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Preparation of Isotopically Enriched Polycrystalline Germanium via Monogermane Pyrolysis

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Inorganic Materials Aims and scope

Abstract—

High-purity isotopically enriched germanium has been prepared by a hydride method, and the main factors capable of reducing the germanium yield in the monogermane pyrolysis process have been identified. To raise the germanium yield, we have optimized pyrolysis conditions in a laboratory-scale flow apparatus. At a monogermane flow rate at the reactor inlet of 30 mL/min, the optimal monogermane decomposition temperature is 420–450°C. Such conditions ensure a decomposition rate of ~6 g/h and a high product yield and make it possible to obtain most of the germanium in polycrystalline form. Using isotopically enriched monogermane pyrolysis, we have obtained high-purity isotopically enriched germanium samples in the form of polycrystalline ingots with a yield above 95%. The ingots are n-type and range in resistivity from 25 to 50 Ω cm. The content of regulated impurities in the 72Ge-,73Ge-, 74Ge-, and 76Ge-enriched germanium ingots thus prepared does not exceed 0.01 to 1 ppm by weight.

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REFERENCES

  1. Cardona, M. and Thewalt, M.L.W., Isotope effects on the optical spectra of semiconductors, Rev. Mod. Phys., 2005, vol. 77, no. 4, pp. 1173–1224. https://doi.org/10.1103/RevModPhys.77.1173

    Article  CAS  Google Scholar 

  2. Plekhanov, V.G., Isotope-based material science, Univers. J. Mater. Sci., 2013, vol. 1, no. 2, pp. 87–147. https://doi.org/10.13189/ujms.2013.010212

    Article  Google Scholar 

  3. Ushakov, O.S., Kalashnikov, A.L., Matyukha, V.A., et al., RF Patent 2 280 616, 2004.

  4. Sennikov, P.G., Golubev, S.V., Shashkin, V.I., et al., RF Patent 2 483 130, 2011.

  5. Sennikov, P.G., Kornev, R.A., Mochalov, L.A., and Golubev, S.V., PECVD preparation of silicon and germanium with different isotopic composition via their tetrafluorides, J. Phys.: Conf. Ser., 2014, vol. 514, paper 012 002. https://doi.org/10.1088/1742-6596/514/1/012002

  6. Aref'ev, D.G., Bulanov, A.D., Vasin, S.A., et al., RF Patent 2 412 747, 2009.

  7. Churbanov, M.F., Bulanov, A.D., Gavva, V.A., et al., RF Patent 2 641 126, 2016.

  8. Aref’ev, D.G., Vasin, S.A., Dolgov, S.V., Zyryanov, S.M., Lutskii, V.A., Skorynin, G.M., Timofeev, M.G., Sharin, G.A., Bulanov, A.D., and Churbanov, M.F., Application of monogermane in germanium isotope separation in gas centrifuges, Perspekt. Mater., 2010, no. 8 (special issue), pp. 19–24.

  9. Potapov, A.M., Kurganova, A.E., Bulanov, A.D., et al., Isotope analysis of 72GeH4, 73GeH4, 74GeH4, and 76GeH4 monogermanes by inductively-coupled plasma high-resolution mass spectrometry (ICP-MS), J. Anal. Chem., 2016, vol. 71, no. 7, pp. 667–675.

    Article  CAS  Google Scholar 

  10. Krylov, V.A., Chernova, O.Yu., Sozin, A.Yu., and Zorin, A.D., Gas chromatography/mass spectrometry analysis of high-purity germane, Anal. Kontrol, 2015, vol. 19, no. 1, pp. 45–51. https://doi.org/10.15826/analitika.2015.19.1.010

    Article  Google Scholar 

  11. Sozin, A.Yu., Bulanov, A.D., Churbanov, M.F., Chernova, O.Yu., Sorochkina, T.G., and Nushtaeva, L.B., Impurity composition of high-purity isotopically enriched monosilane and monogermane, Inorg. Mater., 2017, vol. 53, no. 1, pp. 27–34.

    Article  CAS  Google Scholar 

  12. Devyatykh, G.G. and Frolov, I.A., Kinetics of the thermal decomposition of monogermane, Zh. Neorg. Khim., 1966, vol. 11, no. 4, pp. 708–713.

    CAS  Google Scholar 

  13. Newman, C.G., Dzaronski, L., Ring, M.A., and O’Neal, H., Kinetics and mechanism of the germane decomposition, Int. J. Chem. Kinet., 1980, vol. 12, no. 9, pp. 661–670.

    Article  CAS  Google Scholar 

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ACKNOWLEDGMENTS

We are grateful to A.Yu. Sozin and A.M. Potapov for performing the chemical and isotope analyses of the isotopically enriched monogermane and germanium.

Funding

This work was supported by the Russian Federation Ministry of Science and Higher Education, state research target for the Devyatykh Institute of Chemistry of High-Purity Substances, Russian Academy of Sciences; theme no. 0095-2019-0008.

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Correspondence to V. A. Lipskiy.

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Translated by O. Tsarev

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Lipskiy, V.A., Gavva, V.A. & Bulanov, A.D. Preparation of Isotopically Enriched Polycrystalline Germanium via Monogermane Pyrolysis. Inorg Mater 56, 223–228 (2020). https://doi.org/10.1134/S0020168520020107

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  • DOI: https://doi.org/10.1134/S0020168520020107

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