scholarly journals Study of Ti-V-Cr metal hydrides by neutron powder diffraction

2014 ◽  
Vol 70 (a1) ◽  
pp. C1762-C1762
Author(s):  
Thomas Bibienne ◽  
Roxana Flacau ◽  
Jean-Louis Bobet ◽  
Jacques Huot

Metal hydrides are interesting materials from a fundamental as well as practical point of view. In particular, Ti-based BCC solid solutions are considered as promising candidates for mobile applications because of their high volumetric capacities and room temperature operation. However, the slow kinetics of the first hydrogenation, the so-called activation step, is an important hurdle in the use of these alloys for practical applications. It has recently been shown that doping a Ti-V-Cr composition with Zr7Ni10 leads to a fast activation kinetic without heating treatment [1]. We studied the effect of this doping on two new Ti-V-Cr compositions: 52Ti-12V-36Cr and 42Ti-21V-37Cr. Two different doping methods were investigated: i) a single-melt synthesis where the raw materials (i.e. Ti, V, Cr, Zr and Ni) chunks were mixed and arc-melted; ii) co-melt synthesis where 52Ti-12V-36Cr and 7Zr-10Ni were arc-melted independently and thereafter re-melted together. Using only X-ray diffraction for structural identification does not provide information about hydrogen localization. Therefore, neutron diffraction is essential for complete determination of this class of hydrides. The peculiarity of the present alloys is that, for neutron diffraction, the scattering lengths of the elements almost cancel. Therefore, the neutron pattern of as-cast alloy shows very small Bragg peaks but the advantage is that the hydride is very easy to see and analyze. We performed in-situ neutron diffraction experiments during dehydrogenation of these materials to see the transition from the dihydride to monohydride. These measurements were complementary to X-ray and synchrotron radiation diffraction and enabled a better crystal structure determination of these alloys

2014 ◽  
Vol 70 (a1) ◽  
pp. C939-C939
Author(s):  
Jacques Huot ◽  
Catherine Gosselin ◽  
Thomas Bibienne ◽  
Roxana Flacau

Metal hydrides are interesting materials from a fundamental as well as practical point of view. Hydrogen storage applications have been the main driving force of research on these materials but lately uses such as thermal storage are considered. In this presentation we will review the use of neutron diffraction for the development of new metal hydrides. Two systems will be presented: BCC solid solution alloys and FeTi alloy. Ti-based BCC solid solutions are promising material for hydrogen storage applications which need high volumetric capacity and room temperature operation. One system that has been considered is Ti-V-Cr. Using only X-ray diffraction for structural identification does not provide information about hydrogen localization. Therefore, neutron diffraction is essential for complete determination of this class of hydrides. We will present examples of Ti-V-Cr compounds doped with Zr-Ni alloy. The peculiarity of this type of alloy is that, for neutron diffraction, the scattering lengths of the elements almost cancel. Therefore, the neutron pattern of as-cast alloy shows very small Bragg peaks but the advantage is that the hydride for is very easy to see and analyze. Another good candidate for hydrogen storage applications is the intermetallic compound TiFe which operates at around room temperature (RT) under mild pressure conditions. However one disadvantage of TiFe alloy synthesized by conventional metallurgical method is its poor activation characteristics. The alloy reacts with hydrogen only after complicated activation procedure involving exposure to high temperature (~4000C) and high pressure for several days. Recently we found that by doping this alloy with Zr and Zr7Ni10 the activation could be easily done at room temperature. We present here a neutron diffraction study of these compounds that shows the structural difference between the activated compound and the one cycled under hydrogen.


2014 ◽  
Vol 70 (a1) ◽  
pp. C1767-C1767
Author(s):  
Catherine Gosselin ◽  
Jacques Huot ◽  
Roxana Flacau

Metal hydrides are interesting materials from a fundamental as well as practical point of view. Hydrogen storage applications have been the main driving force of research on these materials but lately, uses such as thermal storage are considered. In this presentation, we will review the use of neutron diffraction for the development of new metal hydrides. A good candidate for hydrogen storage applications is the low cost intermetallic compound TiFe which operates near room temperature (RT) under mild pressure conditions. However, the biggest disadvantage of TiFe alloy synthesized by conventional metallurgical method is it poor activation characteristics [1]. The alloy reacts with hydrogen only after complicated activation procedure involving exposure to high temperature (~4000C) and high pressure for several days. In the '90, some researches showed that the change in the nanocristallinity can modify the sorption property of the TiFe[2]. Other research works found that palladium increase the contaminant resistance. However, addition of palladium is too expansive for practical applications [3]. Recently, we found that, when doping TiFe with Zr and Zr7Ni10, the activation could be easily done at room temperature. We present here a neutron diffraction study of these compounds that shows the structural difference between the activated compound and the one cycled under hydrogen.


