scholarly journals Electrochemical synthesis and characterization of BaB6 from molten melt

2009 ◽  
Vol 45 (1) ◽  
pp. 101-109 ◽  
Author(s):  
T.P. Jose ◽  
L. Sundar ◽  
L.J. Berchmans ◽  
A. Visuvasam ◽  
S. Angappan
Keyword(s):  
Molten Salt ◽  
Lithium Fluoride ◽  
Barium Carbonate ◽  
Supporting Electrolyte ◽  
Eutectic Point ◽  
Graphite Crucible ◽  
Electrolytic Cell ◽  
Phase Identification ◽  
X Ray Diffraction ◽  
Micron Size

Barium hexaboride (BaB6) crystals were electrochemically synthesized using molten salt technique. Barium carbonate (BaCO3) and boron trioxide (B2O3) was used as reactants. Lithium fluoride (LiF) was used as the supporting electrolyte. The molten electrolyte consisted of 50 wt % BaCO3 and B2O3 with different stiochiometric ratios of Ba and B and 50 wt % lithium fluoride. DTA/TGA studies were made to determine the eutectic point of the melt and it was found to be around 821oC. The electrolytic cell had a high purity graphite crucible, which served as the electrolyte holding vessel and also as the anode for the electrolysis. An electro-polished molybdenum rod was employed as the cathode. The electrolysis was performed at 870?C under argon atmosphere, at current densities ranging from 0.2-0.5 A/cm2. The electrodeposited crystals were examined for the phase identification using X-ray diffraction technique. The AAS and the chemical analysis were made for the determination of chemical composition of the synthesized crystals. The purity of the crystals was also assessed using ICP-MS, XRF and EDX, which reveal that the crystals were associated with trace amount of impurities like oxygen, carbon and iron. The compound is found to be more than 99 % pure. The morphology of the crystals was examined using Scanning Electron Microscopy (SEM). From the above studies, it is concluded that the molten salt process is a simple preparative procedure for the synthesis of sub-micron size barium hexaboride crystals.

Electron Microscopy/Diffraction Study of the Ternary Mn-Er-S System

1990 ◽  
Vol 48 (1) ◽  
pp. 76-77
Author(s):  
A. R. Landa Canovas ◽  
L.C. Otero Diaz ◽  
T. White ◽  
B.G. Hyde
Keyword(s):  
Electron Microscopy ◽  
Gas Flow ◽  
Graphite Crucible ◽  
Nominal Composition ◽  
X Ray Diffraction ◽  
Alumina Crucible ◽  
X Ray ◽  
Intermediate Phases ◽  
Twin Band ◽  
Ar Gas

X-Ray diffraction revealed two intermediate phases in the system MnS+Er2S3,:MnEr2S4= MnS.Er2S3, and MnEr4S7= MnS.2Er2S3. Their structures may be described as NaCl type, chemically twinned at the unit cell level, and isostructural with CaTi2O4, and Y5S7 respectively; i.e. {l13} NaCl twin band widths are (4,4) and (4,3).The present study was to search for structurally-related (twinned B.) structures and or possible disorder, using the more sensitive and appropiate technigue of electron microscopy/diffraction.A sample with nominal composition MnEr2S4 was made by heating Mn3O4 and Er2O3 in a graphite crucible and a 5% H2S in Ar gas flow at 1500°C for 4 hours. A small amount of this material was thenannealed, in an alumina crucible, contained in sealed evacuated silica tube, for 24 days at 1100°C. Both samples were studied by X-ray powder diffraction, and in JEOL 2000 FX and 4000 EX microscopes.

scholarly journals Preliminary Study of the Targeted Cleaning of an Artificial Gypsum Layer on White Marble

Coatings ◽  
2021 ◽  
Vol 11 (1) ◽  
pp. 37
Author(s):  
Yan Liu ◽  
Taoling Dong ◽  
Kun Zhang ◽  
Fuwei Yang ◽  
Liqin Wang
Keyword(s):  
Electron Microscopy ◽  
Barium Carbonate ◽  
Color Difference ◽  
X Ray Diffraction ◽  
White Marble ◽  
Capillary Suction ◽  
Sulfate Ions ◽  
X Ray ◽  
Preliminary Study ◽  
Scanning Electron

Targeting cleaning of the artificial gypsum layer on white marble was studied. It was conducted by means of the specific depletion of the calcium and sulfate ions by the barium carbonate scavenger, which led to the continuous dissolution and clearance of gypsum layer. The cleaning effect was evaluated by scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM/EDX), X-ray diffraction (XRD), capillary suction, and color difference measurement. By this method, only the gypsum layer was cleared away and the carbonate substrate of marble was left intact at the same time. This method will be highly useful for the conservation of marble relics from surface weathering.

