Microwave processing was carried out on SiO2 -B2O3 solutions and gels prepared by sol-gel methods. Monolithic gels were prepared from alcoholic solutions of trimethylborate and tetraethylorthosilicate using a two-step hydrolysis process. A novel technique of Liquid State Processing (LSP) was employed for the first time, and it was found to be faster and more effective than the conventional processing techniques. The structural evolution of the dried products was followed using FTIR. The effect of processing was examined via surface area analysis (BET), electron microscopy, and FTIR. The microwave drying has been compared with conventional oven drying and vacuum drying techniques. Shorter processing times, improved microstructures, and unique properties have been obtained.