Author(s):  
Jiří Zimák ◽  
Kristýna Dalajková ◽  
Roman Donocik ◽  
Petr Krist ◽  
Daniel Reif ◽  
...  
Keyword(s):  

Minerals ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 232
Author(s):  
Pedro J. Sánchez-Soto ◽  
Eduardo Garzón ◽  
Luis Pérez-Villarejo ◽  
George N. Angelopoulos ◽  
Dolores Eliche-Quesada

In this work, an examination of mining wastes of an albite deposit in south Spain was carried out using X-ray Fluorescence (XRF), X-ray diffraction (XRD), particle size analysis, thermo-dilatometry and Differential Thermal Analysis (DTA) and Thermogravimetric (TG) analysis, followed by the determination of the main ceramic properties. The albite content in two selected samples was high (65–40 wt. %), accompanied by quartz (25–40 wt. %) and other minor minerals identified by XRD, mainly kaolinite, in agreement with the high content of silica and alumina determined by XRF. The content of Na2O was in the range 5.44–3.09 wt. %, being associated with albite. The iron content was very low (<0.75 wt. %). The kaolinite content in the waste was estimated from ~8 to 32 wt. %. The particle size analysis indicated values of 11–31 wt. % of particles <63 µm. The ceramic properties of fired samples (1000–1350 °C) showed progressive shrinkage by the thermal effect, with water absorption and open porosity almost at zero at 1200–1250 °C. At 1200 °C, the bulk density reached a maximum value of 2.38 g/cm3. An abrupt change in the phase evolution by XRD was found from 1150 to 1200 °C, with the disappearance of albite by melting in accordance with the predictions of the phase diagram SiO2-Al2O3-Na2O and the system albite-quartz. These fired materials contained as main crystalline phases quartz and mullite. Quartz was present in the raw samples and mullite was formed by decomposition of kaolinite. The observation of mullite forming needle-shape crystals was revealed by Scanning Electron Microscopy (SEM). The formation of fully densified and vitrified mullite materials by firing treatments was demonstrated.


2019 ◽  
Vol 27 (2) ◽  
pp. 69-76
Author(s):  
N. Yu. Filonenko ◽  
A. N. Galdina

In this paper we investigate the phase composition and phase transformations in the Fe-B system alloys with boron content in the range of 9.0–15.0 wt.%. We use microstructural, X-ray diffraction, differential thermal and durometric analyzes to determine the physical properties of the alloys. The experimental findings show that in the as-cast alloy structure there is Fe5B3 phase in small quantities along with FeB monoboride and Fe2B boride. The Fe5B3 phase is formed as a result of the peritectic reaction L+FeB→Fe5B3 at the temperature of 1680 K. The eutectic transformation L→Fe5B3 +Fe2B occurs in the boron concentration range of 8.8–10.5 wt.%. After annealing of the Fe-B alloys at the temperature of 1473 K and cooling with the rate of 102 K/s we observe the occurring of the Fe5B3 phase. To spot an opportunity of the secondary monoboride formation in the alloys under consideration, we calculate the thermodynamic characteristics of stability of the system. Accounting for the contribution of the first degree approximation of high-temperature expansion of thermodynamic potential of FeB iron monoboride in a Fe-B binary alloy enables us to study its thermodynamic stability. It is shown that stability decrease of FeB at 1423 K allows suggesting that at this temperature the phase transformation occurs and this fact correlates to the differential thermal analysis results.


1962 ◽  
Vol 28 (2) ◽  
pp. 234-238 ◽  
Author(s):  
Edward J. Olsen

AbstractThe X-ray spectrometer method as an archaeological tool is discussed with special reference to its limitations as a chemical analytical instrument. Qualitative results are presented for six North American copper samples, one European trade brass, and nine artifacts from the Great Lakes region. From this pilot study it is concluded that the most fruitful results in the problem of the determination of provenance of copper artifacts will be obtained from semi-quantitative optical spectographic analyses of carefully collected artifacts and raw materials. The largest inherent error in this problem is that of meaningful sampling techniques. The only recourse is to treat such chemical data statistically and determine the probabilities that given specimens came from the various possible sources.


2021 ◽  
Vol 87 (8) ◽  
pp. 19-22
Author(s):  
D. G. Filatova ◽  
A. A. Arkhipenko ◽  
M. A. Statkus ◽  
I. V. Mikheev ◽  
V. B. Baranovskaya ◽  
...  

An approach to the simultaneous isolation of As (III) and Se (IV) from solutions on a new S,N-containing sorbent followed by determination of the analyte in the sorbent phase using total reflection X-ray fluorescence (TXRF) has been proposed. To match the goal, a sorbent with a branched structure was synthesized on the base of polyacrylamide modified with formaldehyde and hydrogen sulfide. This is a heteroatomic copolymer containing sulfide bridges in the chain and crosslinking by a tertiary amine. Conditions for the quantitative co-extraction of As (III) and Se (IV), i.e., sorption in solutions of 1 M HNO3 with calcium ions present, heating to 60°C and phase contact time of 1 h were determined. The mechanism of sorption interaction of the analytes under specified conditions is discussed. It is shown that a 100-fold excess of iron, zinc and copper does not interfere with the extraction of analytes, thus providing the possibility of As (III) and Se (IV) isolation from different types of raw materials and processed products using the synthesized sorbent. A method for the direct XRF quantification of arsenic and selenium with sr 0.09 and 0.08, respectively, in the sorbent phase has been developed. The correctness of the results was confirmed by the ICP-MS method in analysis of aqueous reference solution after dissolution of the sorbate in HNO3 (1:1).


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