Exfoliating B. mori silk into high aspect ratio nanofibrils facilitated by response surface methodology.

Silk fiber is formed by an assembly of fibrils. The fibrils can be isolated by a top-down mechanical process called microfibrillation and the fibrils are known as microfibrillated silk (MFS). The process involves chopping, milling, enzyme treatment and high-pressure homogenization. The milling is an important manufacturing step and to optimize the milling step, a response surface methodology was used in this work where the influence of fiber content in milled suspension, milling time and alkaline concentration were investigated. Output responses for the optimization were diameter distribution of fibrils, size and percentage of different diameter fractions, and the aspect ratio. The main and interaction effects of the milling parameters on these responses were statistically analysed. Milling time was the most significant factor for producing finer fibrils while the fiber content in milling had the maximum impact in reducing the number of large fibrils. Milling time had a positive correlation with the aspect ratio. The optimized milling resulted in MFS with an average diameter of 55.35 nm and 90% of MFS less than 100 nm based on high-magnification SEM image analysis. The aspect ratio of the MFS was 137. The MFS suspension was stable over the pH range 3-11.