Carbon nanotubes (CNTs) have emerged as revolutionary nanomaterials with exceptional properties. This study focuses on optimizing acid treatment conditions for functionalizing multi-walled carbon nanotubes (MWCNTs) and investigates the synthesis of zirconia-coated CNTs. Acid treatment was conducted with HNO3 and H2SO4 their combinations with different molarity concentrations. Acid oxidation, particularly with nitric acid, enhances CNT solubility and reactivity. The research explores the incorporation of acid-treated MWCNTs into ceramic composites, addressing challenges in dispersion and bonding. Additionally, a hydrothermal process is employed to coat MWCNTs with zirconia, contributing to the development of nanocomposites with unique properties. Characterization studies, including SEM, TEM, XRD, and Raman spectroscopy, provide insights into structural and chemical aspects. The findings contribute to advancing the application of CNT-based nanocomposites in various technological fields. The study's methodology, involving acid treatment optimization and hydrothermal synthesis, provides a robust foundation for further advancements in the field of nanomaterials and composites. This novel approach results in ZrO2-coated CNTs, showcasing potential applications in catalysts, oxygen sensors, fuel cells, and electronic devices.