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Wetting Assessment Using the Dispensed Drop Method in the Field of Hot-Dip Galvanizing Marie-Laurence Giorgi, Alexey Koltsov

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Wetting Assessment Using the Dispensed Drop Method in the Field of Hot-Dip Galvanizing Marie-Laurence Giorgi, Alexey Koltsov Wetting assessment using the dispensed drop method in the field of hot-dip galvanizing Marie-Laurence Giorgi, Alexey Koltsov To cite this version: Marie-Laurence Giorgi, Alexey Koltsov. Wetting assessment using the dispensed drop method in the field of hot-dip galvanizing. Galvatech 2017, Nov 2017, Tokyo, Japan. hal-01810788 HAL Id: hal-01810788 https://hal.archives-ouvertes.fr/hal-01810788 Submitted on 8 Jun 2018 HAL is a multi-disciplinary open access L’archive ouverte pluridisciplinaire HAL, est archive for the deposit and dissemination of sci- destinée au dépôt et à la diffusion de documents entific research documents, whether they are pub- scientifiques de niveau recherche, publiés ou non, lished or not. The documents may come from émanant des établissements d’enseignement et de teaching and research institutions in France or recherche français ou étrangers, des laboratoires abroad, or from public or private research centers. publics ou privés. WETTING ASSESSMENT USING THE DISPENSED DROP METHOD IN THE FIELD OF HOT-DIP GALVANIZING Marie-Laurence Giorgi 1, Alexey Koltsov 2 1 CentraleSupélec, Université Paris-Saclay, Laboratoire de Génie des Procédés et Matériaux (LGPM), 3 rue Joliot-Curie, F-91192 Gif-sur-Yvette cedex, France 2 ArcelorMittal Global R&D - Maizières Process Research Centre, Voie Romaine, 57283 Maizières-lès-Metz ABSTRACT In hot-dip galvanizing, the steel strip is annealed in an atmosphere of N 2 and H 2, containing only traces of water. One of the main purposes of this heat treatment is to reduce the iron oxides present at the steel surface, in order to improve the wettability by liquid zinc. At the same time, the less-noble alloying elements (Mn, Si, P, Cr, Al) of the steel segregate to the surface and preferentially oxidize. The steel surface is then composed of metallic iron (wetted by liquid zinc) and oxide particles or films (non-wetted by liquid zinc). The main features of wetting are first presented (surface energy, triple line, contact angle) together with simple models to estimate the equilibrium contact angle (Young’s, Wenzel’s and Cassie’s models). Two examples of studies performed by means of the dispensed drop technique in the field of hot-dip galvanizing will then be presented: the forced wetting of a partly oxidized steel by liquid Zn - Al and the final contact angle of a liquid Zn - Al droplet on iron / silica heterogeneous surfaces. Keyword: Selective oxidation, heterogeneous wetting, kinetic and surface energies INTRODUCTION Wetting refers to the study of how a liquid deposited on a solid (or liquid) substrate spreads out. To begin with, the main features of wetting will be defined, namely the surface energy, the triple line, the static and dynamic contact angles and the contact angle hysteresis. Then, it will be shown how to predict the equilibrium contact angle in the case of ideal surfaces (Young’s equation) and rough or heterogeneous surfaces (Wenzel’s and Cassie’s equations). Wetting can be studied at the laboratory scale by means of the dispensed drop technique , in which a liquid droplet is released on a solid sample and its spreading is filmed using a high-speed camera. The parameters characteristic of the wetting can be determined from the images of the film, e.g. the impact velocity of the droplet on the solid substrate, the spreading diameter, the left and right contact angles, the contact angle hysteresis. The dispensed drop technique is particularly well suited to investigate the wettability by liquid metals. This technique will be described in the second part of the paper. In hot-dip galvanizing , the wetting of the steel substrate by the liquid metal bath is the first critical step. Before immersion in the molten metal bath, the steel strip is annealed at about 800 °C in a mixture of N2 and H2 (5 to 15 vol.%) containing a low water partial pressure (20 to 50 Pa). This annealing allows to recrystallize the structure of the steel after cold rolling and to prevent the iron oxidation of the steel surface. However, the conditions used favour the segregation towards the surface and the oxidation of the strengthening alloying elements in steel (Si, Al and Mn for example). After annealing, the steel surface is then composed of metallic iron (wetted by liquid zinc) and oxide particles or films (non- wetted by liquid zinc). In this context, two examples of studies performed by means of the dispensed drop technique will be presented: 1) the forced wetting of a partly oxidized steel by a liquid Zn - Al droplet as a function of its initial kinetic energy and 2) the final contact angle of