A combinatorial research methodology is outlined with the potential to investigate material factors in photoresist formations more rapidly than with traditional experimental design. The approach involves generating a gradient. of processing variables in the photoresist film and using a set of analysis tools to "map" the photoresist properties as a function of the gradient variables. While high-thruoghput strategies have proven useful for empirical optimization of photoresist processing conditions, they have not been fully exploited to probe the complex array of material issues in projection lithography. Of primary importance in combinatorial methodologies is the generation of variable gradients. The focus of this article is to) illustrate techniques to generate a gradient in bake temperature and bake time in the polymer films, and to illustrate that these gradient techniques can be used to probe fundamental properties of lithographic materials, such as deprotection kinetics. These gradient techniques were applied to rapidly probe the deprotection behavior of a poly (tertbutyloxy-carbonyloxy-styrene). The deprotection data, obtained by applying the combinatorial gradients, agrees well with previous literature, validating the accuracy of these high throughput methods. The advantage of the combinatorial research strategies lies in the potential to investigate fundamental lithographic phenomena more rapidly than with traditional experimentation.