scholarly journals Investigations of the Deuterium Permeability of As-Deposited and Oxidized Ti2AlN Coatings

Materials ◽  
2020 ◽  
Vol 13 (9) ◽  
pp. 2085 ◽  
Author(s):  
Lukas Gröner ◽  
Lukas Mengis ◽  
Mathias Galetz ◽  
Lutz Kirste ◽  
Philipp Daum ◽  
...  

Aluminum containing Mn+1AXn (MAX) phase materials have attracted increasing attention due to their corrosion resistance, a pronounced self-healing effect and promising diffusion barrier properties for hydrogen. We synthesized Ti2AlN coatings on ferritic steel substrates by physical vapor deposition of alternating Ti- and AlN-layers followed by thermal annealing. The microstructure developed a {0001}-texture with platelet-like shaped grains. To investigate the oxidation behavior, the samples were exposed to a temperature of 700 °C in a muffle furnace. Raman spectroscopy and X-ray photoelectron spectroscopy (XPS) depth profiles revealed the formation of oxide scales, which consisted mainly of dense and stable α-Al2O3. The oxide layer thickness increased with a time dependency of ~t1/4. Electron probe micro analysis (EPMA) scans revealed a diffusion of Al from the coating into the substrate. Steel membranes with as-deposited Ti2AlN and partially oxidized Ti2AlN coatings were used for permeation tests. The permeation of deuterium from the gas phase was measured in an ultra-high vacuum (UHV) permeation cell by mass spectrometry at temperatures of 30–400 °C. We obtained a permeation reduction factor (PRF) of 45 for a pure Ti2AlN coating and a PRF of ~3700 for the oxidized sample. Thus, protective coatings, which prevent hydrogen-induced corrosion, can be achieved by the proper design of Ti2AlN coatings with suitable oxide scale thicknesses.

1991 ◽  
Vol 6 (9) ◽  
pp. 1913-1918 ◽  
Author(s):  
Jiong-Ping Lu ◽  
Rishi Raj

Chemical vapor deposition (CVD) of titanium oxide films has been performed for the first time under ultra-high vacuum (UHV) conditions. The films were deposited through the pyrolysis reaction of titanium isopropoxide, Ti(OPri)4, and in situ characterized by x-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES). A small amount of C incorporation was observed during the initial stages of deposition, through the interaction of precursor molecules with the bare Si substrate. Subsequent deposition produces pure and stoichiometric TiO2 films. Si–O bond formation was detected in the film-substrate interface. Deposition rate was found to increase with the substrate temperature. Ultra-high vacuum chemical vapor deposition (UHV-CVD) is especially useful to study the initial stages of the CVD processes, to prepare ultra-thin films, and to investigate the composition of deposited films without the interference from ambient impurities.


Holzforschung ◽  
2007 ◽  
Vol 61 (5) ◽  
pp. 523-527 ◽  
Author(s):  
Lothar Klarhöfer ◽  
Florian Voigts ◽  
Dominik Schwendt ◽  
Burkhard Roos ◽  
Wolfgang Viöl ◽  
...  

Abstract Metastable induced electron spectroscopy (MIES), ultraviolet photoelectron spectroscopy (UPS), X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM) were applied to study the interaction of Ti metal atoms with spruce surfaces. Spruce surfaces were produced by planing splints from a spruce bar. Ti atoms were adsorbed from a metal evaporator under ultra-high vacuum conditions. The amount adsorbed corresponds to 10 monolayer equivalents. Strong interactions between the spruce surface and metals atoms occurred. Impinging Ti atoms were oxidized by the spruce surface. No Ti agglomeration or particle formation was observed. The surface was smoothed by the Ti applied and was completely covered by a titanium oxide film.


1992 ◽  
Vol 259 ◽  
Author(s):  
H.-H. Park ◽  
K.-H. Kwon ◽  
B.-H. Koak ◽  
S.-M. Lee ◽  
O.-J. Kwon ◽  
...  

ABSTRACTThe effects of SiO2 reactive ion etching (RIE) in CHF3 / C2F6 on the surface properties of the underlying Si substrate have been studied by X-ray photoelectron spectroscopy (XPS) and secondary ion mass spectrometry (SIMS) techniques. The observed two major modifications are (i) a ∼50nm thick silicon layer which contains carbon and fluorine and (ii) 2∼3nm thick residue layer composed entirely of carbon, fluorine, oxygen and hydrogen on the silicon surface. The thermal behaviors of attributed peaks for C 1s, Si 2p, O 1s and F 1s of residue film have been analyzed after in-situ resistive anneal under ultra high vacuum (UHV) condition. C-F1, C-F2 and C-F3 bonds decompose and form C-CFx (x≤3) bonds above 200°C. Above 400°C, C-CFx bonds also decompose to C-C/H bonds. For recovery of the modified silicon surface, reactive ion etched specimens have been exposed to an oxygen plasma. By XPS analysis, the effect of an O2 plasma treatment has been revealed to be completed within 20min. With an O2 plasma pre-treated, a rapid thermal anneal (RTA) treatment as low as 500°2 is found to be effective for removal of impurities in the silicon.


