scholarly journals Characterization of rutile passivation layers formed on Magnéli-phase titanium oxide inert anodes

2011 ◽  
Vol 44 (4) ◽  
pp. 853-857 ◽  
Author(s):  
Matthew Ryan Rowles ◽  
Nicola V. Y. Scarlett ◽  
Ian C. Madsen ◽  
Katherine McGregor
Keyword(s):  
Ex Situ ◽  
X Ray Diffraction ◽  
X Ray ◽  
Inert Anodes ◽  
Magnéli Phases ◽  
Analysis Technique ◽  
Characterization Study ◽  
Passivation Layers

Anex situcharacterization study has been performed on rutile passivation layers on inert anodes used for molten salt electrochemical studies. Rutile layer thicknesses were estimated using a number ofex situmethods, including laboratory and synchrotron X-ray diffraction and optical microscopy. The only phases in the anode detected by diffraction were the Magnéli phases (TinO2n−1,n= 5–6) of the unreacted anode and rutile (TiO2), which forms on electrolysis. These measurements validate a previously developedin situenergy-dispersive X-ray diffraction analysis technique [Scarlett, Madsen, Evans, Coelho, McGregor, Rowles, Lanyon & Urban (2009).J. Appl. Cryst.42, 502–512].

In Situ Characterization of Ain Films Grown on Silicon by MOCVD

1998 ◽  
Vol 512 ◽  
Author(s):  
A. D. Serra ◽  
H. H. Richardson
Keyword(s):  
Film Growth ◽  
Growth Parameters ◽  
Emission Spectra ◽  
Ex Situ ◽  
X Ray Diffraction ◽  
In Situ Characterization ◽  
X Ray ◽  
Ir Emission

ABSTRACTFilms of AIN were grown on Si under vacuum pressure at 900°C and examined ex situ with infrared reflectance spectroscopy and microscopy, scanning electron microscopy, x-ray diffraction and rutherford backscattering spectroscopy. Collection of IR emission spectra for in situ characterization was successful and used to identify growth parameters during film growth.

The Use of Advanced Analytical Techniques for Characterization of the Chemical, Physical, and Crystallographic Nature of a Surface

1973 ◽  
Vol 31 ◽  
pp. 132-133 ◽  
Author(s):  
R. E. Herfert
Keyword(s):  
Surface Characterization ◽  
Analytical Techniques ◽  
X Ray Diffraction ◽  
Depth Of Penetration ◽  
X Ray ◽  
The Past ◽  
Transmission Electron ◽  
Scanning Electron

Studies of the nature of a surface, either metallic or nonmetallic, in the past, have been limited to the instrumentation available for these measurements. In the past, optical microscopy, replica transmission electron microscopy, electron or X-ray diffraction and optical or X-ray spectroscopy have provided the means of surface characterization. Actually, some of these techniques are not purely surface; the depth of penetration may be a few thousands of an inch. Within the last five years, instrumentation has been made available which now makes it practical for use to study the outer few 100A of layers and characterize it completely from a chemical, physical, and crystallographic standpoint. The scanning electron microscope (SEM) provides a means of viewing the surface of a material in situ to magnifications as high as 250,000X.

In Situ X-Ray Diffraction Investigations during Diffusion Anneals of Ni-Cu Thin Film Diffusion Couples

2010 ◽  
Vol 89-91 ◽  
pp. 503-508 ◽  
Author(s):  
J. Sheng ◽  
U. Welzel ◽  
Eric J. Mittemeijer
Keyword(s):  
Thermal Stresses ◽  
Stress Generation ◽  
Ex Situ ◽  
Diffusion Annealing ◽  
X Ray Diffraction ◽  
Individual Layer ◽  
X Ray ◽  
Bilayer System ◽  
Stress Changes

The stress evolution during diffusion annealing of Ni-Cu bilayers (individual layer thicknesses of 50 nm) was investigated employing ex-situ and in-situ X-ray diffraction measurements. Annealing at relatively low homologous temperatures (about 0.3 - 0.4 Tm) for durations up to about 100 hours results in considerable diffusional intermixing, as demonstrated by Auger-electron spectroscopy investigations (in combination with sputter-depth profiling). In addition to thermal stresses due to differences of the coefficients of thermal expansion of layers and substrate, tensile stress con-tributions in the sublayers arise during the diffusion anneals. The obtained stress data have been discussed in terms of possible mechanisms of stress generation. The influence of diffusion on stress development in the sublayers of the diffusion couple during heating and isothermal annealing was investigated by comparing stress changes in the bilayer system with corresponding results obtained under identical conditions for single layers of the components in the bilayer system. The specific residual stresses that emerge due to diffusion between the (sub)layers in the bilayer could thereby be identified.