scholarly journals An Insight into Chemistry and Structure of Colloidal 2D-WS2 Nanoflakes: Combined XPS and XRD Study

Nanomaterials ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 1969
Author(s):  
Riccardo Scarfiello ◽  
Elisabetta Mazzotta ◽  
Davide Altamura ◽  
Concetta Nobile ◽  
Rosanna Mastria ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Xrd Analysis ◽  
Crystal Habit ◽  
Phase Identification ◽  
X Ray Diffraction ◽  
X Ray ◽  
Morphological Evaluation ◽  
Rational Understanding ◽  
Structural Inspection

The surface and structural characterization techniques of three atom-thick bi-dimensional 2D-WS2 colloidal nanocrystals cross the limit of bulk investigation, offering the possibility of simultaneous phase identification, structural-to-morphological evaluation, and surface chemical description. In the present study, we report a rational understanding based on X-ray photoelectron spectroscopy (XPS) and structural inspection of two kinds of dimensionally controllable 2D-WS2 colloidal nanoflakes (NFLs) generated with a surfactant assisted non-hydrolytic route. The qualitative and quantitative determination of 1T’ and 2H phases based on W 4f XPS signal components, together with the presence of two kinds of sulfur ions, S22− and S2−, based on S 2p signal and related to the formation of WS2 and WOxSy in a mixed oxygen-sulfur environment, are carefully reported and discussed for both nanocrystals breeds. The XPS results are used as an input for detailed X-ray Diffraction (XRD) analysis allowing for a clear discrimination of NFLs crystal habit, and an estimation of the exact number of atomic monolayers composing the 2D-WS2 nanocrystalline samples.

THE SOLIDIFICATION MICROSTRUCTURE OF BIOMEDICAL TITANIUM ALLOYS UNDER THE CENTRIFUGAL FORCE

2006 ◽  
Vol 20 (25n27) ◽  
pp. 4685-4690
Author(s):  
ZIYONG CHEN ◽  
LIJUAN XU ◽  
ZHIGUANG LIU ◽  
YUYONG CHEN
Keyword(s):  
Centrifugal Force ◽  
Graphite Crucible ◽  
Xrd Analysis ◽  
X Ray Diffraction ◽  
Crystal Boundary ◽  
X Ray ◽  
Solidification Defects ◽  
Solidification Microstructures ◽  
Centrifugal Equipment ◽  
Graphite Mould

Two biomedical alloys, Ti -39 Nb -5.1 Ta -7.1 Zr ( TNTZ1 ) and Ti -35.3 Nb -5.1 Ta -7.1 Zr ( TNTZ2 ) were melted using LZ5 type centrifugal equipment for casting titanium. The solidification microstructures of TNTZ1 and TNTZ2 alloys cast in graphite crucible without centrifugal force are mostly big arborescent crystal with dispersed porosity in it. After pouring into a graphite mould under centrifugal force, the lower part of ingot showed mostly arborescent crystals with few equiaxed crystals, while the upper part of ingot is basically spherical equiaxed crystals. The solidification defects, such as dispersed pores were very difficult to find. Nb is supposed to refine the arborescent crystals. X-ray diffraction (XRD) analysis showed Ti -phase and Nb -phase existing in the above two alloys. The content of Ti was found relatively low in crystal interior and relatively high in crystal boundary. The content of Nb/Zr was uniform in whole microstructure.

scholarly journals Study of Molten Salt Corrosion of Superni-75 using Termogravimetric Technique

1970 ◽  
Vol 3 (2) ◽  
pp. 77-82 ◽  
Author(s):  
TS Sidhu ◽  
S Prakash ◽  
RD Agrawal
Keyword(s):  
Corrosion Resistance ◽  
Molten Salt ◽  
Hot Corrosion ◽  
Corrosion Behaviour ◽  
Thick Layer ◽  
X Ray Diffraction ◽  
Salt Corrosion ◽  
Marine Engineering ◽  
The Given ◽  
Kinetics Of

