The purpose of this thesis is to outline the research undertaken into the preparation of gallium chalcogenide, indium chalcogenide and tantalum nitride nanomaterials. A brief introduction into the general field of nanomaterials is also provided. The focus of this thesis is split into two main areas: Firstly, the preparation of indium and gallium chalcogenide nanomaterials due to their possible improved applications in solar cell technology. Secondly, the attempted preparation of novel tantalum nitride nanomaterials by conventional synthetic methods. These materials may provide effective environmentally benign replacements in situations where existing compounds' toxicities prove unacceptable. This thesis is divided into five main chapters and one appendix. The first chapter introduces the general field of nanomaterials and possible ways of utilising their properties in a variety of applications. It also contains a brief literature review of the materials covered in later chapters. Chapters two, three and four describe the research undertaken concerning the synthesis and characterisation of the aforementioned nanomaterials. Chapter five contains detailed experimental conditions. It also contains information about the specific apparatus and equipment used throughout this research. The appendix is intended to introduce the functions of the primary techniques of analysis which have been used in this thesis.