The rapid development of nanotechnology has led to the emergence of hybrid nanomaterials with diverse applications across various fields. These materials combine different types of nanoparticles, organic molecules, or polymers to achieve enhanced properties and multifunctionality. To fully exploit the potential of hybrid nanomaterials, accurate and comprehensive characterization methods are crucial for assessing their performance and understanding their structure-function relationships. Characterization techniques such as electron microscopy, spectroscopy, and atomic force microscopy play a pivotal role in unravelling hybrid nanomaterials' intricate structures and properties, facilitating their integration into cutting-edge technologies and innovative solutions. This chapter aims to provide an in-depth exploration of the characterization techniques employed to evaluate the performance of hybrid nanomaterials, showcasing their significance in guiding material design and application development.