1991 ◽  
Vol 05 (08) ◽  
pp. 581-585
Author(s):  
H. ZHANG ◽  
S.Q. FENG ◽  
Q.R. FENG ◽  
X. ZHU

We have performed an X-ray photoelectron spectroscopy investigation on single-phase samples of Sn -doped YBCO system, together with structure analysis, oxygen content analysis, and superconductivity measurements. The experiment gave evidence that there is a strong correlation between the electronic states of copper and oxygen. When the sample was heated to 600°C for 20 minutes in vacuum chamber, the oxygen escaped from the sample, the binding energy of Cu 2p was decreased, and the two indistinct components of O 1s became clear. Keeping the sample in ultra-high vacuum for 24 hours, a similar result was obtained.


2012 ◽  
Vol 445 ◽  
pp. 709-713 ◽  
Author(s):  
A. Roustila ◽  
A. Rabehi ◽  
M. Souici ◽  
J. Chene

ZrNi intermetallic compound is used in several application fields due to its very favorable characteristics for the storage of hydrogen. The hydrogen reactions are important, it is vital to examine the evolution of physico-chemical properties at the surface. X-ray photoelectron spectroscopy, is used to follow the evolution of electronic properties of ZrNi versus the ion sputtering in ultra high vacuum in the range 300-600°C. Morever, the evolution of species concentrations at the surface of ZrNi in the range 100-700°C is followed by means of Auger electron spectroscopy. The present results show that temperature and ion sputtering favor significant changes in surface properties of ZrNi. In situ annealing of ZrNi favors the oxygen decontamination associated with segregation of zirconium metal on the surface. The values of binding energies deduced from the reconstruction of XPS spectra, allowed the identification of species present at the surface. The results indicate that nickel is not contaminated and all the obtained sub-oxides are related to bonding states of oxygen with zirconium (Zr2O, ZrO, ZrO2and Zr2O3). The ion sputtering of the surface of ZrNi causes preferential sputtering phenomenon. The later results from the removal of surface layers and from the appearance of zirconium oxide layers initially present on the surface. The results obtained by AES show the segregation of impurities (oxygen and carbon) and of zirconium on the surface of ZrNi. AES observations of Zr segregation start to be important above 300°C and this is in agreement with XPS analysis showing a Zr enrichment of the surface of ZrNi.


2019 ◽  
Vol 64 (1) ◽  
pp. 89-95
Author(s):  
T. T. Magkoev ◽  
V. B. Zaalishvili ◽  
O. G. Burdzieva ◽  
G. E. Tuaev ◽  
G. S. Grigorkina

Adsorption of atoms of Co, Mn, Fe on the calcite surface in ultra-high vacuum and the interaction of the formed adsorption systems with the water have been studied by means of X-ray photoelectron spectroscopy. It is shown that Mn and Fe form solid solutions CaCO3/Mn(Fe)CO3 on the calcite surface, whereas Co preferentially forms CoO and Co3O4. Upon interaction with water the surface compounds formed by Mn and Fe do not undergo notable changes, unlike the Co oxides which partially transform into soluble hydroxylated complexes.


2012 ◽  
Vol 2 (6) ◽  
pp. 291-294
Author(s):  
S. Karakalos

The growth mode of MgCl2 on Ti (0001) and on SiO2 grown on Si (100) was investigated by X-ray Photoelectron Spectroscopy (XPS) under UHV conditions. Magnesium chloride grows on both Ti (0001) single crystal and SiO2 following the Frank-van der Merve, (FM) growth mode.


2019 ◽  
Author(s):  
Timothy J. Gorey ◽  
Yang Dai ◽  
Scott Anderson ◽  
Sungsik Lee ◽  
Sungwon Lee ◽  
...  

In heterogeneous catalysis, atomic layer deposition (ALD) has been developed as a tool to stabilize and reduce carbon deposition on supported nanoparticles. Here, we discuss use of high vacuum ALD to deposit alumina films on size-selected, sub-nanometer Pt/SiO2 model catalysts. Mass-selected Pt24 clusters were deposited on oxidized Si(100), to form model Pt24/SiO2 catalysts with particles shown to be just under 1 nm, with multilayer three dimensional structure. Alternating exposures to trimethylaluminum and water vapor in an ultra-high vacuum chamber were used to grow alumina on the samples without exposing them to air. The samples were probed in situ using X-ray photoelectron spectroscopy (XPS), low-energy ion scattering spectroscopy (ISS), and CO temperature-programmed desorption (TPD). Additional samples were prepared for ex situ experiments using grazing incidence small angle x-ray scattering spectroscopy (GISAXS). Alumina growth is found to initiate at least 60 times more efficiently at the Pt24 cluster sites, compared to bare SiO2/Si, with a single ALD cycle depositing a full alumina layer on top of the clusters, with substantial additional alumina growth initiating on SiO2 sites surrounding the clusters. As a result, the clusters were completely passivated, with no exposed Pt binding sites.


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