Somrerk Chandra-ambhorn

Possible connection between nodule development and presence of niobium and/or titanium during short time thermal oxidation of AISI 441 stainless steel in wet atmosphere

Abstract AISI 441 ferritic stainless steel is a good candidate for metallic interconnects of solid oxide fuel cells (SOFCs). In this alloy, the minor elements Ti and Nb are used to stabilise the ferritic structure but their influence on steel durability is not well understood. This study focuses on the early stages of oxidation (24 h) at 800°C of AISI 441 under 5%H2O in O2 following the cathodic SOFCs conditions. The typical duplex oxide scale, composed of a (Mn,Cr)3O4 spinel top layer and a Cr2O3 rich sublayer is observed, with oxide nodules growing in places. These objects, in the micrometre range in size, are studied by FIB tomography. The analyses reveal a complex structure and a development strongly linked to the presence of niobium and/or titanium compound(s) in the subjacent substrate.

Development of Tensile Test to Investigate Mechanical Adhesion of Thermal Oxide Scales on Hot-Rolled Steel Strips Produced Using Different Finishing Temperatures

The objective of this work was to carry out tensile tests to investigate the effect of finishing temperature on mechanical adhesion of thermal oxide scale on hot-rolled low carbon steel strips. Two hot-rolled low carbon steel strips were produced in an industrial hot rolling line by fixing a coiling temperature at 620 °C and varying finishing temperatures at 820 and 910 °C. Two testing methods were conducted. First, each of a number of samples was subjected to a given imposed strain with ex-situ imaging of scale surface after straining. Second, only one sample was strained in a test with ex-situ imaging of scale surface at every 2 mm elongation of the sample. A spallation ratio, an area where scale was spalled out and normalised by the total area observed by microscope, was plotted as a function of the imposed strain. These two methods gave the same tendency of results as follows. At a given strain, the spallation ratio of scale on steel produced using higher finishing temperature was larger. The gradient of spallation ratio with respect to the imposed strain of that scale was also steeper. This reflects the higher susceptibility of scale to spall out with increasing imposed strain. This behaviour might be related to the larger thickness of scale on steel produced using higher finishing temperature. For the second testing method, lowering the magnification of microscope to observe scale spallation from 50x to 20x increased R2 of the curve of spallation ratio versus the imposed strain, as well as improved the reproducibility of the test.

Application of the Micro-Tensile Testing to Investigate the Adhesion of Thermal Oxide Scales Grown on AISI 441 Stainless Steel Sheet Oxidised in Air and Water Vapour

A micro-tensile testing has been developed to investigate the adhesion behaviour of the oxide scale thermally grown on AISI 441 stainless steel sheet oxidised at 800 °C in different atmospheres - synthetic air and water vapour. In the test, a sample was placed in a tensile testing machine sitting in the chamber of a scanning electron microscope at room temperature. Evolution of the failure of the oxide scale was monitored in function of the imposed strain. It was found that the scale formed on steel oxidised in synthetic air exhibited the drastically lower spallation ratio in function of strain comparing to the scale on steel oxidised in 20 %v/v H2O/N2. For the sample oxidised in water vapour, it was clearly observed that the scale was primarily failed by the crack perpendicular to the tensile loading direction, followed by the spallation due to the compressive stress generated by the Poisson effect. After the test, precipitates rich in Nb, Si, and possibly Ti were observed at the internal interface between scale and steel substrate. For the oxidised samples that the final polishing direction paralleled to the main sample axis, the strain provoking the first spallation of the samples oxidised in synthetic air and 20%H2O/N2 were 6.23 and 3.52 % respectively. The theoretical model was developed in our previous work to quantify the mechanical adhesion energy. These values were 357 and 68 J.m–2 for the steels oxidised in synthetic air and 20%H2O/N2 respectively.

