The methods compiled in this chapter are important in many areas of materials science and technology because various physical properties of materials (mechanical, thermal, electronic, optical, magnetic, dielectric, biological) depend on their geometric architecture, on scales ranging from the atomic or nanoscopic to the semimicroscopic. Some of the properties are governed only by an elementary atomic group in the structural hierarchy while others are brought about by cooperative functioning of multiple phases or microscopic structures in different dimensions. Corresponding to the vast variety of materials and their properties, a wide range of experimental techniques are available, so that the choice of which technique to employ on starting a study may not be clear. In this respect one should also bear in mind that some of the techniques presented in this chapter are based on physical principles, which are also relevant to the measurement methods compiled in Chaps. 6 and 11.