Characterisation of magnetic nanostructures for spintronic applications by electron microscopy

The work presented in this PhD thesis concerns the characterisation of the physical structure, composition and domain structure of advanced magnetic materials by electron microscopy within the FP6 European Research Training Network "Spinswitch". In particular the investigations concerned MgO/CoFeB/MgO multilayers to be employed in magnetic sensors (this work was done in collaboration with INESC-MN Lisbon-Portugal); Ni80Fe20/Cu electrodeposited nanowires to be employed as spin transfer torque devices (this work was done in collaboration with NIRDTP Iasi-Romania and University of Salamanca); multilayers with perpendicular anisotropy which represent potential candidates to be employed in the next generation of MRAMs (this work was done in collaboration with Spintec-CEA-Grenoble). Chapter 1 will provide an overview of the physics behind the topics treated during this work and a description of the general motivations of the research carried out. Chapter 2 will provide an overview of all the experimental techniques employed for the fabrication and characterisation of the samples investigated for this research. Chapter 3 aims to present an investigation using conventional transmission electron microscopy (CTEM) and Lorentz microscopy (LTEM) to characterise respectively the physical microstructure and the domain structure of the CoFeB free layer, embedded in a multilayer composed by SiN/MgO(50)/CoFeB(t)/MgO(15), with t from 30 Å down to 14 Å. We carried out first the investigation of the physical structure performed by selected area diffraction and bright field imaging of planar samples and physically the plan view sections show the structure of the films appears similar. The magnetization reversal behaviour observed during Lorentz TEM experiments are found to vary considerably with the CoFeB thickness, with both domain wall formation and magnetisation rotation seen. In the thicker film the behaviour was characteristic of a typical soft magnetic material with uniaxial anisotropy. However the magnetic reversal of the thinner film was more complex. A particular characteristic of the 14 Å CoFeB layer is the variation of domain wall angle seen when varying the orientation of the applied field This wall asymmetry suggests the presence of a unidirectional anisotropic energy term. To assist in the interpretation of these experimental results a modified Stoner–Wohlfarth model has been constructed and calculations have been carried out by using a MATLAB code. The purpose of the project presented in Chapter 4 was the advanced characterisation of multilayered electrodeposited NiFe/Cu nanowires grown in alumina and polycarbonate templates. In particular the objective was the characterisation of the structure and local chemistry of the nanowires by TEM and the classification of nanowire switching deduced by Lorentz microscopy experiments, which are challenging for this specific material system. In order to perform TEM studies on single nanowires, they should be extracted from their template. The chemical etching used to remove the nanowires from the template in addition to issues related to the deposition of Cu, led to nanowires with edge and compositional irregularities, detrimental for their magnetic properties. Indeed, we were not able to classify the nanowire switching and investigate domain walls forming during the reversal process, but we could only observe a change in the magnetising state. A lot of the work described in this chapter deals with the difficulties associated with imaging these challenging nanowires. Issues were discovered that may have resulted from deposition and/or etching for TEM preparation, therefore we do rely heavily on simulations and calculations. The research presented in Chapter 5 will describe the investigation of the reorientation process of the easy axis for two different multilayer systems magnetised out of plane, and the evolution of their domain structure for increasing temperature, and trying to understand the role of the insertion of a Co/Pt/Ni/Pt multilayer from a microscopic point of view. The two multilayers represent the free layer of a perpendicular MTJ (pMTJ) and this study represents a state of development of materials for pMTJs. Experiments were performed by MOKE magnetometry in polar configuration and Lorentz Microscopy in Fresnel mode. Materials were prepared in Spintec-CEA, Grenoble (France) where the MOKE experiments were also carried out, and Lorentz Microscopy experiments were performed in Glasgow. For the first multilayer (with Co/Pt/Ni/Pt) we found that for lower temperatures (25°C - 220°C) the specimen appears to have a strong perpendicular anisotropy. We observed a small scale random domain structure that we can ascribe to perpendicularly magnetised domains. For higher temperatures (220°C - 300°C) we found a behaviour typical of a soft magnetic material magnetised in plane with low anisotropy and high susceptibility. For the second multilayer (without Co/Pt/Ni/Pt), for instrumental reasons, we were not able to investigation of the magnetic behaviour of the specimen for temperatures above 110°C. The magnetisation is out of plane for all the temperatures investigated. The sample develops a different domain structure when the sample is heated below 100°C or above 100°C. In the first case isotropic serpentine domain structure is visible, with a large periodicity, whereas in the second case, an anisotropic stripe domain structure is visible with a small periodicity.