fahmi_dry_cyc_impr.eps Acta Polytechnica Vol. 52 No. 2/2012 Influence of the Surface Layer when the CMT Process Is Used for Welding Steel Sheets Treated by Nitrooxidation I. Michalec, M. Marônek Abstract Nitrooxidation is a non-conventional surface treatmentmethod that can provide significantly improvedmechanical prop- erties as well as corrosion resistance. However, the surface layer is a major problem during the welding process, and welding specialists face many problems regarding the weldability of steel sheets. This paper deals with the properties of a nitrooxidized surface layer, and evaluates ways of welding steel sheets treated by nitrooxidation using a Cold Metal Transfer (CMT) process. The limited heat input and the controlled metal transfer, which are considered as the main advantage of theCMTprocess, have anegative impact onweld joint quality. An excessive amount of porosity is observed, probably due to the high content of nitrogen and oxygen in the surface layer of the material and the fast cooling rate of the weld pool. Keywords: steel sheet, nitrooxidation, Cold Metal Transfer, porosity. 1 Introduction Steel sheets with surface treatment are widely used, above all in the automotive industry. This research work is in response to aproblemencountered inprac- tical applications of this material. An investigation is made of a new surface treatment method that has a major effect on improving the surface properties of steel sheets, e.g. their corrosion resistance. Nitrooxi- dation in afluidizedbed is anon-conventional surface treatment method. This process consists of nitrida- tionwith subsequent oxidation. Nitrooxidation leads to a significant increase in corrosion resistance (up to level 10), and also an increase in mechanical prop- erties, e.g. yield strength and tensile strength (1, 2, 3). The process ofwelding damages the surface layer, and it is necessary to find a way to minimize this damage. A pulse process is applied to limit the ther- mal input in arcwelding, where there is periodic pul- sationof theweldingvoltageand thewelding current. The CMT process, an innovative welding method, can also be used. CMT is a revolutionary short- circuit welding method, which works with digitally- controlled short-circuitmetal transfer in the welding arc. For the first time, this method integrates the wire motion into the welding process and into the overall control of the process. In this way, the, ther- mal input can be limited. This is a major advantage of this welding method (1, 4, 5). Aims Previous studies (3, 5, 6) dealt with ways of welding steel sheets treated by nitrooxidation. Several de- fects were identified in most of the tested methods, e.g. spatter, porosity and weld bead irregularities. Only solid-state laser beam welding was considered satisfactory. Because of the high initial cost of laser equipment, our research focused on finding an ade- quate option in field of arcwelding. Themain aimof the research was to evaluate the possibility of weld- ing nitrooxidizedmaterial using the innovativeCMT welding method. 2 Materials and methods Thin DC 01/DIN EN 10130-9 steel sheets 1 mm in thicknesswereused in the experiments. Thechemical compositionof the steel is shown inTable 1. Thema- terial was subjected to the nitrooxidation process. A fluid environment consisting of Al2O3 grains 120 μm in diameter was used in the nitridation treatment. The oxidation process was carried out in vapours of distilled water immediately after nitridation. The nitrooxidation treatmentparameters arepresented in Table 2. Table 1: Chemical composition of DC 01 EN 10130/91 steel EN C Mn P S Si Al designation [%] [ %] [%] [%] [%] [ %] DC 01 max. 0.10 max. 0.45 max. 0.03 max. 0.03 0.01 – 43 Acta Polytechnica Vol. 52 No. 2/2012 Table 2: The nitrooxidation parameters Temperature T Time t [◦C] [min] Nitridation 580 45 Oxidation 350 5 Table 3: The chemical composition of OK AristoRod 12.50 C Si Mn [%] [%] [%] 0.10 0.90 1.50 The experiments were performed at Fronius Ltd., Trnava. The welding process configuration is shown inFigure 1. RobotisedCMTweldingwasused. A to- tal of 26 specimenswithdimensions of 25×10×1mm were produced. The welding parameters are pre- sented in Table 4. I joints, overlapped joints and flange joints were welded. OK AristoRod 12.50, 1mm indiameter,wasused as thefillermetal. COR- GON18 (18%ofCO2, 82%ofArgon)with flow rate 15l · min−1 was applied as the shielding gas. The chemical composition of the