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Characterization of Dual-Phase Steel Microstructure by Combined Submicrometer EBSD and EPMA Carbon Measurements

Published online by Cambridge University Press:  07 June 2013

Philippe T. Pinard ,
Alexander Schwedt ,
Ali Ramazani ,
Ulrich Prahl  and
Silvia Richter
Philippe T. Pinard*
Affiliation:
Central Facility for Electron Microscopy, RWTH Aachen University, Aachen 52074, Germany
Alexander Schwedt
Affiliation:
Central Facility for Electron Microscopy, RWTH Aachen University, Aachen 52074, Germany
Ali Ramazani
Affiliation:
Department of Ferrous Metallurgy, RWTH Aachen University, Aachen 52072, Germany
Ulrich Prahl
Affiliation:
Department of Ferrous Metallurgy, RWTH Aachen University, Aachen 52072, Germany
Silvia Richter
Affiliation:
Central Facility for Electron Microscopy, RWTH Aachen University, Aachen 52074, Germany
*
*Corresponding author. E-mail: [email protected]
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Abstract

Electron backscatter diffraction (EBSD) and electron probe microanalysis (EPMA) measurements are combined to characterize an industrial produced dual-phase steel containing some bainite fraction. High-resolution carbon mappings acquired on a field emission electron microprobe are utilized to validate and improve the identification of the constituents (ferrite, martensite, and bainite) performed by EBSD using the image quality and kernel average misorientation. The combination eliminates the ambiguity between the identification of bainite and transformation-induced dislocation zones, encountered if only the kernel average misorientation is considered. The detection of carbon in high misorientation regions confirms the presence of bainite. These results are corroborated by secondary electron images after nital etching. Limitations of this combined method due to differences between the spatial resolution of EBSD and EPMA are assessed. Moreover, a quantification procedure adapted to carbon analysis is presented and used to measure the carbon concentration in martensite and bainite on a submicrometer scale. From measurements on reference materials, this method gives an accuracy of 0.02 wt% C and a precision better than 0.05 wt% C despite unavoidable effects of hydrocarbon contamination.

Keywords

electron probe microanalysiselectron backscatter diffractiondual-phase steelbainitecarbon quantificationspatial resolution
Type
Materials Applications
Information
Microscopy and Microanalysis , Volume 19 , Issue 4 , August 2013 , pp. 996 - 1006
Copyright
Copyright © Microscopy Society of America 2013 

