Over the past few decades, metal–organic frameworks (MOFs) have gathered considerable attention due to their potential for high surface area, crystallinity, and tunable chemical composition. These porous materials are made of metal nodes bridged by organic linkers. Due to the versatility of MOFs, they can be used for different applications ranging from wastewater remediation to biomedical imaging, amongst others. Rare-earth (RE) elements have unique luminescent properties, including narrow emission peaks, large Stokes’ shifts, and long luminescent lifetimes. RE-MOFs have similar properties as MOFs made from the d-block metals such as high surface areas and the capability of forming tunable pores in addition to having metal-based photoluminescence. This work explores a new series of Tb-based and Eu-based MOFs that were synthesised to study the effect of linker-to-metal energy transfer on the quantum yield of Tb(III) and Eu(III) emission from the MOFs. The MOFs presented in this work are analogues of Tb-UiO-66 and Eu-UiO-66 (UiO: University of Oslo). The synthesis, characterization, and photoluminescent properties of Tb-UiO-66 and Eu-UiO-66 analogues are presented in Chapter 2 and 3, respectively. The structure and properties of the materials presented are studied using powder X-ray diffraction, nitrogen adsorption-desorption isotherms, thermogravimetric analysis, inductively coupled plasma mass spectrometry, scanning electron microscopy, proton nuclear magnetic resonance spectroscopy, diffuse reflectance infrared Fourier transform spectroscopy, diffuse reflectance UV-Vis spectroscopy and photoluminescence spectroscopy including quantum yield.