LLC Gipronickel Institute, Saint Petersburg, Russia

Yu. А. Savinova, Senior Researcher of the Laboratory of Pyrometallurgy, e-mail: SavinovaYuA@nornik.ru
О. S. Novozhilova, Junior Researcher of the Laboratory of Pyrometallurgy, e-mail: NovozhilovaOS@nornik.ru
R. А. Pakhomov, Senior Researcher of the Laboratory of Pyrometallurgy, e-mail: PakhomovRA@nornik.ru

LLC Tescan, Saint Petersburg, Russia

А. А. Kudryavtsev, Head of the Research Department, e-mail: kudryavtsev.andrey@tescan.ru

As the scientific research practice of the Gipronickel Institute in the field of studying products of the metallurgical industry shows, the most informative methods of solid matter analysis are scanning electron microscopy and X-ray spectral microanalysis. These methods are local and allow us to obtain comprehensive information not only about the composition and structure of the material as a whole, but also about its individual components with a size of less than 1 micron. The detection limit of the elemental analysis depends on the type of detector used. When using the most common energy dispersion detector in analytical practice, the limit is about 0.1% (wt.). Unfortunately, this level of sensitivity may not be sufficient (for example, analysis of waste slags and refined products). The Institute’s analytical base is based on the most highly informative equipment. The analysis of trace amounts is carried out on a complex equipped with a detector with a wavelength dispersion of X-ray photons with an exceptionally low detection limit — up to thousandths of a mass percentage. The additional equipment of the electron microscope with an ionic column makes it possible to study the fine morphology of structures that collapse when using traditional mechanical sample preparation. The article shows the indispensable role of local research methods based on specific examples of the work carried out by the Gipronickel Institute to reduce the loss of non-ferrous metals with waste slag, to develop new refining technologies, to select refractories for lining autogenic furnaces and to develop technology for dearsenization of roasting dusts.
The authors express their gratitude and honor the memory of the Doctor of Technical Sciences Lyubov Nikolaevna Ertseva, a unique specialist and mentor.

1. Goldstein J. I., Newbury D. E., Michael J. R., Ritchie N. W. M. et al. Scanning electron microscopy and X-Ray microanalysis. 4^th Edition. Springer, 2018. 550 p.
2. Reichelt R. Scanning electron microscopy. Science of microscopy. Edited by P. W. Hawkes, J. С. H. Spence. Springer Science+Business Media, LLC, 2007. pp. 133–272.
3. Krishtal M. M., Yasnikov I. S., Polunin V. I., Filatov A. M., Ulyaninkov A. G. Scanning electron microscopy and X-ray spectral microanalysis in practical application examples. Мoscow : Tekhnosfera, 2009. 208 p.
4. Ertseva L. N. The experience of scanning electron microscopy and electrone probe microanalysis use for the purpose of non–ferrous materials study. Tsvetnye Metally. 2011. No. 8-9. pp. 86–91.
5. Brandon D., Kaplan U. Microstructure of materials. Research and control methods. Мoscow : Tekhnosfera, 2004. 377 p.
6. Savinova Yu. A., Rumyancev D. V., Mishina O. Yu., Bannikova S. A., Somov P. A. Study of the material composition and morphology of finely dispersed metallurgical dusts by scanning electron-ion microscopy and X-ray spectral microanalysis. Proceedings of the XXVIII Russian Conference on Electron Microscopy. 5–10 September 2020, Chernogolovka. pp. 110–111.
7. Gao Jinghong, Su Weiguang, Wang Xin, Song Xudong et al. Corrosion and degradation mechanisms of high chromia refractory bricks in an entrained-flow gasifier: experimental and numerical analysis. Journal of Materials Research and Technology. 2023. Vol. 24. pp. 8754–8765.
8. Malfliet Annelies, Mazzon Antonio, Otegbeye Oluwabukunmi Omotola, Qiu Zilong et al. Impact of antioxidants in MgO – C refractory on steel cleanliness and refractory degradation. Open Ceramics. 2023. Vol. 14. 100352.
9. Wagri Naresh Kumar, Carlborg Markus, Eriksson Matias, Ma Charlie et al. High temperature interactions between coal ash and MgO-based refractories in lime kiln conditions. Fuel. 2023. Vol. 342. 127711.
10. Lastochkina M. A., Rumyancev D. V., Popov V. A., Savinova Yu. A. On the roasting of platinum-containing copper sludge in the context of subsequent hydrometallurgical processing of cinder. Non-ferrous metals and minerals, 2018 : Proceedings of the Tenth International Congress. pp. 1304–1313.
11. Devochkin A. I. et al. Atlas of mineral raw materials, technological industrial products and marketable products of PJSC MMC Norilsk Nickel. Saint Petersburg : Politekh-Press, 2021. 398 p.
12. Vanyukov A. V., Zaicev V. Ya. Slags and matte of non-ferrous metallurgy. Мoscow : Metallurgiya, 1969. 408 p.
13. Ampilogov V. N., Galancev V. N., Vostrikov G. V., Rusakov M. R. et al. The method of slag depletion. Patent RF, No. 2061072. Applied: 08.07.1991. Published: 27.05.1996.
14. Fomichev V. B. Study and development of technology for depletion of slags containing nickel, cobalt and copper using reducing gases: abstr. thesis. … of Candidate of Technical Sciences. Saint Petersburg, 2003. 23 p.