Crystal Structure Investigation of Ferritic 73Fe24Cr2Si0.8Mn0.1Ni Steel for Multi-purpose Structural Material Applications

Microstructural identification of synthesized steel with significant local content has been carried out. Alloy ingot was prepared using a casting technique. The samples were then formed into bulk steel by a machining process. A high resolution powder neutron diffractometer (HRPD) was used as an equipment for characterization. By applying neutron diffraction techniques, a ferritic steel profile can be resulted in as well as ‘minor peaks’ belong to impurities formed in the sample. These impurities can be identified as small amounts of Al2O3 54SiO2, Al4C3, SiC and Cr23C6. Scanning transmission electron microscopy (STEM) combined with energy dispersive X-ray spectroscopy (EDX) confirmed and revealed neutron identified phase distributions. Joint Committee on Powder Diffraction Standards (JCPDS) least square curves calibration can precisely calculate the dhkl parameters of each reflection plane. As a comparison, another sample of alloy ingot was also investigated using neutron diffraction. The pattern was free from crystal impurities. Rietveld refinements provide satisfactory goodness of fits Rwp = 10.42% and reliability factor S = 1.7. This was so-called a ‘real bulky’ sample of a 73Fe24Cr2Si0.8Mn0.1Ni ferritic steel alloy.

73Fe24Cr2Si0.8Mn0.1Ni Steel; Crystal structure; Neutron diffraction; Transmission electron microscope

In summary, there are some ‘impurity’ compounds, as evidenced by the unidentified reflections in the measured neutron diffractogram. The neutron diffraction techniques revealed, in addition to the ferritic steel profile, some minor peaks which belong to impurities formed in the sample. These impurities can be identified as a small amount of Al2O3 54SiO2, Al4C3, SiC, and Cr23C6. Scanning transmission electron microscopy (STEM) combined with energy dispersive X-ray spectroscopy (EDX) analyses confirmed and revealed the neutron identified phase distributions. JCPDS least square curves calibration can precisely calculate the dhkl parameters of each reflection plane of impurities. As a comparison, another specimen taken from the middle of an alloy-ingot was also investigated by neutron diffraction. The pattern was free from crystal impurities. Rietveld refinements give a satisfactory goodness of fit Rwp = 10.42% and reliability factor S = 1.7. This was then called a ‘real bulky’ sample of 73Fe24Cr2Si0.8Mn0.1Ni ferritic steel alloy.

The writers would like to express thanks to the Head of PSTBM and BSBM, Dr. Arbi Dimyati, Dr. Andon Insani, Drs. Agus Hadi Ismoyo, Mr. Imam Wahyono, Mr. Rohmad Salam and Mr. Heri Mugihardjo for their kindness and help. Also, the writers thank to GFE-RWTH Aachen in Germany, and the financial support of DIPA 2015.

Bella, A.M.T., Henderson, C.M.B., 2016. Rietveld Refinement of the Crystal Structures of Rb₂XSi₅O₁₂ (X = Ni, Mn). Crystallographic Communications, Volume 72, pp. 249–252

Burnett, T.L., Kelley, R., Winiarski, B., Contreras, L., Daly, M., Gholinia,, A., Burke, M.G., Withers, P.J., 2016. Large Volume Serial Section Tomography by Xe Plasma FIB Dual Beam Microscopy. Ultramicroscopy, Volume 161, pp. 119–129

Dani, M., Parikin, Iskandar, R., Dimyati, A., 2017. Investigation on Precipitations and Defects of the Fe-24Cr-2Si-0.8Mn Ferritic Super Alloy Steel. Indonesian Materials Science Journals (Jurnal Sains Materi Indonesia), Volume 18(4), pp. 173–178

Dani, M., Untoro P., Putra T.Y.S.P., Parikin, Mayer, J., Dimyati, A., 2015. Transmission Electron Microscopy Characterization of High-temperature Oxidation of Fe-20Cr-5Al Alloy Prepared by Focused Ion Beam Technique. Makara Journal of Technology, Volume 19(2), pp. 85–89

David, S.A. , Siefert, J.A., Feng, Z., 2013. Welding and Weldability of Candidate Ferritic Alloys for Future Advanced Ultra Supercritical Fossil Power Plants. Science and Technology of Welding and Joining, Volume 18(8), pp. 631–651

Effendi, N., Darwinto, T., Ismoyo, A.H., Parikin, 2014. 24-Chromium Ferritic Steel Magnetic Properties. Indonesian Materials Science Journals (Jurnal Sains Materi Indonesia), Volume 15(4), pp. 187–191

