$$\rightleftharpoonup{xx}$$
$$\longleftharp{xx}$$,
$$\longrightharp{xx}$$,
A variety of electromagnetic (EM) sensors have been developed or commercialized for evaluating and monitoring microstructure, mechanical properties or creep damage in ferritic steels during industrial processing, heat treatment or service exposure1,2. These sensors operate in a non-destructive and non-contact fashion and are based on the principle that microstructural changes in ferritic steels alter their electrical and magnetic properties. In order to interpret the EM signals in terms of microstructures, one has to link the EM signals to their causal magnetic properties and then to the microstructure of the materials. Relationships between the various EM sensor signals such as mutual inductance for multi-frequency EM sensors and the EM properties (e.g. relative permeability and conductivity) are well established in electromagnetics research with analytical relationships having been reported for several typical sensor geometries3. However, the relationships between the EM or magnetic properties (e.g. the initial permeability, coercivity) and specific microstructures still remain more or less empirical, qualitative or, in many cases, unavailable, particularly when there are more than one type of microstructural features of interest affecting the magnetic behavior4.
Ferromagnetic materials contain magnetic domains, consisting of aligned magnetic moments, separated by domain walls (DWs). As a magnetic field is applied, domains will be re-aligned through DW motion, domain nucleation and growth, and/or domain rotation. More details on domain theory can be found elsewhere5. Microstructural features such as precipitates or grain boundaries can interact with these processes and hence affect the magnetic properties of ferromagnetic materials4,6,7,8. The different microstructural features in steels and their magnetic properties can affect the domain structures and the DW movement process when a magnetic field is applied. It is necessary to look into the magnetic domain structure and the interaction between DWs and microstructure features under different applied fields and frequencies in order to establish a fundamental link between the microstructure and magnetic properties in steels.
Magnetic hysteresis loops or BH loops can describe the fundamental magnetic properties of the materials such as the coercivity, remanence, differential and incremental permeability, amongst others. BH loop analysis has become a useful non-destructive testing (NDT) technique for evaluation of microstructure and mechanical properties of ferritic steels9,10. The BH loop is a plot of the magnetic flux density in the material under inspection (B) versus the applied magnetic field (H). As a magnetic field is induced in the sample by an excitation coil provided with a time varying current, B is measured using a second coil encircling the sample under inspection, while H is measured using a magnetic field sensor (commonly a Hall sensor) placed close to the surface of the sample. The most accurate measurement of a material's BH characteristics can be made using a closed magnetic circuit, like that presented by a ring sample, but other methods such as the use of a separate excitation core can yield satisfactory results. It is of both great scientific significance and practical value to be able to carry out in situ observation of the DW movement processes during magnetic measurements and to directly link these to the magnetic properties and microstructure. Meanwhile, it is very challenging to do either the domain observation or the magnetic measurements without affecting the other.
Amongst various domain imaging techniques, the Bitter method, i.e. using fine magnetic particles to reveal magnetic DWs, has some obvious advantages including easy set-up and high sensitivity11. Due to the use of a medium, e.g. ferro-fluid, it takes a lot of experience and time to obtain high quality patterns and consistent results using Bitter methods. Standard metallographic sample preparation, intended and optimized for optical microscopy (OM) and scanning electron microscopy (SEM), usually yields unsatisfactory Bitter patterns for many steels because the Bitter method is less tolerant to the residual subsurface damage and the associated artificial effects than OM and SEM. There are possible artificial effects due to poor application of ferro-fluid. This paper details additional sample preparation procedures, compared to the standard metallographic ones, preparation and application of ferro-fluid, observation of domain structures using optical microscopes and the method for in situ magnetic measurement.
Many studies on the observation of domain structures in single crystals (e.g. Si-iron12) or grain-oriented Si electrical steels have been reported13. In these materials only a small number of microstructural features (i.e. grain/crystal orientation and grain boundaries) were involved and the domain structures are relatively coarse (with the domain width being on the order of 0.1 mm12). In this paper, domain patterns in polycrystalline ferritic steels, including a plain low carbon steel (0.17 wt% C) have been observed and reported. The low carbon steel has much finer grain size (approximately 25 µm on average in equivalent circular diameter) and finer domain structure (with the domain width on the order of micrometers) than the electrical steels and hence show complex interactions between the various microstructural features and DW movement processes.
This paper proposes a novel bespoke rig for dynamic domain imaging using the Bitter method with in situ BH (magnetic hysteresis) measurements. The reported method takes advantage of the convenience and high sensitivity of the traditional Bitter method and enables in situ BH measurement without interrupting or interfering with the domain wall movement processes. This facilitates establishing a direct and quantitative link between the domain wall movement processes-microstructural feature interactions in ferritic steels with their BH loops. This method is anticipated to become a useful tool for the fundamental study of microstructure-magnetic property relationships in steels and to help interpretation of electromagnetic sensor signals for non-destructive evaluation of steel microstructures.