New precision technique for measuring the concentration versus depth of hydrogen in solids

Lanford, W. A.; Trautvetter, H. P.; Ziegler, J. F.; Keller, J. G.

doi:10.1063/1.88826

Cited by 354 publications

(82 citation statements)

References 6 publications

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“…The total D-content of these samples was determined by means of ERD using 3.5 MV Singletron accelerator (HVEE). 12 C reaction [17,18] were performed on equivalent samples after exposure to a hydrogen flux (1 sccm) for periods of 4 and 5 hours. The angle of incidence between the sample surface and the incoming beam was 15°.…”

Section: Methodsmentioning

confidence: 99%

Hydrogen-induced blistering of Mo/Si multilayers: Uptake and distribution

2013

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We report on the uptake of deuterium by thin-film Mo/Si multilayer samples as a result of exposure to fluxes of predominantly thermal atomic and molecular species, but also containing a small fraction of energetic (800-1000 eV) ions. These exposures result in blister formation characterized by layer detachment occurring exclusively in the vicinity of the Mo-on-Si interfaces.This localization is attributed to strained centres introduced within the interfacial region during silicide formation and subsequent Mo crystallization. The correlation between D-content and blistering was studied. After an initial uptake period the D-content stabilized at ~1.3×10 vacancies within the layer as a consequence of its polycrystalline structure and its highlyconstrained state.

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Section: Methodsmentioning

confidence: 99%

Hydrogen-induced blistering of Mo/Si multilayers: Uptake and distribution

2013

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“…The technique is based on the 1 H( 15 N,αγ) 12 C nuclear resonance reaction and provides the depth profile as well as the total amount of hydrogen per metallic atom [32]. For the profiling, the sample is bombarded with 15 N ions with an energy equal to or above the resonance energy (6.385 MeV).…”

Section: Methodsmentioning

confidence: 99%

Structural and optical properties of MgxAl1-xHy gradient thin films: a combinatorial approach

et al. 2006

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The structural, optical and dc electrical properties of Mg x Al 1−x (0.2 ≤ x ≤ 0.9) gradient thin films covered with Pd/Mg are investigated before and after exposure to hydrogen. We use Hydrogenography, a novel high-throughput optical technique to map simultaneously all the hydride forming compositions and the kinetics thereof in the gradient thin film. Metallic Mg in the Mg x Al 1−x layer undergoes a metal-to-semiconductor transition and MgH 2 is formed for all Mg fractions x investigated. The presence of an amorphous Mg-Al phase in the thin film phase diagram enhances strongly the kinetics of hydrogenation. In the Al-rich part of the film, a complex H-induced segregation of MgH 2 and Al occurs. This uncommon large-scale segregation is evidenced by metal and hydrogen profiling using Rutherford backscattering spectrometry and resonant nuclear analysis based on the reaction 1 H( 15 N,αγ) 12 C. Besides MgH 2 , an additional semiconducting phase is found by electrical conductivity measurements around an atomic [Al]/[Mg] ratio of 2 (x = 0.33). This suggests that the film is partially transformed into Mg(AlH 4 ) 2 at around this composition.

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“…The H concentrations were measured at the Dynamitron accelerator at the State University of New York at Albany with resonant nuclear reaction analysis, using the nuclear reaction 15N + 1H ~ 12C + 4He + ",/ (Lanford et al, 1976). This reaction has a large crosssection at a 15N beam energy of 6.385 MeV.…”

Section: Nuclear Reaction Analysismentioning

confidence: 99%

Mechanisms and Crystal Chemistry of Oxidation in Annite: Resolving the Hydrogen-Loss and Vacancy Reactions

Rancourt

2001

Clays and clay miner.

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Abstract--A synthetic octahedral-site-vacancy-free annite sample and its progressive oxidation, induced by heating in air, were studied by powder X-ray diffraction (pXRD), M6ssbauer spectroscopy, nuclear reaction analysis (NRA), Raman spectroscopy, X-ray fluorescence (XRF) spectroscopy, gas cba-omatography (GC), thennogravimetric analysis (TGA), differential thermal analysis (DTA), scanning electron microscopy (SEM), and size-fraction separation methods. For a set heating time and as temperature is increased, the sample first evolves along an annite--oxyannite join, until all H is lost via the oxybiotite reaction (Fe 2+ + OH-~ Fe 3+ + 0 2-+ Hd'). It then evolves along an oxyannite-feiTioxyanuite join, where ideal ferrioxyannite, KFe3+s/3[~mA1Si3012, is defined as the product resulting from complete oxidation of ideal oxyannite, KFe3+2FeZ+A1Si30~2, via the vacancy mechanism (3 Fe z+ ~ 2 Fe 3+ + I61[~ + Fe1"). A pillaring collapse transition is observed as a collapse of c near the point where FeZ+/Fe = 1B and all OH groups are predicted and observed to be lost. Quantitative analyses of H, using NRA, GC, and Raman spectroscopy, corroborate this interpretation and, in combination with accurate ferric/ferrous ratios from M6ssbauer spectroscopy and lattice parameter determinations, allow a clear distinction to be made between vacancy-free and vacancybearing annite. The amount of Fe in ancillary Fe oxide phases produced by the vacancy mechanism is measured by M6ssbauer spectroscopy to be 1 1.3(5)% of total Fe, in agreement with both the theoretical prediction of 1/9 = 11.1% and the observed TGA weight gain. The initiation of Fe oxide formation near the point of completion of the oxybiotite reaction (FeZ+/Fe = 1B) is con-oborated by pXRD, TGA, Raman spectroscopy, and appearance of an Fe oxide hyperfine field sextet in the M6ssbaner spectra. The region of Fe oxide folTnation is shown to coincide with a region of octahedral site vacancy formation, using a new MOssbauer spectral signature of vacancies that consists of a component at 2.2 mm/s in the I6~Fe3+ quadrupole splitting distribution (QSD). The crystal chemical behaviors of annite--oxyannite and of oxyannite fen-ioxyannite are best contrasted and compared to the behaviors of other layer-silicate series in terms of b vs. [D] (average octahedral cation to O bond length). This also leads to a diagnostic test for the presence of octahedral site vacancies in hydrothermally synthesized annite, based on a graph of b vs. Fe2+/Fe. The implications of the observed sequence of thermal oxidation reactions for the thermodynamic relevance of the oxybiotite and vacancy reactions in hydrothermal syntheses are examined and it is concluded that the oxybiotite reaction is the relevant reaction in the single-phase stability field of annite, at high hydrogen fugacity and using ideal starting cation stoichiometry. The vacancy reaction is only relevant in a multi-phase field, at lower hydrogen fugacity, that includes an Fe oxide equilibrium phase (magnetite) that can effectively compete ...

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New precision technique for measuring the concentration versus depth of hydrogen in solids

Cited by 354 publications

References 6 publications

Hydrogen-induced blistering of Mo/Si multilayers: Uptake and distribution

Hydrogen-induced blistering of Mo/Si multilayers: Uptake and distribution

Structural and optical properties of MgxAl1-xHy gradient thin films: a combinatorial approach

Mechanisms and Crystal Chemistry of Oxidation in Annite: Resolving the Hydrogen-Loss and Vacancy Reactions

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