filler metal is shown in Table 3. Fig. 1: Welding process configuration Table 4: Welding parameters of the specimens Specimen Welding Welding Wire Welding Shielding Filler No. current voltage feed rate speed gas metal [A] [V] [m ·min−1] [mm · s−1] 1 92 10.1 3.6 7 Corgon18 OK 12.50 2 92 10.1 3.6 7 Corgon18 OK 12.50 3 81 11.3 3.9 7 Corgon18 OK 12.50 4 90 11.4 3.6 20 Corgon18 OK 12.50 5 89 10.4 3.6 33 Corgon18 OK 12.50 6 90 10.1 3.7 10 Corgon18 OK 12.50 7 88 9.0 5.3 20 Corgon18 OK 12.50 8 88 9.0 5.3 20 Corgon18 OK 12.50 9 88 9.0 5.3 20 Corgon18 OK 12.50 10 92 10.1 3.6 7 Corgon18 OK 12.50 11 92 10.1 3.6 7 Corgon18 OK 12.50 12 81 11.3 3.9 7 Corgon18 OK 12.50 13 90 11.4 3.6 20 Corgon18 OK 12.50 14 89 10.4 3.6 33 Corgon18 OK 12.50 15 90 10.1 3.7 10 Corgon18 OK 12.50 16 98 12.8 5.0 20 Corgon18 OK 12.50 17 86 9.0 5.2 20 Corgon18 OK 12.50 18 94 9.3 5.5 20 Corgon18 OK 12.50 19 103 9.8 6.0 20 Corgon18 OK 12.50 20 103 9.8 6.0 20 Corgon18 OK 12.50 21 107 10.9 4.5 20 Corgon18 OK 12.50 22 120 11.5 5.0 20 Corgon18 OK 12.50 23 158 11.1 5.0 20 Corgon18 OK 12.50 24 107 10.9 4.5 25 Corgon18 OK 12.50 25 179 12.2 6.0 20 Corgon18 OK 12.50 26 158 11.1 5.0 20 Corgon18 OK 12.50 44 Acta Polytechnica Vol. 52 No. 2/2012 The evaluation of the material and of the speci- mens was performed at the Faculty of Materials Sci- ence and Technology in Trnava. Microscopic anal- ysis, spectroscopy and microhardness measurements were performedas an analysis of thematerial proper- ties. Macroscopic analysis, microscopic analysis and microhardness measurements were performed for an evaluation of the joints. GD–OES — QDP (Glow Discharge — Optical Emission Spectroscopy — Quantitative Depth Pro- filing) was performed with the following process pa- rameters: the current was 15 mA at voltage 1000 V. The analysiswas performed on a nitrooxidizedmate- rial andalsoonamaterialwithout surface treatment. Vickers microhardness measurements were per- formed using Buehler IndentaMet 1100 Series equip- ment. The load force applied to the specimen was 981 mN, and the loading time was 10 s. The mea- surementswere carriedout onnitrooxidized andnon- nitrooxidized steel sheets 1 mm in thickness. The measurementsweremade transverselyto thematerial thickness (from top to bottom), and were repeated on three separate specimens (nitrooxidized andwith- out nitrooxidation) in order to obtain averagevalues. The distance between the indents was 80 μm, and the depth of the first indent beneath the surface was 60 μm. 3 Results Material analysis The microstructure of the DC 01 steel after the ni- trooxidation process is shown in Figure 2. Beneath the very thin oxide layer (up to 680 nm), an ε-phase 7–10 μm in thickness was observed. It was composed of Fe2-3N. A compound layer was created under the ε-phase. It consisted of ferritic matrix with needle- shaped γ′–Fe4N nitrides. The compound layer was approximately 200 μm in thickness. These phases were identified by scanning electron microscopy, us- ing a JEOL 7600-F scanning electron microscope. Fig. 2: Microstructure of the DC 01 steel after nitrooxi- dation The results of the GD-OES analysis (Figure 3) showed that, after the nitrooxidation process, the ni- trogen content had increased up to five times in the material surface. This increasewasmainly at the ex- pense of the iron content. The oxygen content at a depth of 1 μm was more than 50% greater. This corresponds with the microscopic analysis, where an oxide surface layer 680 nm in thickness was ob- served. Fig. 3: GD-OES analysis of the material surface a) material without nitrooxidation b) material after nitrooxidation 45 Acta Polytechnica Vol. 52 No. 2/2012 Fig. 4: Microhardness trend comparison of nitrooxidized material (black) and material without surface treatment (red) The results of the microhardness measurements are shown in Figure 4. The graph compares the mi- crohardness of the nitrooxidized material with the microhardness of the material without surface treat- ment. It can be observed that, after the nitrooxi- dation process, the material is affected to a depth of 400 μm. The highest microhardness values were observed on both surfaces of the steel sheet (dis- tances 0 and 1000 μm in the graph). They were 47% higher than the values for the material without surface treatment. Due to limitations of the testing device, the mi- crohardness values in the area of the ε-phase, where much higher values were expected (4), could not be observed. Analysis of the joints: