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2024 №04 (06) DOI of Article
10.37434/sem2024.04.07
2024 №04 (08)

Electrometallurgy Today 2024 #04
Electrometallurgy Today (Suchasna Elektrometallurgiya), 2024, #4, 51-56 pages

Determination of the content of oxygen, nitrogen, and hydrogen impurities in germanium

R.V. Kozin, O.M. Kalinyuk, A.M. Kibkalo, M.M. Kalinyuk, S.G. Grygorenko

E.O. Paton Electric Welding Institute of the NAS of Ukraine 11 Kazymyr Malevych Str., 03150, Kyiv, Ukraine. E-mail: kosinrv@gmail.com

Abstract
Literature review of the methods of producing polycrystalline and monocrystalline germanium and determination of oxygen, nitrogen, and hydrogen contents in them is given. The main method of determination oxygen content in germanium is IR-spectroscopy, and for determination of hydrogen content it is reduction melting in a flow of carrier gas (nitrogen). Germanium does not react with carbon and gaseous nitrogen under the analysis conditions (temperatures of 750…2500 °C, pressure of gaseous nitrogen of ~1…3 at. %). Only the content of oxygen, dissolved in the matrix of germanium (optically active), can be determined by IR-spectroscopy. It is impossible to determine the content of oxygen bound in GeO2 by this method. Preparation of the sample for this method took ~ 1.5 …2.0 h. Time of analysis was ~ 30 min. Express method of determination oxygen content in germanium by reduction melting in a graphite crucible in a helium flow with preliminary elimination of the influence of surface contamination on the sample was developed: oxygen, dissolved in the matrix of germanium (optically active); oxygen bound in GeO2; oxygen optically active and bound in GeO2, which are determined during analysis of one sample. Sample preparation for this method took ~ 5…10 min. Time of analysis was from 40 to 120 s. Comparison of these methods with IR-spectroscopy is given. Method of determination of hydrogen content in germanium was developed. 19 Ref., 4 Tabl., 5 Fig.
Keywords: determination, germanium, oxygen, hydrogen, nitrogen

Received: 17.05.2024
Received in revised form:02.10.2024
Accepted: 07.11.2024

References

1. Claeys, C., Simoen, E. (2007) Germanium-based technologies. From Materials to Devices.
2. De Gryse, O., Vanmeerbeek, P., Vanhellemont, J., Clauws, P. (2006) Infrared analysis of the precipitated oxide phase in silicon and germanium. J. Physica, B 376-377, 113-116. https://doi.org/10.1016/j.physb.2005.12.030
3. Weber, J., Hiller, M., Lavrov, F.V. (2006) Hydrogen in germanium. Materials Sci. in Semiconductor Processing, 9(4-5), 564-570. https://doi.org/10.1016/j.mssp.2006.08.007
4. Karandashev, V.K., Bezrukov, L.B., Kornoukhov, V.N. et al. (2009) Analysis of specimens of germanium and germanium dioxide by methods of mass-spectrometry and atomic emission. Zh. Analit. Khimii, 64(3), 274-282 [in Russian]. https://doi.org/10.1134/S1061934809030095
5. Pavlyuk, T.O., Filatov, R.A., Gorodishcheva, A.N., Ulturgasheva, A.V. (2015) Influence of annealing on oxygen behavior in germanium single crystals. In: Nanomaterialy i Nanotekhnologii v Aerokosmicheskoi Otrasli, 538-539 [in Russian].
6. Gracheva, M.A., Golubovskaya, N.O. (2015) Study of oxygen behavior in germanium single crystals. Aktualnye Problemy Aviatsii i Kosmonavtiki, 2(11), 72-75 [in Russian].
7. Shimanski, A.F., Pavluk, T.O., Kopytkova, S.A., Gorodishcheva, A.N. (2017) Effect of oxygen dissolved in germanium on defect formation and optical properties of single crystals. In: Proc. of 21st Inter. Sci. Conf. on Reshetnev Reading, 1-5.
8. Podkopaev, O.I., Kulakovskaya, T.V., Shimansky, A.F. et al. (2013) Interaction of gas phase with melt during growing process of germanium single crystals. Zh. Sibirsk. Federal. Unta, Tekhnika i Tekhnologii, 6, 674-679 [in Russian].
9. Krylov, V.A., Chernova, O.Yu. Sozin, A.Yu., Zorin, A.D. (2015) Chromato-mass-spectrometric analysis of high purity germanium. Analitika i Kontrol, 19(1), 45-51 [in Russian].
10. De Gryse, O., Vanhellemont, J., Clauws, P. (2006) Determination of oxide precipitate phase and morphology in silicon and germanium using infrared absorption spectroscopy. Materials Sci. in Semiconductor Processing, 9, 246-251. https://doi.org/10.1016/j.mssp.2006.01.041
11. Hagen, H., Sieverts, A. (1930) Germanium, Indium, Niob, Titan und Wasserstoff. Z. Anorg. und Allgem. Chem., 185, 225-238. https://doi.org/10.1002/zaac.19301850119
12. Lyakishev, N.P., Bannykh, O.A., Rykhlin, L.L. (1996) State diagrams of binary metallic systems: Refer. book in 3 Vol., Vol. 1, Moscow, Mashinostroenie [in Russian].
13. Vasserman, A.M., Kunin, L.L., Surovoj, Yu.N. (1976) Determination of gases in metals. Moscow, Nauka [in Russian].
14. Litvinov, V.V., Svensson, B.G., Murin, L.I. et al. (2006) Determination of interstitial oxygen concentration in germanium by infrared absorption. J. Appl. Physics, 100, O 33525. https://doi.org/10.1063/1.2219987
15. Nazarenko, V.A. (1973) Analytical chemistry of germanium. Moscow, Nauka [in Russian].
16. Kozin, R.V., Kalinyuk, O.M., Kibkalo, A.M. et al. (2024) Analyzing silicon for the content of oxygen, nitrogen and hydrogen impurities. Suchasna Elektrometal., 1, 49-56 [in Ukrainian]. https://doi.org/10.37434/sem2024.01.06
17. Kalinyuk, O.M., Kozin, R.V., Kalinyuk, M.M. et al. (2023) Active and passive preparation of analytical samples of metals for determination of oxygen, nitrogen and hydrogen concentrations in them. Suchasna Elektrometal., 4, 54-60 [in Ukrainian]. https://doi.org/10.37434/sem2023.04.07
18. Standard ASTM F122-70T: Method of Test for Interstitial Atomic Oxygen Content of Germanium by Infrared Absorption.
19. Aleksandrova, G.I., Goncharov, L.A., Iljin, M.A. et al. (1976) Determination of oxygen in germanium. Zavod. Laboratoriya, 42(9), 1079-1081 [in Russian].

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