Hostname: page-component-586b7cd67f-rcrh6 Total loading time: 0 Render date: 2024-11-30T07:48:55.612Z Has data issue: false hasContentIssue false

Quantitative composition determination by Mössbauer spectroscopy

Published online by Cambridge University Press:  16 December 2019

B. Scott
Affiliation:
Department of Chemistry, Dalhousie University, Halifax, Nova Scotia, CanadaB3H 4R2
C.A.M. Brown
Affiliation:
Department of Chemistry, Dalhousie University, Halifax, Nova Scotia, CanadaB3H 4R2
R.A. Dunlap
Affiliation:
Department of Physics and Atmospheric Science, Dalhousie University, Halifax, Nova Scotia, CanadaB3H 4R2
M.N. Obrovac*
Affiliation:
Department of Chemistry, Dalhousie University, Halifax, Nova Scotia, CanadaB3H 4R2 Department of Physics and Atmospheric Science, Dalhousie University, Halifax, Nova Scotia, CanadaB3H 4R2 Clean Technologies Research Institute, Dalhousie University, Halifax, Nova Scotia, CanadaB3H 4R2
*
Address all correspondence to M.N. Obrovac at [email protected]
Get access

Abstract

Quantitative Fe content determination of powders by Mössbauer spectroscopy is described. In this method, powder samples and internal standard are combined homogeneously in a plastic film ensuring a thin absorber. This method was verified by quantifying the Fe content of a series of samples and independently confirming by inductively coupled plasma optical emission spectroscopic analysis. Additionally, for the first time, Fe contamination in ball-milled Si as a function of milling time was quantified. It was found that Fe contamination increased with time but surprisingly became steady state at 1.12 ± 0.04 at.% Fe after grain size reduction.

Type
Research Letters
Copyright
Copyright © Materials Research Society 2019

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

1.McGraw, J.D., Fleischauer, M.D., Dahn, J.R., and Dunlap, R.A.: Mössbauer effect and X-ray diffraction investigation of Si-Fe thin films. Philos. Mag. 86, 5017 (2006).CrossRefGoogle Scholar
2.Sorescu, M.: A new method for direct determination of the recoilless fraction using a single room-temperature Mössbauer measurement of a two-foil absorber. Mater. Lett. 54, 256 (2002).CrossRefGoogle Scholar
3.Nowik, I., Jacob, I., and Moreh, R.: Mössbauer study of crystallographic and magnetic phase transition, phonon softening, and hyperfine interactions in Zr(AlxFe1−x)2. Phys. Rev. B 47, 723 (1993).CrossRefGoogle Scholar
4.Allwes, M., Mekaoui, M., and Sorescu, M.: Mutual solubility of scandium oxide-hematite magnetic nanocomposites: Mössbauer spectroscopy investigation. Solid State Commun. 261, 46 (2017).CrossRefGoogle Scholar
5.Arredondos, P.I., Barrero, C.A., Garcia, K.E., and Greneche, J.M.: Enhancing the possibilities of 57Fe Mössbauer spectrometry to the study of chemical and physical properties of iron in medicines. Polyhedron 105, 27 (2016).CrossRefGoogle Scholar
6.Hatchard, T.D., Genkin, A., and Obrovac, M.N.: Rapid mechanochemical synthesis of amorphous alloys. AIP Adv. 7, 045201 (2017).CrossRefGoogle Scholar
7.Smith, F.E. and Arsenault, E.A.: Microwave-assisted sample preparation in analytical chemistry. Talanta 43, 1207 (1996).CrossRefGoogle ScholarPubMed
8.Tarascon, J.-M., Gozdz, A.S., Schmutz, C., Shokoohi, F., and Warren, P.C.: Performance of Bellcore's plastic rechargeable Li-ion batteries. Solid State Ionics 86–88, 49 (1996).CrossRefGoogle Scholar
9.Richard, M.N.: A cell for in situ X-ray diffraction based on coin cell hardware and Bellcore plastic electrode technology. J. Electrochem. Soc. 144, 554 (1997).CrossRefGoogle Scholar
10.Obrovac, M.N. and Chevrier, V.L.: Alloy negative electrodes for Li-ion batteries. Chem. Rev. 114, 11444 (2014).CrossRefGoogle ScholarPubMed
11.Gauthier, M., Mazouzi, D., Reyter, D., Lestriez, B., Moreau, P., Guyomard, D., and Roué, L.: A low-cost and high performance ball-milled Si-based negative electrode for high-energy Li-ion batteries. Energy Environ. Sci. 6, 2145 (2013).CrossRefGoogle Scholar
12.Wertheim, G.K., Wernick, J.H., and Buchanan, D.N.E.: Mössbauer effect in Co1−xFezSi. J. Appl. Phys. 37, 3333 (1966).CrossRefGoogle Scholar
13.Desimoni, J. and Sánchez, F.H.: Overview of the Mössbauer results obtained on silicon-rich iron silicide epitaxial phases on Si. Hyperfine Interact. 122, 277 (1999).CrossRefGoogle Scholar
14.Dézsi, I., Fetzer, C., Bujdosó, L., Brötz, J., and Balogh, A.G.: Mechanical alloying of Fe–Si and milling of α- and β-FeSi2 bulk phases. J. Alloys Compd. 508, 51 (2010).CrossRefGoogle Scholar
15.El-Eskandarany, M.S., Aoki, K., and Suzuki, K.: Rod milling for solid-state formation of Al30Ta70 amorphous alloy powder. J. Less Common Met. 167, 113 (1990).CrossRefGoogle Scholar
Supplementary material: File

Scott et al. supplementary material

Tables S1-S2

Download Scott et al. supplementary material(File)
File 43.8 KB