I had studied development aspects of sustained release microspheres of Diclofenac sodium that release the drug Up to 24 hour and improve Bioavailability of Diclofenac Sodium by using spray drying and simple solvent evaporation technique.Preparation of Chitosan Microsphere with Diclofenac Sodium by various techniques such as spray drying and simple solvent evaporation technique. For Spry Drying technique the optimization of Spry Dried Parameter such as inlet Temperature and Feed pump Rate. Optimization of Temperature by taking the 130 degree C,as a starting Temperature and showing the Characteristic of Microspheres. Study Shows that the fine Partical were found in 150 degree C. Temperature,Feed Pump rate was also optimizes by this way and 2ml/min feed pump rate shows good Microspheres with higher %yield. So parameters were taken 150 degree C temperature and 2ml/min feed pump rate and Microspheres were Prepared. Further study with Drug to polymer ratio like 1:1,1:3 and 1:5 are carried out.As increase in the drug to polymer ratio from 1:1,1:3 and 1:5 the Entrapment efficiency was also increase and the release rate were Extended.