Size dependent behavior of Fe3O4crystals during electrochemical (de)lithiation: an in situ X-ray diffraction, ex situ X-ray absorption spectroscopy, transmission electron microscopy and theoretical investigation

2017 ◽  
Vol 19 (31) ◽  
pp. 20867-20880 ◽  
Author(s):  
David C. Bock ◽  
Christopher J. Pelliccione ◽  
Wei Zhang ◽  
Janis Timoshenko ◽  
K. W. Knehr ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Structural Changes ◽  
Ex Situ ◽  
X Ray Diffraction ◽  
X Ray ◽  
Size Dependent ◽  
Transmission Electron ◽  
Dependent Behavior ◽  
X Ray Absorption

Crystal and atomic structural changes of Fe3O4upon electrochemical (de)lithiation were determined.

scholarly journals The Case Study of the Medieval Town Walls of Gubbio in Italy: First Results on the Characterization of Mortars and Binders

Heritage ◽  
2018 ◽  
Vol 1 (2) ◽  
pp. 468-478 ◽  
Author(s):  
Fernanda Carvalho ◽  
Andreia Lopes ◽  
Antonella Curulli ◽  
Teresa da Silva ◽  
Maria Lima ◽  
...  
Keyword(s):  
Polarized Light ◽  
Ex Situ ◽  
X Ray Diffraction ◽  
X Ray ◽  
Heritage Sites ◽  
First Results ◽  
Restoration Practices ◽  
Climate Events

Good conservation and restoration practices of cultural heritage assets rely on the knowledge of original materials. In the framework of the HERACLES Project (HERACLES—HEritage Resilience Against CLimate Events on Site, H2020 Grant Agreement 700395), dealing with the effects of climatic actions and natural hazards on built heritage, a set of important heritage sites are currently under study to improve their resilience against climate events. Among these are the medieval Gubbio Town Walls in Italy. The present work focuses on the mortars and binders of this monument and collected samples related to different parts of the Walls, corresponding to various historical periods of construction and interventions. They were characterized to determine their minerochemical composition, thermal behavior, and morphology. For that purpose, ex-situ laboratory techniques, such as X-ray diffraction (XRD), wavelength dispersive X-ray fluorescence (WDXRF), optical microscopy (OM), polarized light microscopy (PLM), scanning electron microscopy (SEM), and simultaneous differential thermal analysis and thermogravimetry (TG-DTA) were used to discern trends in different sampling areas due to construction/reconstruction periods and building techniques.

scholarly journals A study on preparation and characterization of carbon doped TiO2 nanotubes

2014 ◽  
Vol 6 (1) ◽  
Author(s):  
Srimala Sreekantan ◽  
Roshasnorlyza Hazan ◽  
Zainovia Lockman ◽  
Ishak Mat
Keyword(s):  
Methyl Orange ◽  
Tio2 Nanotubes ◽  
Pure Tio2 ◽  
Ex Situ ◽  
X Ray Diffraction ◽  
Methyl Orange Degradation ◽  
Doped Tio2 ◽  
X Ray ◽  
Carbon Doped

The present study is directed to clarify the influence of carbon doping on the degradation of methyl orange. TiO2 nanotubes were prepared by anodizing titanium foils in a two electrode configuration bath with titanium foil as the anode and platinum as the counter electrode. The electrochemical bathconsists of 1 M Na2SO4 with 0.7 g ammonium fluoride, NH4F. The nanotubes obtained were further doped with carbon via in-situ and ex-situ method. Incorporation of carbon on TiO2 via in-situ method is accomplished during the anodization process by introducing oxalic acid into electrolyte while theex-situ doping involves carbon incorporation into pre-fabricated TiO2 nanotube via flame annealing using carbon blackN330. Characterization such as Scanning Electron Microscope (SEM), Energy Dispersive X-ray Analysis (EDX), and X-Ray Diffraction (XRD) are used to determine the surfacemorphology, composition of dopants, and phases exists. Well ordered nanotube with good adherence and smooth surface was obtained for both methods. When the oxide was annealed, X-ray diffraction analysis revealed the presence of anatase and rutile phase. The photocatalytic properties of thepure TiO2 and carbon doped TiO2 were tested for methyl orange degradation and the result indicated that the in-situ doped TiO2 has much better degradation than the ex-situ and pure TiO2. The percentage of methyl orange degradation for in-situ was 20% and 41% higher than ex-situ doped TiO2 and pure TiO2, respectively.