Plasma Arc Welding between AISI 304 and AISI 201 Stainless Steels Using a Technique of Mixing Nitrogen in Shielding Gas

Plasma arc welding was applied to join AISI 304 and AISI 201 stainless steel sheets. Nitrogen was mixed in argon shielding gas to help control microstructure and improve corrosion property of the weld. It was found that increasing nitrogen in shielding gas from 0 to 12 %v/v reduced the amount of delta ferrite in austenite matrix of the weld from 20 to 16 %v/v. This indicated the role of nitrogen as an austenite stabiliser. From polarisation test in 3.5wt% NaCl solution at 25 °C, increasing nitrogen in shielding gas nobly shifted a pitting corrosion potential from 401 to 472 mV vs Ag/AgCl. This corresponded to the increase of nitrogen content in the weld from 0.11 to 0.19 wt%.

Microstructure, Mechanical and Corrosion Behaviour of Dissimilar Weldments between AISI 304 Stainless Steels and AISI 1020 Carbon Steels Produced by Gas Tungsten Arc Welding Using Different Consumables

Gas tungsten arc welding was applied to join AISI 304 stainless steel and AISI 1020 carbon steel sheets with three types of consumables – AISI 308L, AISI 309L and AISI 316L stainless steel wires. Weld metals produced by all consumables exhibited the identical hardness of ca. 350 HV. This value was higher than those of stainless steel and carbon steel base metals, indicating the relatively high strength of weld metals. The corrosive behaviour of weld metals was investigated by a potentiodynamic method. Specimens were tested in 3.5 wt% NaCl solution saturated by laboratory air at 27°C. A pitting potential of weld metal produced by the AISI 309L consumable was higher than those of weld metals produced by the AISI 308L and AISI 316L consumables respectively. The chemical compositions and microstructure of weld metals were also investigated. The pitting corrosion resistance of weld metals produced by different consumables is discussed in the paper in terms of the pitting resistance equivalent number (PREN) calculated from the chemical compositions and the content of delta ferrite in the austenite matrix of the weld metals.

Characterisation and Pickling Behaviour of Thermal Oxide Scale on Low Carbon Steel Produced from a Thin Slab

Thin slab interested in this work was the one with the thickness of ca. 50 mm and mainly made from recycled steel. Chemical composition of the studied steel strip produced from such slab was Fe with 0.077 wt% C, 0.233 wt% Mn, 0.191 wt% Si, 0.159 wt% Cu and 0.052 wt% Ni. Scale retained on that steel after hot rolling was studied. The hot-rolled sample was pickled in 10%v/v HCl aqueous solution at 80 °C. Weight loss and relative XRD peaks of hematite-per-iron and magnetite-per-iron were measured at different pickling periods of time. It was observed that the as-received scale was crack-free. Hematite-and-iron ratio approached zero at the pickling time of 3 seconds. Magnetite-per-iron ratio gradually decreased with increased pickling time and approached zero later. These results indicated that pickling solution attacked the outermost hematite layer resulting in removing of this layer first. Sublayers of scale consisting of magnetite were completely pickled later. Pickling behaviour was not merely volumetric since scale was crack-free. Mechanical adhesion of scale on steel substrate was additionally investigated by tensile test to help characterise the oxide scale.

Prediction of the Mechanical Properties of Hot-Rolled Low Carbon Steel Strips in Correlation to Chemical Compositions and Rolling Conditions

Seven thousand sets of data consisting of mechanical properties, chemical compositions, and rolling parameters of industrial hot-rolled coils were analysed using multiple regression. This was to establish empirical formulas to predict mechanical properties of steel as a function of chemical compositions and rolling parameters. The empirical formulas predicting yield strength (YS), ultimate tensile strength (UTS) and percentage of elongation (EL) of low carbon steel strip were obtained, e.g. YS = 461+ 418 C + 61.6 Mn + 796 P ¬– 303 S + 159 Si + 146 Cu + 204 Ni + 49.7 Cr + 1127 V + 1072 Ti + 3674 Nb – 266 Mo – 6299 B – 76.3 Al – 557 Sn – 3.54 THK – 0.00758 WID – 0.114 FT – 0.223 CT. The rolling parameters in equation included finishing temperature (FT), coiling temperature (CT), thickness (THK) and width (WID) of strip. R-Square values for the formulas predicting YS, UTS, and EL were 82.3%, 90.1%, and 75.8% respectively. These equations were validated by using another 120 hot-rolled coils. The averages of absolute values of the difference between the predicted and actual values of YS, UTS, and EL were 9.6 MPa, 7.8 MPa, and 2.7 % respectively. Correlation of chemical compositions and rolling conditions with mechanical properties was discussed in the paper.

