Journal of Materials Science

, Volume 52, Issue 19, pp 11643–11658 | Cite as

Quantitative phase fraction analysis of steel combined with texture analysis using time-of-flight neutron diffraction

  • Yusuke Onuki
  • Akinori Hoshikawa
  • Shigeo Sato
  • Toru Ishigaki
  • Toshiro Tomida


The accuracy of the phase fraction determined by time-of-flight neutron diffraction measurement at iMATERIA was verified by preparing model samples consisting of laminations of ferritic and austenitic stainless-steel sheets. Rietveld texture analysis, based on 132 diffractograms, was employed as the analysis method. The analyzed volume fractions of austenite agree with the prepared fractions (0.61–49.3 vol%) with a maximum error of only 5%, relative to the prepared fractions. This is due to the excellent fitting quality of the multi-diffractogram-based Rietveld refinement with consideration given to the textures of both the major and minor phases. Although the quality of the texture analysis for the austenite phase becomes poor, at <5 vol%, the consideration of the textures improves the accuracy of the phase fraction determination. Also described is how the textures affect the phase fractions, as determined by the conventional diffraction method. It is clearly shown that texture cannot be ignored in phase fraction analysis and, in turn, a reasonable consideration of the texture realizes precision in the analysis.


  1. 1.
    Ardell J (1985) Precipitation hardening. Metall Trans A 16:2131–2165CrossRefGoogle Scholar
  2. 2.
    Matsumura O, Sakuma Y, Takechi H (1992) Retained austenite in 0.4 C-Si-1.2 Mn steel sheet intercritically heated and austempered. ISIJ Int 32:1014–1020CrossRefGoogle Scholar
  3. 3.
    Louzguine DV, Kato H, Louzguina LV, Inoue A (2004) High-strength binary Ti–Fe bulk alloys with enhanced ductility. J Mater Res 19:3600–3606CrossRefGoogle Scholar
  4. 4.
    Ogawa Y, Ando D, Sutou Y, Koike J (2016) A lightweight shape-memory magnesium alloy. Science 353:368–370CrossRefGoogle Scholar
  5. 5.
    Zhao L, Van Dijk NH, Brück E, Sietsma J, Van der Zwaag S (2001) Magnetic and X-ray diffraction measurements for the determination of retained austenite in TRIP steels. Mater Sci Eng A 313:145–152CrossRefGoogle Scholar
  6. 6.
    Chen SC, Tomota Y, Shiota Y, Toomine Y, Kamiyama T (2006) Measurements of volume fraction and carbon concentration of the retained austenite by neutron diffraction. Tetsu-to-Hagané 92:557–561CrossRefGoogle Scholar
  7. 7.
    Eskandari M, Zarei-Hanzaki A, Mohtadi-Bonab MA, Onuki Y, Basu R, Asghari A, Szpunar JA (2016) Grain-orientation-dependent of γ–ε–α′ transformation and twinning in a super-high-strength, high ductility austenitic Mn-steel. Mater Sci Eng A 674:514–528CrossRefGoogle Scholar
  8. 8.
    Jacques PJ, Allain S, Bouaziz O, De A, Gourgues A-F, Hance BM, Houbaert Y, Huang J, Iza-Mendia A, Kruger SE, Radu M, Samek L, Speer J, Zhao L, van der Zwaag S (2009) On measurement of retained austenite in multiphase TRIP steels—results of blind round robin test involving six different techniques. Mater Sci Technol 25:567–574CrossRefGoogle Scholar
  9. 9.
    Wilson AW, Madison JD, Spanos G (2001) Determining phase volume fraction in steels by electron backscattered diffraction. Scr Mater 45:1335–1340CrossRefGoogle Scholar
  10. 10.
    Scarlett NVY, Madsen IC, Cranswick LMD, Lwin T, Groleau E, Stephenson G, Aylmoree M, Agron-Olshina N (2002) Outcomes of the international union of crystallography commission on powder diffraction round robin on quantitative phase analysis: samples 2, 3, 4, synthetic bauxite, natural granodiorite and pharmaceuticals. J Appl Crystallogr 35:383–400CrossRefGoogle Scholar
  11. 11.
    Toraya H (2000) Estimation of statistical uncertainties in quantitative phase analysis using the Rietveld method and the whole-powder-pattern decomposition method. J Appl Crystallogr 33:1324–1328CrossRefGoogle Scholar
  12. 12.