a liquid Zn - Al droplet obtained on heterogeneous surfaces composed of silica and iron as a function of the surface area fraction covered by silica. SOME FUNDAMENTALS EQUATIONS OF WETTING 1-3) Wetting refers to the study of how a liquid deposited on a solid (or liquid) substrate spreads out. To begin with, the main features of wetting will be defined, namely the surface energy, the triple line, the static and dynamic contact angles and the contact angle hysteresis. Then, it will be shown how to predict the equilibrium contact angle in the case of ideal surfaces (Young’s equation) and rough or heterogeneous surfaces (Wenzel’s and Cassie’s equations). Definitions (surface or interfacial tension, triple line, contact angle) The increase in the surface of a liquid L in contact with a vapour V requires work so that: = . (1) The surface (or interfacial) tension of liquid L in contact with vapour V is then defined as the work by surface unit (in mJ.m -2) required to increase the area of the liquid. For pure liquid zinc, at a temperature T in the range [420, 600°C] 4) , [mJ m ] = 817 ± 15 − 0.23 ± 0.03 . [°C ] − 420 (2) and, in particular, at 450°C, = 810 ± 1 mJ m . Surface energies for solid / vapour and solid / liquid interfaces, called interfacial tensions and noted ! and ! respectively, are defined in the same way. To our knowledge, the surface energies required in the field of hot-dip galvanizing, namely α-iron in equilibrium with saturated zinc vapour and α-iron in contact with liquid zinc, have not been measured yet. As a consequence of Eq. (1), in order to minimize the system’s energy, a droplet placed on a solid takes the shape of a spherical cap if it is small enough in size for gravity to have negligible effect (Figure 1a). The rim of the droplet where the three phases (liquid, solid and vapour) are in contact is called the triple line. The wetting or contact angle θ is defined by the tangent to the droplet and the horizontal substrate. The term of perfect wetting is used if θ = 0°, high partial wetting if θ < 90°, low partial wetting if θ > 90° and no wetting if θ = 180°. When the droplet is spreading on the solid, the contact angle depends on time and is called dynamic contact angle. a) γ LV b) c) θ θW θC vapour liquid γ solid γ SL SV rW f1 f2 Figure 1: A small droplet in equilibrium on a) a flat horizontal surface (Young contact angle " = "#), b) a rough surface (Wenzel contact angle " = "$) and c) an heterogeneous surface (Cassie contact angle " = "%). Equilibrium, advancing and receding contact angles The contact angle at equilibrium on an ideal surface (i.e., smooth and homogeneous), "#, is called the Young contact angle. "# is constant at every point of the triple line and is given by Young’s equation: ! − ! cos "# = (3) For non-ideal solids (i.e. rough and / or chemically heterogeneous), the contact angle θ is not unique but lies between a receding contact angle ") and an advancing contact angle "* . This is called the contact angle hysteresis. Wenzel’s and Cassie’s equation As mentioned earlier, the Young's equation is only valid for a smooth and chemically homogeneous surface. Wenzel 5) and Cassie 6) were among the first ones to be interested in the equilibrium contact angle obtained on rough and heterogeneous surfaces (Figures 1b and 1c). On a randomly rough substrate (Figure 1b), the apparent contact angle at the macroscopic scale "$ is given by Wenzel’s law. Let us consider an infinitesimal displacement + of the triple contact line on the homogeneous rough surface. The change in the Helmholtz free energy , $ associated with this infinitesimal displacement per unit length of the triple contact line is given by: , $ = ! − ! -$+ . cos "$ + (4) Assuming that the local contact angle corresponds to the Young contact angle (Eq. 3), the macroscopic contact angle " can be given by Wenzel’s law at equilibrium ( , $ = 0): /01 "$ = -$ 2 /01 "# (5) with -$ the surface roughness, also called Wenzel’s roughness, defined by the ratio between the actual surface area and its apparent value obtained by the horizontal plane ( -$ 3 1). Let us now consider the case of a smooth and randomly heterogeneous surface (Figure 1c), consisting of two different solids 1 and 2, with Young contact angles "#4 and "# and surface area fractions 54 and 5 = 1 − 54. An infinitesimal displacement + of the triple contact line on the surface causes a change in the Helmholtz free energy , % per unit length of the triple contact line: , % = ! 4 − ! 4 54+ . ! − ! 5+ . cos "% + (6) where !6 and !6 are the surface energies for the solid / liquid and solid / vapour interfaces of solid i (i = 1 or 2). At equilibrium, the apparent contact angle is given by Cassie’s law: /01 "% = 54/01 "#4 . 5/01" # (7) METHODS OF MEASURING WETTABILITY PARAMETERS At high temperature, wetting can be studied by means of the sessile drop method or the wetting balance technique.
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