Abstract No. 46 Study of element segregation in steel 20 15 Ann De Vyt, Chris Xhoffer and Jan Scheers ArcelorMittal Global R&D Gent (Belgium) Modern types of high strength steel typically contain a lot of Mn and C. These elements, among others, are known to segregate strongly during solidification. This enriched area cannot be removed once it is present. After rolling, bands of segregation occur. These bands are not just bands with different compositions but also with different microstructures. As such, the mechanical properties vary within the steel. Therefore it is necessary to study the extent of this segregation analytically. Studying segregation zones requires a combination of sensitivity and lateral resolution. Depending on the techniques used, either one or the other, or both can be achieved. S When segregation occurs near the surface and parallel to it, GDOES is a fast and sensitive technique that allows local analysis due to its excellent depth resolution. With Laser Ablation ICP-MS a line scan studying various elements can be acquired across a section of the sample. ICP-MS also gives excellent sensitivity but its lateral resolution may be insufficient. CE TA EPMA and TOF-SIMS combine sensitivity and lateral resolution and provide similar results with an advantage for SIMS regarding the elements in low concentration. Figure 1: After Nital etching of HSLA steels, segregation bands are often observed. Their presence indicates a heterogeneous distribution of specific elements at micro scale. TOF-SIMS elemental maps and line scans across segregation bands (dim.: 300x300μm). Abstract No. 46 CE TA S 20 15 Various examples will be given showing the advantages of the used techniques, compared to each other. 20 15 Study of element segregation in steel TA S CETAS 2015 Session 12 Micro and nano scale characterization • Segregation in materials refers to the enrichment of a material constituent at a free surface or an internal interface of a material • In steel it can be an enrichment or a depletion of certain elements in the central line, at grain boundaries or at the surface • It influences the mechanical properties of the steel CE © ArcelorMittal – All rights reserved for all countries Cannot be disclosed, used, or reproduced without prior written specific authorization of ArcelorMittal CONFIDENTIAL – Privileged Information - ArcelorMittal proprietary information Definition ¾ How can we study it? 1 CE © ArcelorMittal – All rights reserved for all countries Cannot be disclosed, used, or reproduced without prior written specific authorization of ArcelorMittal CONFIDENTIAL – Privileged Information - ArcelorMittal proprietary information Element segregation • EPMA linescan S TA 20 15 © ArcelorMittal – All rights reserved for all countries Cannot be disclosed, used, or reproduced without prior written specific authorization of ArcelorMittal CONFIDENTIAL – Privileged Information - ArcelorMittal proprietary information Element segregation • Centre line segregation • Some elements are known to segregate strongly during solidification • This enriched area cannot be removed once present. • After rolling, bands of segregation occur. • These bands are not just bands with different compositions but also with different microstructures. ¾The mechanical properties vary within the steel. 2 3 CE © ArcelorMittal – All rights reserved for all countries Cannot be disclosed, used, or reproduced without prior written specific authorization of ArcelorMittal CONFIDENTIAL – Privileged Information - ArcelorMittal proprietary information Decarburization • Carbon present at the surface of steel reacts with oxygen containing species forming CO at high temperatures • Surface concentration of carbon decreases • Can be beneficial or detrimental depending on the application of the steel S TA © ArcelorMittal – All rights reserved for all countries Cannot be disclosed, used, or reproduced without prior written specific authorization of ArcelorMittal CONFIDENTIAL – Privileged Information - ArcelorMittal proprietary information 1 mm • EPMA and TOF-SIMS C Si Mn 1 mm 20 15 Element segregation 4 300µm ¾Need to know 5 CE © ArcelorMittal – All rights reserved for all countries Cannot be disclosed, used, or reproduced without prior written specific authorization of ArcelorMittal CONFIDENTIAL – Privileged Information - ArcelorMittal proprietary information Surface hardening • Various techniques to analyze N • EPMA versus hardness S TA 20 15 © ArcelorMittal – All rights reserved for all countries Cannot be disclosed, used, or reproduced without prior written specific authorization of ArcelorMittal CONFIDENTIAL – Privileged Information - ArcelorMittal proprietary information Decarburization • Metallography combined with • GDOES depth profiling before and after annealing 6 7 CE © ArcelorMittal – All rights reserved for all countries Cannot be disclosed, used, or reproduced without prior written specific authorization of ArcelorMittal CONFIDENTIAL – Privileged Information - ArcelorMittal proprietary information Surface hardening • LIBS S TA Intensités N normalisées © ArcelorMittal – All rights reserved for all countries Cannot be disclosed, used, or reproduced without prior written specific authorization of ArcelorMittal CONFIDENTIAL – Privileged Information - ArcelorMittal proprietary information • SIMS 1,00E+04 9,00E+03 8,00E+03 Top 7,00E+03 Bottom 6,00E+03 5,00E+03 4,00E+03 3/4 3,00E+03 1/4 2,00E+03 1,00E+03 0,00E+00 1/2 0 200 Distance 20 15 Surface hardening 400 600 800 9 1000 8 1200 CE © ArcelorMittal – All rights reserved for all countries Cannot be disclosed, used, or reproduced without prior written specific authorization of ArcelorMittal CONFIDENTIAL – Privileged Information - ArcelorMittal proprietary information Local enrichments • EPMA gives combination of sensitivity and lateral resolution S TA © ArcelorMittal – All rights reserved for all countries Cannot be disclosed, used, or reproduced without prior written specific authorization of ArcelorMittal CONFIDENTIAL – Privileged Information - ArcelorMittal proprietary information • GDOES 20 15 Surface hardening 10 Fe4N needles Grain Boundaries rich in N 11 CE Inclusion analysis S TA © ArcelorMittal – All rights reserved for all countries Cannot be disclosed, used, or reproduced without prior written specific authorization of ArcelorMittal CONFIDENTIAL – Privileged Information - ArcelorMittal proprietary information 20 15 © ArcelorMittal – All rights reserved for all countries Cannot be disclosed, used, or reproduced without prior written specific authorization of ArcelorMittal CONFIDENTIAL – Privileged Information - ArcelorMittal proprietary information Inclusion analysis • Local enrichments can lead to particles • Fracture risks • Centre fracture visible 12 • SEM-EDX particle analysis • Performed at ¼ thickness and ½ thickness ¾Potential cause of fracture ¾Search for inter laboratory cross check 13 20 15 © ArcelorMittal – All rights reserved for all countries Cannot be disclosed, used, or reproduced without prior written specific authorization of ArcelorMittal CONFIDENTIAL – Privileged Information - ArcelorMittal proprietary information Conclusions To study variations in the local element concentration several requirements are needed for the technique used: • Good sensitivity • Good lateral resolution • Good depth resolution Examples were shown, proving that many techniques can be used • For sensitive surface analysis GDOES seems a good solution • SIMS gives a reasonable combination of sensitivity and lateral resolution • For optimal resolution EM and EPMA are preferred Inter laboratory tests are very welcome. TA CE © ArcelorMittal – All rights reserved for all countries Cannot be disclosed, used, or reproduced without prior written specific authorization of ArcelorMittal CONFIDENTIAL – Privileged Information - ArcelorMittal proprietary information S 14 30/03/2012 Chris Xhoffer Cynthia Roegiers Dimitri Monteyne Henrique Duarte Alvarenga LIST TASCON Applied Spectra ¾For the scientific stuff All of you ¾For you attention Confidential - ArcelorMittal Global Research and Development Gent 15
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