    Blondé R, Jimenez-Melero E, Zhao L, Wright JP, Brück E, Van der Zwaag S, Van Dijk NH (2012) High-energy X-ray diffraction study on the temperature-dependent mechanical stability of retained austenite in low-alloyed TRIP steels. Acta Mater 60:565–577CrossRefGoogle Scholar
  13. 13.
    De Meyer M, Vanderschueren D, De Blauwe K, De Cooman BC (1999) The characterization of retained austenite in TRIP steels by X-ray diffraction. In: 41st Mechanical working and steel processing conference proceedings, pp. 483–492Google Scholar
  14. 14.
    De AK, Murdock DC, Mataya MC, Speer JG, Matlock DK (2004) Quantitative measurement of deformation-induced martensite in 304 stainless steel by X-ray diffraction. Scr Mater 50:1445–1449CrossRefGoogle Scholar
  15. 15.
    ASTM E975-13 (2013) Standard practice for X-ray determination of retained austenite in steel with near random crystallographic orientation. ASTM International, West Conshohocken.
  16. 16.
    Matthies S, Lutteroti L, Wenk HR (1997) Advances in texture analysis from diffraction diffractograms. J Appl Crystallogr 30:31–42CrossRefGoogle Scholar
  17. 17.
    Wenk HR, Lutterotti L, Vogel S (2003) Texture analysis with the new HIPPO TOF diffractometer. Nucl Instrum Methods Phys Res Sect A 515:575–588CrossRefGoogle Scholar
  18. 18.
    Kockelmann W, Chapon LC, Radaelli PG (2006) Neutron texture analysis on GEM at ISIS. Phys B 385:639–643CrossRefGoogle Scholar
  19. 19.
    Keppler R, Ullemeyer K, Behrmann JH, Stipp M (2014) Potential of full pattern fit methods for the texture analysis of geological materials: implications from texture measurements at the recently upgraded neutron time-of-flight diffractometer SKAT. J Appl Crystallogr 47:1520–1534CrossRefGoogle Scholar
  20. 20.
    Ishigaki T, Hoshikawa A, Yonemura M, Morishima T, Kamiyama T, Oishi R, Aizawa K, Sakuma T, Tomota Y, Arai M, Hayashi M, Ebata K, Takano Y, Komatsuzaki K, Asano H, Takano Y, Kasao T (2009) IBARAKI materials design diffractometer (iMATERIA)—versatile neutron diffractometer at J-PARC. Nucl Instrum Methods Phys Res Sect A 600:189–191CrossRefGoogle Scholar
  21. 21.
    Onuki Y, Hoshikawa A, Sato S, Xu P, Ishigaki T, Saito Y, Hayashi M (2016) Rapid measurement scheme for texture in cubic metallic materials using time-of-flight neutron diffraction at iMATERIA. J Appl Crystallogr 49:1579–1584CrossRefGoogle Scholar
  22. 22.
    Onuki Y, Hoshikawa A, Sato S, Ishigaki T (2017) Rapid measurement of texture of metals by time-of-flight neutron diffraction at iMATERIA and its applications. Mater Sci Forum 879:1426–1430CrossRefGoogle Scholar
  23. 23.
    Lutterotti L, Chateigner D, Ferrari S, Ricote J (2004) Texture, residual stress and structural analysis of thin films using a combined X-ray analysis. Thin Solid Films 450:34–41CrossRefGoogle Scholar
  24. 24.
    Young RA (1993) The rietveld method. Oxford University Press, OxfordGoogle Scholar
  25. 25.
    Sato H, Kamiyama T, Kiyanagi Y (2011) A Rietveld-type analysis code for pulsed neutron Bragg-edge transmission imaging and quantitative evaluation of texture and microstructure of a welded α-iron plate. Mater Trans 52:1294–1302CrossRefGoogle Scholar
  26. 26.
    Shull CG, Wollan EO, Koehler WC (1951) Neutron scattering and polarization by ferromagnetic materials. Phys Rev 84:912–921CrossRefGoogle Scholar
  27. 27.
    Toby BH (2006) R factors in Rietveld analyses: how good is good enough? Powder Diffr 21:67–70CrossRefGoogle Scholar
  28. 28.
    Xie Y, Lutterotti L, Wenk HR, Kovacs F (2004) Texture analysis of ancient coins with TOF neutron diffraction. J Mater Sci 39:3329–3337. doi:10.1023/B:JMSC.0000026933.28906.19 CrossRefGoogle Scholar
  29. 29.
    Dollase WA (1986) Correction of intensities for preferred orientation in powder diffractometry: application of the March model. J Appl Crystallogr 19:267–272CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media, LLC 2017

Authors and Affiliations

  1. 1.Frontier Research Center for Applied Atomic SciencesIbaraki UniversityTokaiJapan
  2. 2.Graduate School of Science and EngineeringIbaraki UniversityHitachiJapan
  3. 3.Ibaraki Prefectural GovernmentTokaiJapan

Personalised recommendations