Design of experiment is a powerful Quality Engineering tool that can help researchers and engineers to identify main variables which affects the performance. Silicon carbide particles and whiskers were produced by pyrolysis of stoichiometerically balanced rice husk. The aim of this paper is to increase the yield of silicon carbide whiskers by optimizing process conditions. Rice milling generates a by-product known as husk. This husk contains about 75 % organic volatile matter and the balance 25 % is inorganic matter. Inorganic matter is rich in silica and organic matter is rich in carbon. To balance stoichiometric proportion, rice husk was treated with different silica sources. Different process conditions that affect the quality of whisker formation were identified and experiments were conducted using Taguchi’s design of experiment. Four factors at three different levels were selected and L9 array design of experiments was conducted. To determine the effect each variable on the output, the signal-to-noise ratio was calculated and factor effect diagram was drawn for each experiment conducted. The process parameters optimized using this design include silica source, pyrolysis temperature, silica to carbon ratio and heating rate. Silicon carbide produced from rice husk was characterized using scanning electron microscope to identify the microstructure. From Taguchi factor effect diagram it has been found that carbon to silica ratio and pyrolysis temperature plays a major role in whisker formation among the selected levels.