The authors proposed an X-ray phase analysis (XPA) approach, which makes it possible with improved statistics to identify and quantitatively estimate the ultrafine grained solids phase composition. As a result of a new survey approach, which consists in shooting an averaged diffraction pattern from a series of measurements obtained at different azimuth angles of the sample inclination, it became possible to more accurately estimate the ultrafine grained solid’ weight fraction with a low content. In this paper, we consider the extension of the capabilities the proposed XPA approach and its application for mineral deposits analysis in oilfield equipment’s ferritic-martensit steel. It has been established that the conventional method of measuring x-ray patterns on Cu radiation leads to their fluorescence, in which the present phases’ diffraction reflections are significantly absorbed, as a result of which the x-ray patterns’ interpretation often leads to erroneous results. Based on a theoretical analysis the parameters that make it possible to control the intensity of detected X-ray quanta, ways are shown to obtain optimal x-ray patterns from the point of view the reflections intensity ratio and background radiation. An algorithm for quantitative evaluation phases is shown as a result of refinement the shape and size of crystallites, crystallographic texture, Debye – Waller factor, evolutions of atoms on crystal lattice and their displacements. To assess the accuracy and reliability the obtained data, for the first time the XPA quantitative results were recalculated into oxide forms and compared with the data of x-ray fluorescence spectrometry, which showed their convincing convergence. For additional verification of obtained results, scanning electron microscopy methods were used. The proposed approach makes it possible to obtain extended information about the type and quantitative ratio of phases, which opens up new opportunities for studying the corrosion mechanisms and scaling on oilfield equipment steels.
References
1. Markin A.N., Sukhoverkhov S.V., Brikov A.V., Neftepromyslovaya khimiya: analiticheskie metody (Oilfield chemistry: Analytical methods), Yuzhno-Sakhalinsk: Sakhalin Regional Printing House, 2016, 212 p.
2. Brikov A.V., Markin A.N., Neftepromyslovaya khimiya: prakticheskoe rukovodstvo po bor'be s obrazovaniem soley (Oilfield chemistry: A practical guide to salt control), Moscow: De Libri Publ., 2018, 335 p.
3. Ibragimov N.G. et al., Oslozhneniya v neftedobyche (Complications in oil production): edited by Ibragimov N.G., Ishemguzhin E.I., Ufa : Monografiya Publ., 2003, 302 p.
4. Puchina G.R., Ragulin V.V., Voloshin A.I. et al., Neftepromyslovaya khimiya. Sovremennye metody bor'by s soleotlozheniyami v dobyche nefti (Oilfield chemistry. Modern methods of scaling control in oil production), Ufa: Bashkirskaya entsiklopediya Publ., 2020, 72 p.
5. Volkov M.G., Presnyakov A.Yu., Klyushin I.G. et al., Monitoring and management the abnormal well stocks based on the Information System Mekhfond of Rosneft Oil Company (In Russ.), Neftyanoe khozyaystvo = Oil Industry, 2021, no. 2, pp. 90–94, https://doi.org/10.24887/0028-2448-2021-2-90-94
6. Sitdikov V.D., Nikolaev A.A., Kolbasenko E.A. et al., A new approach to the analysis of clay minerals in rocks by X-Ray scattering (In Russ.), Neftegazovoe delo, 2021, V. 19, no. 5, pp. 75–83, https://doi.org/10.17122/ngdelo-2021-5-75-83
7. Gorelik S.S, Skakov Yu.A., Rastorguev L.N., Rentgenograficheskiy i elektronno-opticheskiy analiz (X-ray and electron-optical analysis), Moscow: Publ. of MISIS, 1994, 328 p.
8. Nakhmanson M.S., Feklichev V.G., Diagnostika sostava materialov rentgendifraktsionnymi i spektral'nymi metodami (Diagnostics of the composition of materials by X-ray diffraction and spectral methods), Leningrad: Mashinostroenie Publ., 1990, 356 p.
9. Sitdikov V.D., Nikolaev A.A., Ivanov G.V. et al., Microstructure and crystallographic structure of ferritic steel subjected to stress-corrosion cracking (In Russ.) Pis'ma o materialakh, 2022, V. 12, no. 1, pp. 65–70.
10. Zevin L.S., Kimmel G., Quantitative X-ray diffractometry, Springer Science & Business Media, 2012, 372 p.
11. Sitdikov V.D., Murashkin M.Yu., Valiev R.Z., New X–ray technique to characterize nanoscale precipitates in aged aluminium alloys, J. Mater. Eng. Perform., 2017, V. 26, no. 10, pp. 4732–4737, https://doi.org/10.1007/s11665-017-2915-0
12. Zhou S., Potzger K., Talut G. et al., Using X–ray diffraction to identify precipitates in transition metal doped semiconductors, J. Appl. Phys., 2008, V. 103(7), https://doi.org/10.1063/1.2828710
13. Rietveld H.M., A profile refinement method for nuclear and magnetic structures, J. Appl. Crystallogr., 1969, V. 2, pp. 65–71, https://doi.org/10.1107/S0021889869006558
14. Snellings R., Machiels L., Mertens G., Elsen J., Rietveld refinement strategy for quantitative phase analysis of partially amorphous zeolitized tuffaceous rocks, Geologica Belgica, 2010, V. 13/3, pp. 183–196.
15. Dollase W.A., Correction of intensities for preferred orientation in powder diffractometry: application of the March model, Journal of Applied Crystallography, 1986, V. 19, pp. 267-272, https://doi.org/10.1107/S0021889886089458
16. Para T.A., Sarkar S.K., Challenges in rietveld refinement and structure visualizatio in ceramics, In: Advanced Ceramic Materials, London, United Kingdom: IntechOpen, 2021, 296 р., https://doi.org/10.5772/intechopen.96065n
17. Zeng Z., Lu H., Zhao Y., Qin Y., Analysis of the mineral compositions of swell-shrink claysfrom Guangxi province, China, Clays and Clay Minerals, 2020, V. 68, pp. 161–174, https://doi.org/10.1007/s42860-019-00056-7