Synthesis and Characterization of the PANI/ITO Conducting Nanocomposites

2010 ◽  
Vol 663-665 ◽  
pp. 542-545 ◽  
Author(s):  
Bing Jie Zhu ◽  
Xin Wei Wang ◽  
Mei Fang Zhu ◽  
Qing Hong Zhang ◽  
Yao Gang Li ◽  
...  
Keyword(s):  
Doping Concentration ◽  
In Situ Polymerization ◽  
Synthesis And Characterization ◽  
Conductivity Measurements ◽  
X Ray Diffraction ◽  
X Ray ◽  
Maximum Conductivity ◽  
Scanning Electron

The PANI/ITO conducting nanocomposites have been synthesized by in-situ polymerization. The obtained nanocomposites were characterized by X-ray diffraction pattern, scanning electron microscopy and Fourier transform infrared. Electrical conductivity measurements on the samples pressed into pellets showed that the maximum conductivity attained 2.0 ± 0.05 S/cm for PANI/ITO nanocomposites, at ITO doping concentration of 10 wt%. The results of the present work may provide a simple, rapid and efficient approach for preparing PANI/ITO nanocomposites.

scholarly journals Characterization of the Interface Between the Bulk Glass Forming Alloy Zr41Ti14Cu12Ni10Be23 with Pure Metals and Ceramics

2000 ◽  
Vol 15 (7) ◽  
pp. 1617-1621 ◽  
Author(s):  
Jan Schroers ◽  
Konrad Samwer ◽  
Frigyes Szuecs ◽  
William L. Johnson
Keyword(s):  
Sessile Drop ◽  
Bulk Glass ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Glass Forming ◽  
Processing Times ◽  
Thermal Stability Of

The reaction of the bulk glass forming alloy Zr41Ti14Cu12Ni10Be23 (Vit 1) with W, Ta, Mo, AlN, Al2O3, Si, graphite, and amorphous carbon was investigated. Vit 1 samples were melted and subsequently solidified after different processing times on discs of the different materials. Sessile drop examinations of the macroscopic wetting of Vit 1 on the discs as a function of temperature were carried out in situ with a digital optical camera. The reactions at the interfaces between the Vit 1 sample and the different disc materials were investigated with an electron microprobe. The structure and thermal stability of the processed Vit 1 samples were examined by x-ray diffraction and differential scanning calorimetry. The results are discussed in terms of possible applications for composite materials.

Synthesis and Characterization of Tetraphenylphosphonium Tetraazidoborate

2002 ◽  
Vol 57 (6) ◽  
pp. 621-624 ◽  
Author(s):  
Wolfgang Fraenk ◽  
Heinrich Nöth ◽  
Thomas M. Klapötke ◽  
Max Suter
Keyword(s):  
Single Crystal ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray

AbstractTetraphenylphosphonium tetraazidoborate, [P(C6H5)4][B(N3)4], was obtained from B(N3)3 - in situ prepared from BH3 · O(C2H5)2 and HN3 - and [P(C6H5)4][N3]. Recrystallization from an acetonitrile / hexane mixture yielded colorless crystals in 60% yield. The molecular structurewas determined by single crystal X-ray diffraction and the [B(N3)4]- anionwas shown to possess S4 symmetry.

scholarly journals The Viscosity and Atomic Structure of Volatile-Bearing Melilititic Melts at High Pressure and Temperature and the Transport of Deep Carbon

Minerals ◽  
2020 ◽  
Vol 10 (3) ◽  
pp. 267 ◽  
Author(s):  
Vincenzo Stagno ◽  
Veronica Stopponi ◽  
Yoshio Kono ◽  
Annalisa D’Arco ◽  
Stefano Lupi ◽  
...  
Keyword(s):  
Experimental Data ◽  
High Pressure ◽  
Atomic Structure ◽  
Ex Situ ◽  
X Ray Diffraction ◽  
High Pressure And Temperature ◽  
X Ray ◽  
Falling Sphere ◽  
Basaltic Melts

Understanding the viscosity of mantle-derived magmas is needed to model their migration mechanisms and ascent rate from the source rock to the surface. High pressure–temperature experimental data are now available on the viscosity of synthetic melts, pure carbonatitic to carbonate–silicate compositions, anhydrous basalts, dacites and rhyolites. However, the viscosity of volatile-bearing melilititic melts, among the most plausible carriers of deep carbon, has not been investigated. In this study, we experimentally determined the viscosity of synthetic liquids with ~31 and ~39 wt% SiO2, 1.60 and 1.42 wt% CO2 and 5.7 and 1 wt% H2O, respectively, at pressures from 1 to 4.7 GPa and temperatures between 1265 and 1755 °C, using the falling-sphere technique combined with in situ X-ray radiography. Our results show viscosities between 0.1044 and 2.1221 Pa·s, with a clear dependence on temperature and SiO2 content. The atomic structure of both melt compositions was also determined at high pressure and temperature, using in situ multi-angle energy-dispersive X-ray diffraction supported by ex situ microFTIR and microRaman spectroscopic measurements. Our results yield evidence that the T–T and T–O (T = Si,Al) interatomic distances of ultrabasic melts are higher than those for basaltic melts known from similar recent studies. Based on our experimental data, melilititic melts are expected to migrate at a rate ~from 2 to 57 km·yr−1 in the present-day or the Archaean mantle, respectively.

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