Analysis ◽  
Differential Thermal Analysis ◽  
Raw Materials ◽  
Third Century ◽  
Western Coast ◽  
X Ray Diffraction ◽  
X Ray ◽  
The Third ◽  
Good Number ◽  
Scanning Electron

ABSTRACTNineteen roman ceramic sherds found near Salobreña (Granada, Spain), in the western coast of the Mediterranean Sea, as well as different ceramic clays from the surroundingsare studied. Both clays and ceramic sherds are characterizad by X-ray diffraction and spectrometry, differential thermal analysis, and scanning electron and optical microscopies. A good number of the ceramic pieces, among which some “Terrae Sigillatae”, have a composition similar to that of the local clays and, thus, have been probably manufactured at Salobreña. Only a few of them have a foreign origin. For most of them, the firing temperature was about 800-850 °C, although some have been produced at 900-1000 °C, and some others at 1000-1100 °C. It is concluded that Salobreña appearsto have been an important settlement just in the third century of the Christian era.

Synthesis, IR spectrum, thermal behaviour and crystal structure of a novel one-dimensional cyano-bridged zinc(II)/nickel(II) complex

2005 ◽  
Vol 220 (1) ◽  
Author(s):  
Ahmet Karadag ◽  
Hümeyra Pasaoglu ◽  
Gökhan Kastas ◽  
Orhan Büyükgüngör
Keyword(s):  
Crystal Structure ◽  
Thermal Analysis ◽  
Coordination Polymer ◽  
Single Crystal ◽  
Ir Spectrum ◽  
Polymeric Chain ◽  
X Ray Diffraction ◽  
Bimetallic Complex ◽  
One Dimensional ◽  
X Ray

AbstractThe cyano-bridged heteronuclear coordination polymer of zinc(II)/nickel(II) has been prepared by N-(2-hydroxyethyl)-ethylendiamine (hydet-en), alternatively named 2-(2-aminoethylamino)-ethanol and characterised by IR and thermal analysis. In the bimetallic complex, the decomposition of hydet-en ligands is seen to be endothermic whereas that of the cyano ligands is found to be exothermic. The crystal structure of the complex has been determined by single-crystal X-ray diffraction. The crystal structure of the zinc(II)-nickel(II) complex consists of a one-dimensional polymeric chain –Zn(hydet-en)

Metal Phenoxyalkanoic Acid Interactions. XXV. The Crystal Structures of (2-Formyl-6-Methoxyphenoxy)Acetic Acid and Its Zinc(II) Complex and the Lithium, Zinc(II) and Cadmium(II) Complexes of (2-Chlorophenoxy)Acetic Acid

1987 ◽  
Vol 40 (7) ◽  
pp. 1147 ◽  
Author(s):  
EJ Oreilly ◽  
G Smith ◽  
CHL Kennard ◽  
TCW Mak
Keyword(s):  
Acetic Acid ◽  
Crystal Structures ◽  
Free Acid ◽  
Rotational Symmetry ◽  
Carboxyl Groups ◽  
X Ray Diffraction ◽  
X Ray ◽  
The Third ◽  
Planar Complex ◽  
Hydrogen Bonded

The crystal structures of (2-formyl-6-methoxyphenoxy)acetic acid (1), diaquabis [(2-formyl-6-methoxyphenoxy) acetato ]zinc(11) (2), tetraaquabis [(2-chlorophenoxy) acetato ]zinc(11) (3), triaquabis [(2-chlorophenoxy) acetato ]cadmium(11) dihydrate (4) and lithium (2-chloro- phenoxy )acetate 1.5 hydrate (5) have been determined by X-ray diffraction. The acid (1) forms centrosymmetric hydrogen-bonded cyclic dimers [O…0, 2.677(6) �] which are non-planar. Complex (2) is six-coordinate with two waters [Zn- Ow , 1.997(2) �] and four oxygens from two asymmetric bidentate carboxyl groups [Zn-O, 2.073, 2.381(2) �] completing a skew trapezoidal bipyramidal stereochemistry. Complex (5) is also six-coordinate but is octahedral, with two trans-related unidentate carboxyl oxygens [mean Zn-O, 2.134(9) �] and four waters [mean Zn-O, 2.081(9) �]. The seven-coordinate complex (4) has crystallographic twofold rotational symmetry relating two :symmetric bidentate acid ligands [ Cd -O, 2.26, 2 48(:) �] and two waters [ Cd -O, 2.34(2) �] while the third water lies on this axis [ Cd -O, 2.27(2) �]. In contrast to the monomers (2)-(4), complex (5) is polymeric with tetrahedral lithium coordinated to one water and three carboxylate oxygens [mean Li-0, 1.95(1) �]. The essential conformation of the free acid is retained in complexes (2), (3) and (4) but in (5), it is considerably changed.

A Conformational Analysis of the Spirocyclic Quaternary Ammonium Cation [(CH2)4N(CH2)4]+ in its Bromide and Picrate Salts

2004 ◽  
Vol 59 (3) ◽  
pp. 259-263 ◽  
Author(s):  
Uwe Monkowius ◽  
Stefan Nogai ◽  
Hubert Schmidbaur
Keyword(s):  
Gas Phase ◽  
Quaternary Ammonium ◽  
Point Group ◽  
High Yield ◽  
X Ray Diffraction ◽  
X Ray ◽  
Quaternary Ammonium Cations ◽  
Twist Conformation ◽  
Twist Form ◽  
Group D

High-yield syntheses of the bromide (1a) and picrate salts (1b) of the 5-azonia-spiro[4]nonane cation [(CH2)4N(CH2)4]+ are reported. In the single crystal X-ray diffraction analyses of the two salts the spirocyclic quaternary ammonium cations have their five-membered rings in envelop and twist conformations modified by packing forces. The conformation found experimentally for 1a has C2-symmetry as predicted for the gas phase by quantum-chemical calculations (RI-DFT, RI-MP2), but the five-membered rings are intermediate between the expected envelop and the twist form. For 1b, both of the two independent cations can be described as a combination of rings in an envelop and a twist conformation. According to the NMR spectra, in solution the cations are highly flexible and pseudosymmetrical (point group D2d)

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