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References

Amman, M., Sleight, J.W., Lombardi, D.R., Welser, R.E., Deshpande, M.R., Reed, M.A. & Guido, L.J. (1996). Atomic force microscopy study of electron beam written contamination structures. J Vac Sci Technol, B 14, 54–62.Google Scholar
Angeli, J., Elisabeth, F., Panholzer, M. & Kneissl, A.C. (2006). Etching techniques for characterizing the phases of low-alloy dual-phase and TRIP steels. Prakt Metallogr 43, 489–504.Google Scholar
Bastin, G.F. & Heijligers, H.J.M. (1990). Quantitative electron probe microanalysis of carbon in binary carbides. Third and extended revision. Technical Report. Eindhoven, The Netherlands: Eindhoven University of Technology. Google Scholar
Bleck, W. & Gerdemann, F. (2011). Improved mechanical properties by control of bainite transformation. Mater Manuf Processes 26, 43–50.Google Scholar
Caballero, F., Miller, M., Clarke, A. & Garcia-Mateo, C. (2010). Examination of carbon partitioning into austenite during tempering of bainite. Scr Mater 63, 442–445.CrossRefGoogle Scholar
Cheng, L., Böttger, A., de Keijser, T.H. & Mittemeijer, E. (1990). Lattice parameters of iron-carbon and iron-nitrogen. Scr Metall Mater 24, 509–514.Google Scholar
Deal, A., Hooghan, T. & Eades, A. (2008). Energy-filtered electron backscatter diffraction. Ultramicroscopy 108, 116–125.Google Scholar
Drouin, D., Couture, A.R., Joly, D., Tastet, X., Aimez, V. & Gauvin, R. (2007). CASINO V2.42—A fast and easy-to-use modeling tool for scanning electron microscopy and microanalysis users. Scanning 29, 92–101.Google Scholar
Duerr, J.S. & Ogilvie, R.E. (1972). Electron probe microdetermination of carbon in ferrous alloys. Anal Chem 44, 2361–2367.Google Scholar
Goldstein, J., Newbury, D.E., Joy, D.C., Lyman, C.E., Echlin, P., Lifshin, E., Sawyer, L.C. & Michael, J.R. (2002). Scanning Electron Microscopy and X-Ray Microanalysis, 3rd ed. New York: Springer.Google Scholar
Hielscher, R. & Schaeben, H. (2008). A novel pole figure inversion method: Specification of the MTEX algorithm. J Appl Crystallogr 41, 1024–1037.Google Scholar
Hirsch, P., Kassens, M., Puttmann, M. & Reimer, L. (1994). Contamination in a scanning electron microscope and the influence of specimen cooling. Scanning 16, 101–110.Google Scholar
Humphreys, F.J. (2004). Characterisation of fine-scale microstructures by electron backscatter diffraction (EBSD). Scr Mater 51, 771–776.Google Scholar
ISO16592 (2006). Microbeam Analysis—Electron Probe Microanalysis—Guidelines for Determining the Carbon Content of Steels Using a Calibration Curve Method. Geneva, Switzerland: International Organization for Standardization.Google Scholar
Marinenko, R.B. & Leigh, S. (2010). Uncertainties in electron probe microanalysis. IOP Conf Ser: Mater Sci Eng 7, 012017-1–10.Google Scholar
Miyama, E., Voit, C. & Pohl, M. (2011). The identification of cementite for differentiating between the various types of bainite in modern low-alloyed multi-phase steels. Prakt Metallogr 48, 261–272.CrossRefGoogle Scholar
Petrov, R., Kestens, L., Wasilkowska, A. & Houbaert, Y. (2007). Microstructure and texture of a lightly deformed TRIP-assisted steel characterized by means of the EBSD technique. Mater Sci Eng, A 447, 285–297.CrossRefGoogle Scholar
Pickering, F. (1967). The structure and properties of bainite in steels. In Transformation and Hardenability in Steels, pp. 109–129. Ann Arbor, MI: Climax Molybdenum Company of Michigan.Google Scholar
Ramazani, A., Mukherjee, K., Quade, H., Prahl, U. & Bleck, W. (2012). Correlation between 2D and 3D flow curve modelling of DP steels using a microstructure-based RVE approach. Mater Sci Eng A 560, 128–139.Google Scholar
Reed, S. (1993). Electron Microprobe Analysis, 2nd ed. Cambridge, UK: Cambridge University Press.Google Scholar
Reimer, L. (1998). Scanning Electron Microscopy, 2nd ed. Berlin: Springer.Google Scholar
Robaut, F., Crisci, A., Durand-Charre, M. & Jouanne, D. (2006). Practical aspects of carbon content determination in carburized steels by EPMA. Microsc Microanal 12, 331–334.Google Scholar
Rocha, R., Melo, T., Pereloma, E. & Santos, D. (2005). Microstructural evolution at the initial stages of continuous annealing of cold rolled dual-phase steel. Mater Sci Eng, A 391, 296–304.Google Scholar
Ryde, L. (2006). Application of EBSD to analysis of microstructure in commercial steels. Mater Sci Technol 22, 1297–1306.Google Scholar
Saunders, S., Karduck, P. & Sloof, W.G. (2004). Certified reference materials for micro-analysis of carbon and nitrogen. Microchim Acta 145, 209–213.Google Scholar
Scott, C. & Drillet, J. (2007). A study of the carbon distribution in retained austenite. Scr Mater 56, 489–492.Google Scholar
Silvis-Cividjian, N., Hagen, C., Leunissen, L. & Kruit, P. (2002). The role of secondary electrons in electron-beam-induced-deposition spatial resolution. Microelectron Eng 61–62, 693–699.Google Scholar
Smith, D.A., Fowlkes, J.D. & Rack, P.D. (2008). Simulating the effects of surface diffusion on electron beam induced deposition via a three-dimensional Monte Carlo simulation. Nanotechnology 19, 415704-1–11.Google Scholar
Szabó, P.J. & Szalai, I. (2005). Effect of monotonic and cyclic deformation on the IQ-maps of austenitic stainless steel. Mater Sci Forum 473–474, 267–272.Google Scholar
Takahashi, J., Kawakami, K. & Kobayashi, Y. (2011). Quantitative analysis of carbon content in cementite in steel by atom probe tomography. Ultramicroscopy 111, 1233–1238.Google Scholar
Wendt, M. (1980). The role of contamination layers in electron probe microanalysis. Krist Tech 15, 1367–1375.Google Scholar
Wright, S.I. & Nowell, M.M. (2006). EBSD image quality mapping. Microsc Microanal 12, 72–84.Google Scholar
Wu, J., Wray, P.J., Garcia, C.I., Hua, M. & Deardo, A.J. (2005). Image quality analysis: A new method of characterizing microstructures. ISIJ Int 45, 254–262.Google Scholar
Zaefferer, S. (2007). On the formation mechanisms, spatial resolution and intensity of backscatter Kikuchi patterns. Ultramicroscopy 107, 254–266.CrossRefGoogle ScholarPubMed
Zaefferer, S., Romano, P. & Friedel, F. (2008). EBSD as a tool to identify and quantify bainite and ferrite in low-alloyed Al-TRIP steels. J Microsc 230, 499–508.Google Scholar