Metal–organic frameworks (MOFs) also known as porous coordination polymers (PCP) are crystalline compounds including metal ion or cluster of metal ions coordinated to organic linkers. To provide more functionalities and enhance the MOFs properties, design and construction of MOFs composites have been proposed. MOF composites are materials that consist of combination of nanoparticles and MOFs. In this chapter, first a brief review of MOF materials and their synthesis approaches is presented. Then, MOF composites and their synthesis methods and applications are reviewed. Finally, the latest applications of advanced atomic force microscopy techniques to study the crystallization, morphology and structures of MOFs and their composites with nanomechanical characterization are reviewed.