M. Lamberigts

Use of XPS to investigate surface problems in ULC deep drawing steels

Abstract During continuous annealing prior to hot dip galvanising, the surface of ULC ( U ltra L ow C arbon) deep drawing steels undergoes a range of chemical modifications that can affect interface reactions, thus influencing the quality of the metallic protective coating and the products final users properties. These phenomena were investigated by XPS, in a high-resolution, fully automatic spectrometer coupled with a tight preparation chamber, where the treatment can be simulated very faithfully, in terms of both heat cycle and protective atmosphere. Under vacuum, the equilibrium (Gibbs) surface segregation of alloying — or tramp — elements such as P, Sn, Sb, As, S and C is clearly the predominant phenomenon. Selective oxidation grows much more significant when annealing is performed under a water vapour containing N2–5%H2 protective atmosphere. It involves highly oxidisable elements such as Al, Mn and Si. Though much less intense than under vacuum, Gibbs segregation however remains present, in direct competition with selective oxidation.

Texture Evolution of Tertiary Oxide Scale during Steel Plate Finishing Hot Rolling Simulation Tests

Thin tertiary scale layers have been grown on ULC steel specimens under controlled conditions. After heating under a protective atmosphere (nitrogen), the samples have been oxidised in air for various oxidation times at 1050°C. These experiments are considered a quantitatively and qualitatively reasonable simulation of the scale formation and growth occurring before hot rolling. Immediately after controlled oxidation, some of the samples were subjected to plane strain compression, in order to simulate the finishing hot rolling process. This approach provided a better insight into the deformation behaviour of the tertiary oxide layer in the first hot rolling pass. The layers produced were examined under the SEM using the EBSD technique for texture characterisation and phase morphology determination. The texture of the deformed oxide scales, originally grown on ULC steel at 1050°C, was determined in order to achieve a better understanding of their complex deformation behaviour. This paper gives a first approach of the study of deformed oxides by EBSD. Strongly textured wustite grains with a clearly pronounced columnar structure were observed after oxidation at 1050°C. As the substrate deformation probably affects the oxide layer, orientation relationships between scale layer and substrate were observed. The detailed EBSD study reveals that the oxide layer can accommodate a significant amount of deformation. The oxide layers exhibit good adhesion to the substrate and remain homogeneous over the thickness after compression.

High Temperature Oxidation of Ultra-Low-Carbon Steel

An oxide scale layer always forms at the strip surface during the hot rolling process. Its properties have a large impact on surface quality. The most important features of the oxide layer are its thickness, composition, structure, adherence and coherence. Temperature, time and gas atmosphere determine the growth of oxide layers. In this paper, the high temperature oxidation properties of ultra low carbon steels are discussed in terms of oxide growth mechanism, kinetics and phase morphology. The oxidation kinetics of ultra-low carbon steel (ULC) in air, its scale structure and composition were investigated over the temperature range 923-1473K. Oxidation experiments were performed either under controlled atmosphere or in air, to analyse the oxidation process during strip production. A first series of experiments was carried out in an electric furnace at temperatures ranging from 923 to 1473K, for times between 16 and 7200s. A second series was carried out in a device especially designed to control the atmosphere. After heating under pure nitrogen, the samples were oxidised in air at temperatures between 923-1323K for various oxidation times. Thus treated specimens were characterised by metallography and their scale thickness was measured under the optical microscope. Scale morphology was studied and scale composition confirmed by EDS (Energy Dispersive Spectroscopy) and EBSD (Electron Backscattered Diffraction) analysis. Results show that scale growth under controlled atmosphere is significantly faster than under non controlled conditions, additionally the adherence of the scale formed in the laboratory device was significantly better than the other one. It is clear that scale thickness and constitution depend strongly on the oxidation potential of atmosphere. Computed parabolic activation energies (Ea) values are in good agreement with those found in the literature.

Surface reactions occurring on Fe-based alloys submitted to heat treatments under protective or reactive atmospheres

Surface condition control is particularly important in industrially processed materials, because apparently minor surface phenomena involving selective oxidation or low concentration element segregation can modify the surface reactivity and alter the materials response to downstream treatments. These phenomena, therefore, must be investigated by the most sophisticated simulation and surface analysis techniques, to ensure that accidental contamination is avoided. The paper reports on combined XPS, AES and SIMS spectroscopy to assess quantitatively the surface modifications taking place in Fe-based alloys during annealing treatments under various atmospheres. A new method has been developed from the equations initially put forward by Seah to assess element and compound surface coverage, based on experimental XPS peak intensities, computed inelastic mean free paths and atom densities. It has been applied successfully to annealed specimens made of Fe, Fe-0.5%Si binary alloy and ultralow carbon (ULC) deep-drawing steel.

Tertiary Scale Behaviour during Finishing Hot Rolling of Steel Flat Products

Steel strip surface oxidation during hot mill processing represents an industrial and environmental problem: secondary oxide is removed after roughing, but tertiary oxide scales already start to form before entering the finishing stands. Their properties affect the final steel surface quality and its response to further processing. Controlling the oxide layer growth kinetics and mechanical properties can make pickling easier and improve downstream behaviour. A thin wustite-dominated scale layer (<20 μm) is created under controlled conditions in an original laboratory device adequately positioned in a compression test machine to investigate plane strain compression. A first series of oxidation tests were performed on a ULC steel grade to measure the kinetics of oxide scale growth. The samples were first heated up under a protective atmosphere (nitrogen), before being oxidised in air at different temperatures for various oxidation times. These experiments can be considered fair quantitative and qualitative simulations of scale growth as it occurs in a hot strip mill, insofar as the results thus obtained are in good agreement with the literature. After the oxide growth, plane strain compression (PSC) was performed immediately to simulate the hot rolling process. The oxide layers were characterised before and after compression tests by optical and secondary electron microscopy. As expected, the oxide is seen to deform during compression. The obtained oxide layers exhibit good adhesion to the substrate and homogeneity over the thickness, even after compression.

Temperature Evolution During Plane Strain Compression Of Tertiary Oxide Scale On Steel

An oxide scale layer always forms at the steel surface during hot rolling. This scale layer separates the work roll from the metal substrate. Understanding the deformation behaviour and mechanical properties of the scale is of great interest because it affects the frictional conditions during hot rolling and the heat‐transfer behaviour at the strip‐roll interface. A thin wustite scale layer (<20 μm) was created under controlled conditions in an original laboratory device adequately positioned in a compression testing machine to investigate plane strain compression. Oxidation tests were performed on an ULC steel grade. After the oxide growth at 1050°C, plane strain compression (PSC) was performed immediately to simulate the hot rolling process. PSC experiments were performed at a deformation temperature of 1050°C, with reduction ratios from 5 to 70%, and strain rates of 10s−1 under controlled gas atmospheres. Results show that for wustite, ductility is obvious at 1050°C. Even after deformation oxide layers...