Effendi, N., Jahja, A.K., Bandriana, Adi, W.A., 2012. Some Data of Second Sequence non Standard Austentic Ingot A2. Urania, Scientific Journal of Nuclear Fuel Cycle, Volume 18(1), pp. 48–58

Frølich, S., Leemreize, H., Jakus, A., Xiao, X., Shah, R., Birkedal, H., Almer, J.D., Stock, S. R., 2016. Diffraction Tomography and Rietveld Refinement of a Hydroxyapatite Bone Phantom. Journal of Applied Crystallography, Volume 49(1), pp. 103–109

Harjo, S., Kawasaki, T., Gong, W., Aizawa, K., 2016. Dislocation Characteristics in Lath Martensitic Steel by Neutron Diffraction.  Journal of Physics: Conference Series Volume 746, pp. 1–7

Humphreys, C.J., 2013. The Significance of Bragg’s Law in Electron Diffraction and Microscopy, and Bragg’s second law. Foundations of Crystallography, Acta Crystallography, Volume A(69), pp. 45–50

JCPDS (Joint Committee on Powder Diffraction Standards), 2014.  International Centre for Diffraction Data, PCPDFWIN, PDF-2 Powder Diffraction File, Release 2014. Cambridge University Press, USA

Kanthavela, K., Arunkumar, K., Vivek, S., 2014. Investigation of Chill Performance in Steel Casting Process using Response Surface Methodology. Procedia Engineering, Volume 97, pp. 329–337

Kim, H.J., Choi, S.H., Bae, H.B., Lee, T.W., 2012. Transmission Electron Microscopy (TEM) Sample Preparation of Si1–xGex in c-Plane Sapphire Substrate. NASA STI Program, pp.1–29

Kumar, V., Kumari, S., Kumar, P., Kar, M., Kumar, L., 2015. Structural Analysis by Rietveld Method and its Correlation with Optical Propertis of Nanocrystalline Zinc Oxide, Advanced. Materials Letters, Volume 6(2), pp. 139–147

NEA (Nuclear Energy Agency), 2013. Status Report on Structural Materials for Advanced Nuclear Systems, Nuclear Energy Agency Organisation for Economic Co-operation and Development. Available online at http://www.oecd-nea.org/science/pubs/2013/6409-sr-mans.pdf, Accessed on October 27, 2017

Parikin, Bandriyana, Wahyono, I., Ismoyo, A.H., 2013. Non-destructive Residual Stress Analysis around the Weld-joint of Fuel Cladding Materials of ZrNbMoGe Alloys. Atom Indonesia Journals, Volume 39(2), pp. 65–74

Parikin, Ismoyo, A.H., Dimyati, A., 2017. Residual Stress Measurements on the TIG Weld Joint of 57Fe15Cr25Ni Austenitic Steel for Structural Material Applications by Means X- Ray Diffraction Techniques. Makara Journal of Technology, Volume 21(2), pp. 49–57

Parikin, Killen, P., Rafterry, A., 2009. Measurements of Residual Stresses  in  Cold-Rolled 304 Stainless Steel Plates using X-ray Diffraction with Rietveld  Refinement Method. Atom Indonesia Journals, Volume 35(1), pp. 19–36

Pereira, P.F.S., Nogueira, I.C., Longo, E., Nassar, E.J., Rosa, I.L.V., Cavalcante, L.S., 2015. Rietveld Refinement and Optical Properties of SrWO4:Eu3+ Powders Prepared by the Non- hydrolitic Sol-Gel Method. Journal of Rare Earths, Volume 33(2), pp. 113–128

Taban, E., Kaluc, E., Atici, T., Kaplan, E., 2012. 9-12% Cr Steels: Properties and Weldability Aspects, the Situation in Turkish Industry. In: Proceeding of the 2^nd International Conference on WeldingTechnologies and Exhibition. Ankara-Turkey, pp. 203–212

Wahyono, I., Salam, R., Parikin, Dimyati, A., 2015. Characterisation of Microstructures By using SEM and XRD on Corrosion Resistant of SS430 Commercial Steel and F1 non Commercial Steel. In: Prosiding Seminar Nasional XI SDM Teknologi Nuklir (Indonesian National Seminar XI SDM Nuclear Technology), pp.112–117

Woo, W., Huang, E.W., Yeh, J.W., Choo, H., Lee, C., Tu, S.Y., 2015. In-situ Neutron Diffraction Studies on High-temperature Deformation Behavior in a CoCrFeMnNi High Entropy Alloy. Intermetallics, Volume 62, pp. 1–6