Comments on the quantification of mechanical adhesion energy of thermal oxide scale on metallic substrate using tensile test

The tensile test, accompanied by the corresponding theoretical model, has been developed to quantify the mechanical adhesion energy of the oxide scale on metallic substrate in our previous works. The method to quantify the adhesion energy took into account the effect of residual stress. The effect of the variation of the measured residual stress on the quantified adhesion energy is assessed in this paper. For the scales failed at strains initiating the spallation of 0.018 and 0.011 followed by the transverse crack, it was found that the quantified adhesion energy of the oxide is not sensitive to the variation of the residual stress measured in the range from 0.5 to 2.0 GPa. This is due to the compensation of the decrease in stored energy due to the stress applied in the loading direction (x direction) and the increase in stored energy due to the stress applied in the direction perpendicular to the loading direction (y direction) when the residual stress increases. For the scale failed by the transverse crack followed by the spallation, the quantified adhesion energy tends to be sensitive to the variation of the measured residual stress. The assumption of energy relaxation during the tensile test is alternatively proposed. It is assumed that the energy stored due to the stress in x and y directions is totally released at the first crack. The energy stored due to the stress in y direction from strain initiating the crack to strain initiating the spallation is used in the quantification of the adhesion energy. The scatter of the adhesion energy values quantified by this method and those measured by the inverted-blister test is reduced comparing to the results reported in the previous work.

Advanced Microstructural Investigations of AISI 441 Early Stage Oxidation in Wet Atmosphere

AISI 441 ferritic stainless steel is a good candidate for metallic interconnects in solid oxide fuel cells (SOFCs). The minor elements Ti and Nb are used to stabilize the ferritic matrix and also to reduce creep by a combination of solid solution strengthening and precipitation of intermetallic Laves phase particles along the grain boundaries. However their influence on the oxidation behavior is not well understood. This study focuses on the early stages oxidation (from 4 to 24 h) at 800 °C of AISI 441 under 5% H2O in O2. A relatively smooth micro-crystallized oxide scale and Ti, Nb containing nodules are observed. The internal microstructure of these objects is studied by FIB tomography which allows computing cross sectional views in any direction of interest. FIB study reveals a complex microstructure and a development strongly linked to the presence of niobium and/or titanium in the substrate.

Mechanical Adhesion and Pickling Behaviour of Thermal Oxide Scales on Hot-Rolled Low Carbon Steel Strips Produced by Different Finishing Temperatures

Hot-rolled low carbon steel strips were produced using two different finishing temperatures at 910 and 820 °C in an industrial hot-rolling line. Mechanical adhesion of scale on the steel substrate at 40 mm from the edge was investigated by tensile test. It was found that the strain initiating the first spallation of scale produced at higher finishing temperature was lower. Spallation ratio which is a spalled area of scale divided by the total area of scale examined under an optical microscope was steeper when the scale was produced at higher finishing temperature. The lower values of strain initiating the first spallation and the higher values of spallation ratio of scale formed both at higher finishing temperature were due to higher thickness of that scale. Pickling behaviour of the hot-rolled steels was investigated by immersing the studied steels in a 10%v/v HCl solution at 80 °C. X-ray diffraction (XRD) peak of hematite relative to that of iron decreased with pickling time and approached zero during pickling periods from 3 to 10 s, while magnetite-and-iron ratio gradually decreased and tended to be zero at longer pickling time. This might indicate the existence of hematite as the outermost layer of scale and subscale containing magnetite as the inner part.