Studies of ferrite, borosilicate and intercalation materials

This thesis is concerned with several aspects of the chemistry of iron compounds. The preparation (with particular emphasis on coprecipitation and sol-gel techniques) and processing of ferrites are discussed. Chapter 2 describes the synthesis of Ni-Zn ferrites with various compositions by three methods. These methods include coprecipitation and sol-gel techniques. The Ni-Zn ferrites were characterised by powder X-ray diffactometry (PXRD), scanning electron microscopy (SEM), vibrating sample magnetometry (VSM), Mössbauer spectroscopy and resistivity measurements. The results for the corresponding ferrites prepared by each method are compared. Chapter 3 reports the sol-gel preparation of a lead borosilicate glass and its addition to Ni-Zn ferrites prepared by the sol-gel method in Chapter 2. The glass-ferrites formed were analysed by the same techniques employed in Chapter 2. Alterations in the microstructure, magnetic and electronic properties of the ferrites due to glass addition are described. Chapter 4 introduces compounds containing Fe-O-B, Fe-O-Si or B-O-Si linkages. The synthesis and characterisation of compounds containing Fe-O-B units are described. The structure of [Fe(SALEN)]2O.CH2Cl2 (17), used in attempts to prepare compounds with Fe-O-Si bonds, was determined by X-ray crystallography. Chapter 4 also details the synthesis of three new borosilicate compounds containing ferrocenyl groups, i.e. [FcBO)2(OSiBut2)2] (19), [(FcBO)2(OSiPh2)2] (20) and [FcBOSiPh3] (21). The structure of (19) was determined by X-ray Crystallographic analysis. Chapter 5 reviews the intercalation properties of the layered host compound iron oxychloride (FeOCI). Intercalation compounds prepared with the microwave dielectric heating technique are also discussed. The syntheses of intercalation compounds by the microwave method with FeOCI as host and ferrocene, ferrocenylboronic acid and 4-aminopyridine as guest species are described. Characterisation of these compounds by powder X-ray diffractometry (PXRD) and M{ssbauer spectroscopy is reported. The attempted synthesis of an intercalation compound with the borosilicate compound (19) as guest species is discussed. Appendices A-E describe the theory and instrumentation involved in powder X-ray diffractometry (PXRD), scanning electron microscopy (SEM0, vibrating sample magnetometry (VSM), Mössbauer spectroscopy and electrical resistivity measurements, respectively. Appendix F details the attempted syntheses of compounds with Fe-O-B and Fe-O-Si linkages.

The Viking age glass beads of Ireland and their North Atlantic context

Hitherto, the majority of studies which have included the discussion of Viking glass beads have mainly focused on the assemblages from individual sites, with limited use of known parallels. Exceptions to this include recent publications regarding the Icelandic material and Callmer’s 1977 catalogue of the finds from mainland Scandinavia, now over thirty years old. Analysis of these finds from Ireland was, for the most part, non-existent. The aim of this research is to address this lack of analysis within Ireland, while incorporating the wider context of the beads within the Viking North Atlantic. The research thus examines the use of glass beads of diagnostically Scandinavian manufacture and import found in Ireland, particularly in relation to their context and distribution. The history of research from Ireland as well as from across the Viking world is considered and explored throughout the thesis, with critique of methods and discussions used. Focussed analysis of both published and unpublished material detailing artefacts from Scandinavia (especially Vestfold), Britain, Iceland, the Faroe Islands and L’Anse aux Meadows is presented within the thesis in order to provide the greater picture for the core section of the thesis, the glass beads found in Ireland. Three appendices are included within Volume 2, databases of the glass beads under discussion from Ireland, the Vestfold region graves in Norway and the topsoil finds from the Kaupang trading place, also located within Vestfold. These appendices therefore represent the first-hand analysis of glass beads by the author. In total, this research represents the most up-to-date analysis of Viking glass beads from Ireland and presents a new look at the patterns of use, trade and interpersonal contact that affected the everyday lives of individuals living within Viking Age Ireland.