In the presence of green technology or biodegradable options, vegetable oils emerged as replacements for mineral oil as base oils due to their properties of high viscosity index, high flash point, low toxicity, low volatility, and high biodegradability. Nano fluids were a relatively new class of fluids that consisted of a base fluid with nano-sized particles (1–100 nm) suspended within them. The synthesis and characterization of biodegradable hybrid nano fluids and their combination with base materials were carried out in this paper, playing a vital role in machining operations. SiC and TiO2 were used as nano particles, with the base fluid being palm oil, and sodium dodecyl sulphate (SDS) was employed as a surfactant to maintain fluid stability. All samples were prepared in individual and hybrid modes, including palm oil as the base fluid without any emulsifier/surfactant, palm oil + SiC with nano particle concentrations of 0.1%, 0.2%, and 0.3% by volume, palm oil + TiO2 with nano particle concentrations of 0.1%, 0.2%, and 0.3% by volume, and palm oil + SiC + TiO2 with nano particle concentrations of 0.1%, 0.2%, and 0.3% by volume. The FTIR results showed that the SiC + palm oil and SiC + TiO2 + palm oil samples had better chemical composition and surface characterization as biodegradable hybrid nano fluids. The zeta potential values were observed to increase at volume concentrations of 1%, 2%, and 3%. Particularly, the biodegradable hybrid nano fluid samples (palm oil + 1% Vol. SiC + TiO2) and (palm oil + 2% Vol. SiC) demonstrated increased stability as well as enhanced physical, thermal, and rheological properties in machining applications.