Manufacturing Technology 2025, 25(3):357-365 | DOI: 10.21062/mft.2025.037

Influence of Surface Preparation on XRD Peak Parameters and Residual Stress Measurements

Pavel Salvetr ORCID...1, Aleksandr Gokhman ORCID...2, Jan Drahokoupil ORCID...3
1 COMTES FHT. Průmyslová 995, 334 41 Dobřany. Czech Republic
2 Department of Physics, South Ukrainian National Pedagogical University (SUNPU). Staroprotfrankivska 26, 65020 Odessa. Ukraine
3 FZU – The Institute of Physics of the Czech Academy of Sciences, Na Slovance 1999/2, Prague 8, 182 21. Czech Republic

X-ray diffraction (XRD) is an analytical technique used to investigate the crystal structure properties of materials. However, the accuracy of XRD measurements can be significantly affected by the sam-ple's surface preparation. This study evaluates the impact of various surface preparation methods on the diffraction peak characteristics, phase composition, and residual stress analysis of two metallic materials: very low alloyed iron-based alloy labelled as pure iron and hardened 54SiCr6 steel. Various final steps of metalographic preparation of the surface for XRD were used, including mechanical grinding with coarse (P120) and fine (P1200) sandpapers, polishing with OPS colloidal silica, chemical etching in hot hydrochloric acid, and electrolytic etching. The results show that surface conditions influence more on the full width at half maximum (FWHM) than the intensity of diffraction peaks. Furthermore, the annealed pure iron sample (with low hardness) exhibited a more pronounced sensi-tivity to surface preparation compared to hardened 54SiCr6 steel, with its martensitic microstructure. Residual stress analysis using the sin²ψ method further revealed that mechanical grinding induces substantial compressive residual stress while polishing and etching methods produce nearly neutral or slightly tensile residual stresses. These findings highlight the importance of consistent and appropri-ate surface preparation methods for reliable XRD analysis.

Keywords: XRD diffraction, Peak characteristics, Residual stress, Surface preparation, Dislocation density
Grants and funding:

The development of this paper was financed by the institutional support for the long-term conceptual development of the research organization. Decision No. 3/2023 of the Ministry of Industry and Trade of the Czech Republic

Received: February 25, 2025; Revised: May 6, 2025; Accepted: May 23, 2025; Prepublished online: June 11, 2025; Published: July 4, 2025  Show citation

ACS AIP APA ASA Harvard Chicago IEEE ISO690 MLA NLM Turabian Vancouver
Salvetr P, Gokhman A, Drahokoupil J. Influence of Surface Preparation on XRD Peak Parameters and Residual Stress Measurements. Manufacturing Technology. 2025;25(3):357-365. doi: 10.21062/mft.2025.037.
Share...
Download citation
  • BibTeX (.bib)
  • Bookends (.ris)
  • EasyBib (.ris)
  • EndNote (.enw)
  • EndNote 8 (.xml)
  • ISI WoS (.isi)
  • Medlars (.medlars)
  • Mendeley (.ris)
  • MODS (.xml)
  • Papers (.ris)
  • RefWorks (.txt)
  • RefManager (.ris)
  • RIS (.ris)
  • MS Word (.xml)
  • Zotero (.ris)
    • Open full article

