Refractory materials are present in a large panel of industrial applications due to their specific properties. They are applied in several parts of many installations designed to face severe working environments such as high temperature, corrosion and thermal shock solicitations. Among the required properties, thermal shock resistance is a key parameter to enhance their service life. This thermal shock resistance is usually directly related to a specific mechanical behaviour induced by a voluntary micro-cracked microstructure. Indeed, depending on micro-cracking level, the mechanical behaviour will change from pure elastic to a “non-linear” one.
In order to accurately determine constitutive laws for such materials to feed finite element method (FEM), it was necessary, during the past 15 years, to develop uniaxial tests taking into account that these materials are characterized by a low level of strain-to-rupture. Nowadays, accurate instrumented tensile test using extensometers are available. However, such tensile devices involve some complexity for tests management (sample machining and well aligned loading grips). Fortunately, the occurrence of optical techniques such as digital image correlation (DIC) which allows to obtain the overall strain fields on a given loaded sample, coupled to FEM modelling, give today new opportunities for experimental investigations of refractory materials exhibiting a non-linear mechanical behaviour.
In this context, the main objective of the present PhD was to enrich the mechanical characterization of refractory materials by evaluating the efficiency of DIC applied on quite common mechanical tests in this scientific community: such as four-points bending test, Brazilian test and Wedge splitting test. For this purpose, it was necessary first for SPCTS laboratory to master this new DIC measurement tools and to apply them on refractory materials which exhibit low level of strain-to-rupture.
This research activity has been developed in the framework of the Federation for International Refractory Research and Education (F.I.R.E) which aims to promote a worldwide collaboration between academic institutes and industrial companies to pool the expertise at master and PhD levels in the field of refractories. In this purpose, multi-partners programs are regularly launched to support research activities. The present PhD (funded by the region of Limoges) has been part of F.I.R.E project D which took place between 2011 and 2014 and which was devoted to “dense refractories with enhanced flexibility for thermal shock”. This research program was organized through a collaboration between two laboratories (SPCTS-Limoges-France, RWTH-Aachen-Germany) and four industrial partners (Alteo-France, RHI-Austria, Tatasteel-Netherland and Tenaris-Argentina).
Even if the objective of the present PhD was to apply DIC techniques to refractory characterization, one should note here that absolutely no DIC expertise was present at SPCTS laboratory before the present work. Thus, in addition to the previously indicated partnerships, and in order to take advantage of the great expertise in photo-mechanics which has been developed for many years in Pprime Institute-Poitiers, a close collaboration has been also established with these colleagues. Nevertheless, due to the very low level of strain-to-rupture of refractory materials, it has been necessary to improve DIC techniques for our own purpose.
The first chapter is dedicated to establish the state of the art concerning thermal shock of refractories and non-linear behaviour by mechanical and energetic approaches. Then, optical methods used to complete the mechanical investigation of refractories such as DIC and mark tracking method have been introduced. Besides, in order to overcome the problem of mechanical characterization of the non-linear behaviour, kinematic fields obtained by DIC are conjugated to FEM in the framework of the identification technique by finite element method updating (FEMU-U).
The chapter II aims to present different experimental characterization techniques. The mechanical ones are associated to optical methods which are here described in details. Then, the studied materials chosen in order to develop and to valid efficiency of DIC are introduced. Among these materials, a model one based on aluminium titanate (AT) developed for academic purposes, and some industrial ones based on magnesia spinel systems delivered by industrial partners.
The main objective of the first investigation, detailed in chapter III, is to demonstrate the efficiency of the DIC technique as an effective tool to complete the mechanical analysis of refractory materials. This first study highlights the specific non-linear mechanical behaviour of AT during four-points bending test at room temperature.
In chapter IV, the acquired DIC expertise has been used to complete the characterization of industrial magnesia spinel refractories. Even if spinel inclusions are used to promote micro-cracking by thermal expansion mismatch with the magnesia matrix, the low level of flexibility of these industrial materials which is less accentuated than AT, pushed us to improve the accuracy of DIC measurements.
After having studied experimentally the non-linear mechanical behaviour of several refractories, chapter V is dedicated to the numerical development of FEMU-U for linear elastic behaviour materials under four-points bending test, then, the developed approach has been applied for flexible AT materials.