X-ray diffraction and electron microprobe analysis of sulfide crystals of MIBMIIBS type

1976 ◽  
Vol 35 (1) ◽  
pp. 10-16 ◽  
Author(s):  
M. Charbonnier ◽  
M. Murat
1984 ◽  
Vol 28 ◽  
pp. 367-375 ◽  
Author(s):  
R. G. Johnston ◽  
M. B. Strope ◽  
R. P. Anantatmula

AbstractX-ray diffraction and electron microprobe analysis were used in combination to identify reaction phases that formed on the surfaces of low-carbon steel specimens reacted with a 75% basalt-25% bentonite mixture and anion-doped water in sealed pressure vessels at 100°C and 250°C. Reaction phases on specimen surfaces and in adhering geologic material were identified by conventional X-ray diffraction scans of entire specimens with intact reaction layers. Comparison of results from adhering geologic material and scans of selectively removed layers allowed establishment of approximate reaction gradients in the adhering packing material. Electron microprobe analysis of specimens in cross-section provided quantitative chemical analyses of adhering reaction phases, and identification of reaction layer composition gradients and thicknesses. Magnetite formed on the surface of specimens reacted at 250°C for 4 weeks. Iron-enriched clay was also observed on specimen surfaces and in the adjacent basalt-bentonite mixture. The 100°C experiments yielded surface films of a siderite-structure phase, (Fe,Ca,Mn)CO3, that were not observed in previous experiments with synthetic ground-water. Less extensive iron enrichment of the adjacent clays compared to that seen in the 250°C experiments was observed. The siderite-structure phase generally formed when no carbonate ion was present in the initial solution, implying dissolution of impurity calcite in the bentonite as the controlling factor in the reaction. The results demonstrate the utility of combining X-ray diffraction and electron microprobe analysis for characterization of reaction phases on alloys reacted with complex geologic materials.


Author(s):  
Aleksandar Kremenović ◽  
Biljana Lazic ◽  
Hannes Krüger ◽  
Martina Tribus ◽  
Predrag Vulić

Crystals of KAlSiO4-O1(potassium aluminium silicate) were synthesized using a flux method and analysed utilizing single-crystal X-ray diffraction and electron microprobe analysis. Both methods confirm that the crystals are nonstoichiometric according to K1−xAl1−xSi1+xO4withx= 0.04 (1). KAlSiO4-O1is closely related to the stuffed derivatives of tridymite, although the topology of the Si/Al-ordered framework is different. Six-membered rings of UUDDUD and UUUDDD (U = up and D = down; ratio 2:1) configurations are present in layers parallel to theabplane. In contrast, the framework of tridymite exhibits UDUDUD rings. The crystals are affected by inversion, pseudo-orthorhombic and pseudo-hexagonal twinning.


Author(s):  
G. A. Pribytkov ◽  
I. A. Firsina ◽  
V. V. Korzhova ◽  
M. G. Krinitсyn ◽  
A. A. Polyanskaya

TiC + NiCrBSi binder metal matrix composites were obtained by self-propagating high-temperature synthesis (SHS) in the reaction powder mixtures of titanium, carbon (carbon black) and NiCrBSi alloy. It has been found that steady combustion in a stationary mode occurs when the content of the thermally inert metal binder in reactive mixtures does not exceed 50 vol.%. Porous SHS cakes were crashed and resulting granules were separated to fractions by screening to get the composite powder fraction necessary for coating application. Synthesis products were studied by optical and scanning electron microscopy, X-ray diffraction and electron microprobe analysis. It has been found that the average size of carbide inclusions depends on the content of thermally inert alloy powder in the reaction mixtures and can be purposefully regulated in a wide range. The microhardness of composite powder granules obtained by crushing the SHS conglomerates decreases monotonically with an increasing content of the metal binder having hardness less than that of titanium carbide. According to X-ray diffraction data, the titanium carbide lattice parameter turns out to be considerably less than values known for equiatomic titanium carbide. It has been found by electron microprobe analysis of carbide inclusions in the composite structure that the ratio of carbon and titanium mass contents is 0,21 as compared with 0,25 in equiatomic titanium carbide. Iron and silicon contents in the carbide are negligible, oxygen and nickel contents are below 1 wt.%, and chromium content is 2,5 wt.%. The analysis of known data on the effect of all the above-listed dopants on the titanium carbide lattice allows for a conclusion that the carbon deficit is a main reason of the lattice parameter reduction.


2007 ◽  
Vol 71 (5) ◽  
pp. 519-537 ◽  
Author(s):  
E. Schingaro ◽  
F. Scordari ◽  
S. Matarrese ◽  
E. Mesto ◽  
F. Stoppa ◽  
...  

AbstractVolcanic activity at Mt Vulture lasted throughout the Middle Pleistocene and produced SiO2- undersaturated volcanics. Deposits from the Monte Vulture stratovolcano have been classified into four subsynthems and clustered into the Barile Synthem. In the present investigation, trioctahedral micas from the uppermost units (the Ventaruolo Subsynthem) of the Barile Synthem are considered. The samples are labelled VUT187. The phlogopitic micas were separated from the host rock (an olivinefoidite) and underwent chemical (electron microprobe analysis - EMPA and C-H-N), structural (singlecrystal X-ray diffraction) and spectroscopic (Mössbauer) investigations.The EMPA yielded: MgO (17.62–21.89 wt.%), FeOtot (5.98–9.78 wt.%), TiO2 (1.81–3.92 wt.%) and Al2O3 (14.47–17.98 wt.%), with H2O contents = 2.86 (±0.42) wt.% determined by C-H-N analyses. Mössbauer investigation provided [VI]Fe2+ = 12.6%, [VI]Fe3+ = 87.4%. The chemical and structural data are consistent with the occurrence of Ti-oxy, [VI]M2+ + 2(OH)– ⇋ [VI]Ti4+ + 2O2– + H2, and M3+-oxy substitutions, [VI]M2+ + (OH)– ⇋ [VI]M3+ + O2– + 1/2H2, with M3+ = Fe3+, Al3+. In particular, Fe3+-oxy substitution has affected the Fe2+/Fe3+ ratioin the studied sample. This is probably due to the fact that interaction with underground water or a hydrothermal system may have altered the oxygen fugacity and raised the Fe3+ content of VUT187 phlogopite with respect to magmatic values.


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