The present study aims to evaluate the hot corrosion behaviour of the Ni-based alloy Superni- 75 in the molten salt environment of Na2SO-60%V2O5 at 900°C under cyclic conditions. The thermogravimetric technique was used to establish the kinetics of corrosion. X-ray diffraction, scanning electron microscopy/energy-dispersive analysis and electron probe microanalysis techniques were used to analyse the corrosion products. Superni-75 has successfully provided the hot corrosion resistance to the given molten salt environment. The hot corrosion resistance of the Superni-75 has been attributed to the formation of uniform, homogeneous and adherent thick layer of the scale consisting mainly of oxides of nickel and chromium, and refractory Ni(VO3)2. These oxides and refractory nickel vanadates have blocked the penetration of oxygen and other corrosive species to the substrate. Keywords: Hot corrosion, nickel-based alloy, superalloy, molten salt environment   DOI: 10.3329/jname.v3i2.922 Journal of Naval Architecture and Marine Engineering 3(2006) 77-82

Diffraction

2012 ◽  
Vol 20 (2) ◽  
pp. 7-7
Author(s):  
Charles Lyman
Keyword(s):  
Electron Diffraction ◽  
100Th Anniversary ◽  
Primary Phase ◽  
Phase Identification ◽  
X Rays ◽  
X Ray Diffraction ◽  
Identification Methods ◽  
X Ray ◽  
Structure Of Matter

This year marks the 100th anniversary of the discovery of X-ray diffraction and the 85th anniversary of electron diffraction (see Microscopy Pioneers). For most of the time since their introduction, microscopists have known these two techniques as the primary phase identification methods used in conjunction with various microscopies. However, these two diffraction methods also have played enormous roles in understanding the structure of matter, as well as the nature of both X rays and electrons.

scholarly journals Electroless Deposition of Cu-SWCNT Composites

2019 ◽  
Vol 5 (4) ◽  
pp. 61 ◽  
Author(s):  
Raja ◽  
Esquenazi ◽  
Jones ◽  
Li ◽  
Brinson ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Electroless Deposition ◽  
Reaction Times ◽  
Phase Identification ◽  
X Ray Diffraction ◽  
Copper Surfaces ◽  
X Ray ◽  
Dispersing Agent ◽  
Defect Sites ◽  
Walled Carbon Nanotubes

In this work, as-received HiPCO single walled carbon nanotubes (SWCNTs) are incorporated in a controllable manner at various concentrations into Cu-SWCNT composites via electroless plating, by varying the related reaction times, with polyethylene glycol (PEG) used as a dispersing agent. The resultant samples were analyzed using scanning electron microscopy (SEM) for morphology assessment, energy dispersive X-ray analysis (EDX) and X-ray photoelectron spectroscopy (XPS) for elemental analysis, X-ray diffraction (XRD) for the assessment of crystal phase identification, and Raman spectroscopy for the confirmation of the presence of the incorporated SWCNTs. The Cu-SWCNT composites were found to contain carbon, catalytic iron (associated with the raw, as-received SWCNTs), oxygen, and copper; the latter was found to be inversely proportional to carbon and iron contents. The oxygen (associated with both the SWCNT defect sites and oxidized copper surfaces) remained more or less constant regardless of the proportion of SWCNTs in the composites. The Raman IG:ID ratio remains within the experimental error constant, indicating that the electroless deposition does not have a deleterious effect on the SWCNTs. At short deposition times, SEM revealed a relatively dense structure comprising a distinctive fibrous morphology, suggestive of an underlying SWCNT substrate coated with copper; however, with increasing deposition, a more porous morphology is observed. The size of the granular particles increases up until 10 min of reaction, after which time it remains unchanged.

scholarly journals Study on the nonexistence of liquid miscibility gap in the Ce-Mn system

2007 ◽  
Vol 43 (1) ◽  
pp. 21-28 ◽  
Author(s):  
C. Tang ◽  
Y. Du ◽  
H. Xu ◽  
S. Hao ◽  
L. Zhang
Keyword(s):  
Xrd Analysis ◽  
Miscibility Gap ◽  
Composition Analysis ◽  
Phase Identification ◽  
X Ray Diffraction ◽  
X Ray ◽  
Microstructure Observation ◽  
Arc Melting ◽  
Ice Water ◽  
Liquid Miscibility Gap

To ascertain whether the liquid miscibility gap exists in the Ce-Mn system, 3 key alloys are prepared by arc melting the pure elements, annealed at specified temperature for 20 minutes, quenched in ice water and then subjected to X-ray diffraction (XRD) analysis for phase identification and to scanning electron microscopy (SEM) with energy dispersive X-ray analysis for microstructure observation and composition analysis. The XRD examination indicated that terminal solutions based on Ce and Mn exist in the water-quenched alloys. No compound was detected. Microstructure observation and composition analysis indicate the nonexistence of the liquid miscibility gap. The newly assessed Ce-Mn phase diagram was presented. .

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