    References

    1. KRATOCHVÍL, B., HUŠÁK, M., BRYNDA, J., SEDLÁČEK, J. (2008). What can the current X-ray structure analysis offer?. In: Chemicke Listy, Vol. 102, No. 10, pp. 889-901. ISSN 1213-7103
    2. KRATOCHVÍL, B., HUŠÁK, M., KOROTKOVA, E.I., JEGOROV A. (2016). The importance of x-ray crystal structure determinations for pharmacy. In: Chemicke Listy, Vol. 110, No. 1, pp. 40-47. ISSN 1213-7103
    3. KRAUS, I., GANEV, N. (2004). Technické aplikace difrakční analýzy, Vyd. 1, Publisher: CTU, Prague. ISBN 9788001030998
    4. LUŠTINEC, J., OČENÁŠEK, V. (2019). Residual Stresses and Cracks in Forgings of Heat-treatable Aluminium Alloys. In: Manufacturing Technology, Vol. 19, No. 4, pp. 637-643. ISSN 1213-2489 Go to original source...
    5. BLATNICKÁ, M., ŠAJGALÍK, M., SÁGA, M., BLATNICKÝ, M. (2018). Comparison of Residual Stress in High Strength Steel Sample before and after Laser Welding. In: Manufacturing Technology, Vol. 18, No. 3, pp. 369-371. ISSN 1213-2489 Go to original source...
    6. ANASIEWICZ, K., JÓZWIK, J., LELEŃ, M., PIEŚKO, P., LEGUTKO, S., TOMCZAK, J., PATER, Z., BULZAK, T. (2024). Identification of Internal Defects in Forged Shafts by Measurement of Residual Stresses Using X-Ray Method. In: Manufacturing Technology, Vol. 24, No. 5, pp. 711-720. ISSN 1213-2489 Go to original source...
    7. DRAHOKOUPIL, J. (2011). INTERPRETATION OF DIFFRACTION PROFILES, Doctoral thesis, Czech Technical University in Prague, 2011.
    8. SHINTANI, T., MURATA, Y. (2011). Evaluation of the dislocation density and dislocation character in cold rolled Type 304 steel determined by profile analysis of X-ray diffraction, In: Acta Materialia, Vol. 59, No. 11, pp. 4314-4322. ISSN 1359-6454 Go to original source...
    9. WEI, Y., YU, X., HAO, T., YANG, S., SU, Y., ZHAO, W. (2024). Effect of the Surface Carbon Content on Microstructure and Deformation of M50 Steel. In: Journal of Materials Engineering and Performance, Vol. 33, No. 15, pp. 7990-7997. ISSN 1059-9495 Go to original source...
    10. MUIRURI, A., MARINGA, M., DU PREEZ, W. (2020). Evaluation of Dislocation Densities in Various Micro-structures of Additively Manufactured Ti6Al4V (Eli) by the Method of X-ray Diffraction. In: Materials, Vol. 13, No. 23, pp. 5355. ISSN 1996-1944 Go to original source...
    11. CHEN, Y., SUN, H., LI, Z., WU, Y., XIAO, Y., CHEN, Z., ZHONG, S., WANG, H. (2020). Strategy of Residual Stress Determination on Selective Laser Melted Al Alloy Using XRD. In: Materials, Vol. 13, No. 2, pp. 451. ISSN 1996-1944 Go to original source...
    12. BARROW, A.T.W., KANG, J.-H., RIVERA-DÍAZ-DEL-CASTILLO, P.E.J. (2012). The ϵ→η→θ transition in 100Cr6 and its effect on mechanical properties. In: Acta Materialia. Vol. 60, No. 6-7, pp. 2805-2815. ISSN 1359-6454 Go to original source...
    13. PAGLIARO, P., PRIME, M.B., ROBINSON, J.S., CLAUSEN, B., SWENSON, H., STEINZIG, M., ZUCCARELLO, B. (2011). Measuring Inaccessible Residual Stresses Using Multiple Methods and Superposition, In: Experimental Mechanics. Vol. 51, No. 7, pp. 1123-1134. ISSN 0014-4851 Go to original source...
    14. KLEMM-TOOLE, J., BENZ, J., VIEIRA, I., CLARKE, A.J., THOMPSON, S.W., FINDLEY, K.O. (2020. Strengthening mechanisms influenced by silicon content in high temperature tempered martensite and bainite. In: Materials Science and Engineering: A, Vol. 786, pp. 139419. ISSN 0921-5093 Go to original source...
    15. YAZDANMEHR, A., JAHED, H. (2020) On the Surface Residual Stress Measurement in Magnesium Alloys Using X-Ray Diffraction. In: Materials, Vol. 13, No. 22, pp. 5190. ISSN 1996-1944 Go to original source...
    16. LUKAS, M., MAYER, M., STARK, A., FRIESSNEGGER, B., HÖNIGMANN, T., GALLER, M., RESSEL, G. (2022). Influence of Tempering on Macro and Micro-Residual Stresses and Yield Stress of Ferritic-Pearlitic Drawn, Coiled, and Straightened Wires. In: Metallurgical and Materials Transactions A, Vol. 53, No. 11, pp. 3977-3985. ISSN 1073-5623 Go to original source...
    17. E468-18; Practice for X-RAY Determination of Retained Austenite in Steel with Near Random Crystallographic Orientation. ASTM International: West Conshohocken, PA, USA, 2013.
    18. RIETVELD, H.M. (1969). A profile refinement method for nuclear and magnetic structures. In: Journal of Applied Crystallography, Vol. 2, No. 2, pp. 65-71. ISSN 0021-8898 Go to original source...
    19. UNGÁR, T., BORBÉLY, A. (1996). The effect of dislocation contrast on x-ray line broadening: A new approach to line profile analysis. In: Applied Physics Letters, Vol. 69, No. 21, pp. 3173-3175. ISSN 0003-6951 Go to original source...
    20. UNGÁR, T., DRAGOMIR, I., RÉVÉSZ, Á., BORBÉLY, A. (1999). The contrast factors of dislocations in cubic crystals: the dislocation model of strain anisotropy in practice. In: Journal of Applied Crystallography. Vol. 32, No. 5, pp. 992-1002. ISSN 0021-8898 Go to original source...
    21. AMANOV, A., YEO, I.K., JEONG, S.H. (2025). Advanced post-processing of Ti-6Al-4V alloy fabricated by selective laser melting: A study of laser shock peening and ultrasonic nanocrystal surface modification. In: Journal of Materials Research and Technology, Vol. 35, pp. 4020-4031. ISSN 2238-7854 Go to original source...
    22. KUMAR, S., SINGH, S.B. (2023). Quantification of Retained Austenite in Low-Carbon Steels. In: Metal-lurgi-cal and Materials Transactions A, Vol. 54, No. 11, pp. 4283-4294. ISSN 1073-5623 Go to original source...

    This is an open access article distributed under the terms of the Attribution-NonCommercial 4.0 International License (CC BY-NC 4.0), which permits non-comercial use, distribution, and reproduction in any medium, provided the original publication is properly cited. No use, distribution or reproduction is permitted which does not comply with these terms.


    Return to the content