Shear creep of injectable collagen biomaterials

Shear creep experiments in a parallel-plate apparatus were carried out on two injectable forms of collagen: semidilute nonfibrillar solutions (32 and 45 mg protein/mL) and aqueous fibrillar suspensions (at 35 and 65 mg/mL). Nonfibrillar solutions were more easily deformed than fibrillar suspensions, and both materials continued to deform slowly, even at long times (up to 6 X 10(4) sec). When the creep compliance, J(t), was plotted versus t1/3, regions of linear dependence were identified, which indicated that the materials were undergoing Andrade creep. At higher stress levels, J(t) diverged from t1/3, and true viscous flow occurred. A delayed viscosity could be calculated which agreed with viscosities derived from measurements under conditions of steady shear Couette flow. The time of onset of viscous flow was identified with a specific strain for each material, suggesting yield strain behavior. An analysis of recovery curves showed that at low stress levels or for short experimental times, the Boltzmann superposition was approximately obeyed, indicating linear behavior. At high stress levels and times greater than 10(3) sec, both nonfibrillar solutions and fibrillar suspensions showed marked curvature of stress-strain curves, which indicated that the materials are nonlinear in creep.