SYNOPSISThe influence of gultaraldehyde (GA) crosslinking, basic chromium sulfate (Cr) tanning, and thermal treatments on the fracture behavior and morphology of spun collagen fibers has been studied. The fracture morphology of the fibers is characterized by longitudinal splitting along the fiber axis. Although the essential fracture morophology was not influenced by GA crosslinking, Cr tanning, and thermal treatments, the process of splitting depended on the kind of crosslink. Noncrosslinked and Cr-tanned fibers were split into fibrils, but GA-crosslinked fiber was split without fibrillation. The thermal treatments have two effects: One is decrease in number of defects and/or flaws; the other is gelatinization. In the thermal treatment above 14OoC, the gelatinization plays a more important role for the tensile properties than does the effect of a decrease of a defect. Gelatinization results in the enhancements of slippage and separation of macrofibrils and/or fibrils after the yield point. 0 1996 John Wiley & Sons, Inc.
I NTRO DU CTI ONThe spun collagen fiber, which is the strongest among protein fibers,' is a kind of man-made protein fiber. There have been many studies in the 1930s on the protein fibers to make silk from natural proteins such as casein, soybean, corn, and peanut.' Besides, the spun collagen fibers were studied to apply to a surgical suture to utilize the byproducts in the leather i n d u~t r y .~-~ Nevertheless, at the present time, the industrialization of protein fibers made from natural proteins is still not successful because of the insufficient mechanical properties for a practical use.The structure, properties, and fracture morphology of natural collagen fibers such as rat tail tendon (RTT) were discussed in some review^^^^ and many report^.^-'^ There have been some articles discussing the influence of extraction rate, time of coagulation, coagulation agents, and gultaraldehyde ( GA ) crosslink on the tensile strength of spun collagen fibe~-.~,~ For example, Harmed and Rodriguez reported that both crosslinking and scission reactions compete * To whom correspondence should be addressed. with each other during irradiation.16 Schimpf and Rodriguez described that tensile strength shows the maximum value when the fibers are treated at 0.2% GA concentration and then decreases due to the competing crosslink and chain scission mechan i s m~.~ The structure and mechanical properties of the collagen fiber from pepsin-soluble collagen were also reported by Utsuo and T a n i g u~h i .~,~. '~ However, there has been no detailed studies on the fracture mechanism of the spun collagen fibers from a viewpoint of fracture morphology comparing GA-crosslinked fibers with basic chromium sulfate ( Cr ) tanning fibers. The purpose of this article was to investigate the influence of GA crosslinking, Cr tanning, and thermal treatments on the fracture behavior and morphology of the collagen fibers spun from alkaline-soluble collagen.
EXPERIMENTAL Preparation of Collagen SolutionAs the method of preparing collagen ...