This course will introduce basic principles of widely used surface and structural characterization techniques to advanced undergraduate and graduate students. Useful experimental methods to discern and identify both macro- and nano-scale properties will be discussed in depth, while focusing on the surface and interfacial analysis of various materials such as metals, semiconductors, polymers, and biological materials. During the course, students will apply basic knowledge of chemistry, physics, and biology to understand scientific fundamentals, operating principles, and instrumental designs of many spectroscopy- or microscopy-based methods. The course teaches a range of these experimental methods for determining surface topology, metrology, elemental composition, chemical states, and other crucial material properties. Some examples of these techniques include secondary-ion mass spectrometry, scanning probe microscopy, electron microscopy, optical microscopy, electron spectroscopy, Raman spectroscopy, scanning confocal florescent microscopy, diffraction techniques, X-ray photoelectron spectroscopy, and ellipsometry. When appropriate, the course will cover pertinent derivations and formulations to explain suitable applications, technical requirements, capabilities and limitations of each characterization technique. Students will learn how the principles of such surface and structural characterization techniques are used for controlling and improving desired properties of materials during their synthesis from real-life examples taken in the active research area of Surface Science.