Inappropriate joints were rejected in a visual inspec- tion. Several defects, e.g. weld bead irregularity and weld bead reinforcement were detected. Only speci- menswith theminimumamountofdefectswereanal- ysed. The macroscopic analysis results are presented in Figure 5. The picture shows an excessive amount of porosity, distributed over almost the full length of the joint. Weld bead irregularity together with lack of fusion was also detected. The probable reason for the high porosity lies in the surface layer, which is rich in nitrogen and oxygen. However, the fast cool- ing ratemay also have caused increased porosity, due to insufficient time for the escape of gases originat- ing in the nitrooxidized surface layer and dissolved in WM during its melting process. These are until now just hypotheses, and will be a topic for further research. The microscopic analysis results are shown in Fi- gure 6. The Weld Metal (WM — see Figure 6a) was mainly composed of acicular ferrite. Globular ferrite was observed along the column grain bound- aries. Widmanstätten ferrite was also observed spo- radically. Figure 6b shows the interface between theHighTemperatureHeatAffected Zone (HTHAZ) and WM. HTHAZ consisted of upper bainite, in which the Fe3C needles were secreted, together with coarse-grained acicular ferrite and proeutectoid fer- rite. Coarsening of the primary austenitic grainswas also identified. The Heat Affected Zone (HAZ — see Figure 6c) was composed of a fine-grained structure consisting of globular ferrite. Fig. 5: Macrostructure of the joints Fig. 6: Microstructure of the joints a) WM area b) WM — HTHAZ interface c) HAZ — BM interface 46 Acta Polytechnica Vol. 52 No. 2/2012 Fig. 7: Microhardness values trend The results of the microhardness measurements (Figure 7)proved that thehighestmicrohardnessval- ues were detected in WM. A continuous drop in mi- crohardness was identified towardsHAZ. In the area of BM, the microhardness stabilized, because there was no thermal affection within this area. The re- sults presented here correspondwith the microscopic analysis, where acicular ferrite was observed in the WM area. 4 Conclusion The results show that for steel sheets treated by ni- trooxidation there was a radical increase in micro- hardness values, up to 47%, in comparison with the values for the same material without surface treat- ment. Microscopic analysis identified individual sur- face phases of thematerial treated bynitrooxidation. On the basis of the research results presented here, it can be stated that the given parameters of the CMT process were not suitable for welding steel sheets treated by nitrooxidation, due to the high level of porosity. Future research will focus on changing the shielding gas and the filler metal, and on optimizing the parameters. Acknowledgement This paper was prepared with support from the Slovak Research and Development Agency, grant No. 0057-07 and from the Scientific Grant Agency, grant No. 1/0203/11. References [1] Michalec, I.: CMT Technology Exploitation for Welding of Steel SheetsTreated byNitrooxidation. Master’s thesis, 2010. [2] Michalec, I. et al.: Metallurgical joining of steel sheets treated by nitrooxidation by a hybrid CMT – laser process. In Metal 2011 – 20th An- niversary InternationalConference onMetallurgy and Materials, Brno : Tanger, 2011. [3] Marônek, M. et al.: Welding of steel sheets treated by nitrooxidation, In JOM-16: 16th In- ternational Conference on the Joining of Materi- als & 7th International Conference on Education in Welding ICEW-7, Tisvildeleje, 2011. [4] Dománková,M. et al: Influence ofnitridationand nitrooxidation processes on microstructure and corrosion properties of low carbon deep-drawing steels. In Materials Science and Technology [on- line]. Vol. 11, No. 1, 2011, p. 40–51. [5] Bárta,J. et al.: Joiningof thin steel sheets treated bynitrooxidation. In15th seminar of ESAB:Pro- ceedings of lectures of the 15th ESAB + MTF- STU seminar in the scope of seminars about welding and weldability. Trnava : AlumniPress, 2011, p. 57–67. [6] Jančár, J. et al.: Laser beam utilisation in weld- ing of steel sheets treated by nitrooxidation. In Využit́ı laseru v průmyslu.Plzeň : 2011, p. 25–35. Ivan Michalec E-mail: ivan.michalec@stuba.sk Materiálovotechnologická fakulta STU Katedra zvárania J. Bottu 25, 917 24 Trnava Milan Marônek E-mail: milan.maronek@stuba.sk Materiálovotechnologická fakulta STU Katedra zvárania J. Bottu 25, 917 24 Trnava 47