Viscoelastic properties of isolated collagen fibrils.

Understanding the viscoelastic behavior of collagenous tissues with complex hierarchical structures requires knowledge of the properties at each structural level. Whole tissues have been studied extensively, but less is known about the mechanical behavior at the submicron, fibrillar level. Using a microelectromechanical systems platform, in vitro coupled creep and stress relaxation tests were performed on collagen fibrils isolated from the sea cucumber dermis. Stress-strain-time data indicate that isolated fibrils exhibit viscoelastic behavior that could be fitted using the Maxwell-Weichert model. The fibrils showed an elastic modulus of 123 ± 46 MPa. The time-dependent behavior was well fit using the two-time-constant Maxwell-Weichert model with a fast time response of 7 ± 2 s and a slow time response of 102 ± 5 s. The fibrillar relaxation time was smaller than literature values for tissue-level relaxation time, suggesting that tissue relaxation is dominated by noncollagenous components (e.g., proteoglycans). Each specimen was tested three times, and the only statistically significant difference found was that the elastic modulus is larger in the first test than in the subsequent two tests, indicating that viscous properties of collagen fibrils are not sensitive to the history of previous tests.

In vitro fracture testing of submicron diameter collagen fibril specimens.

Mechanical testing of collagenous tissues at different length scales will provide improved understanding of the mechanical behavior of structures such as skin, tendon, and bone, and also guide the development of multiscale mechanical models. Using a microelectromechanical-systems (MEMS) platform, stress-strain response curves up to failure of type I collagen fibril specimens isolated from the dermis of sea cucumbers were obtained in vitro. A majority of the fibril specimens showed brittle fracture. Some displayed linear behavior up to failure, while others displayed some nonlinearity. The fibril specimens showed an elastic modulus of 470 ± 410 MPa, a fracture strength of 230 ± 160 MPa, and a fracture strain of 80% ± 44%. The fibril specimens displayed significantly lower elastic modulus in vitro than previously measured in air. Fracture strength/strain obtained in vitro and in air are both significantly larger than those obtained in vacuo, indicating that the difference arises from the lack of intrafibrillar water molecules produced by vacuum drying. Furthermore, fracture strength/strain of fibril specimens were different from those reported for collagenous tissues of higher hierarchical levels, indicating the importance of obtaining these properties at the fibrillar level for multiscale modeling.

Influence of contamination and cleaning on bond strength to modified zirconia.

OBJECTIVE: To evaluate the influence of contamination and cleaning procedures on shear bond strength (SBS) to modified zirconia surfaces. METHODS: One hundred zirconium-oxide ceramic disks fabricated with a rough modified surface (Nobel Bond), which allows more micromechanical interlocking for adhesive cementation, were divided into five groups. Groups were contaminated with organic (OC; human blood and saliva) and/or inorganic contaminants (IC; type IV dental stone). For cleaning, modified surfaces were etched with phosphoric acid for 1min (PA) or fired in a ceramic furnace up to 910 degrees C and cleaned in an ultrasonic bath in ethanol (FU). Following combinations of contamination and cleaning protocols were chosen: group 1: OC-PA; group 2: IC-FU; group 3: OC+IC-PA+FU; group 4: OC+IC-no cleaning; group 5: no contamination-no cleaning. Level of contamination and efficacy of cleaning were evaluated using X-ray photoelectron spectroscopy (XPS). Composite cylinders were bonded to the disks using dual curing adhesive resin cement (RelyX ARC). Fifty samples were subjected to 20,000 thermal cycles (TC). All samples were tested for SBS. Statistical analysis was performed using one-way ANOVA with alpha=0.05. RESULTS: SBS ranged from 16.6 to 18.8MPa (non-TC) and 10.6-21.7MPa (TC). TC did not lower SBS, except for group 1. XPS showed that OC produced higher levels of carbon, nitrogen, and silica, whereas IC generated elevated levels of calcium, sulfur, carbon, and potassium. Cleaning with both procedures reduced contamination significantly. SIGNIFICANCE: A combination of FU and PA is an efficient method for cleaning contaminated modified zirconia surfaces.

Stress-strain experiments on individual collagen fibrils.

Collagen, a molecule consisting of three braided protein helices, is the primary building block of many biological tissues including bone, tendon, cartilage, and skin. Staggered arrays of collagen molecules form fibrils, which arrange into higher-ordered structures such as fibers and fascicles. Because collagen plays a crucial role in determining the mechanical properties of these tissues, significant theoretical research is directed toward developing models of the stiffness, strength, and toughness of collagen molecules and fibrils. Experimental data to guide the development of these models, however, are sparse and limited to small strain response. Using a microelectromechanical systems platform to test partially hydrated collagen fibrils under uniaxial tension, we obtained quantitative, reproducible mechanical measurements of the stress-strain curve of type I collagen fibrils, with diameters ranging from 150-470 nm. The fibrils showed a small strain (epsilon < 0.09) modulus of 0.86 +/- 0.45 GPa. Fibrils tested to strains as high as 100% demonstrated strain softening (sigma(yield) = 0.22 +/- 0.14 GPa; epsilon(yield) = 0.21 +/- 0.13) and strain hardening, time-dependent recoverable residual strain, dehydration-induced embrittlement, and susceptibility to cyclic fatigue. The results suggest that the stress-strain behavior of collagen fibrils is dictated by global characteristic dimensions as well as internal structure.

Novel method for mechanical characterization of polymeric nanofibers.

A novel method to perform nanoscale mechanical characterization of highly deformable nanofibers has been developed. A microelectromechanical system (MEMS) test platform with an on-chip leaf-spring load cell that was tuned with the aid of a focused ion beam was built for fiber gripping and force measurement and it was actuated with an external piezoelectric transducer. Submicron scale tensile tests were performed in ambient conditions under an optical microscope. Engineering stresses and strains were obtained directly from images of the MEMS platform, by extracting the relative rigid body displacements of the device components by digital image correlation. The accuracy in determining displacements by this optical method was shown to be better than 50 nm. In the application of this method, the mechanical behavior of electrospun polyacrylonitrite nanofibers with diameters ranging from 300 to 600 nm was investigated. The stress-strain curves demonstrated an apparent elastic-perfectly plastic behavior with elastic modulus of 7.6+/-1.5 GPa and large irreversible strains that exceeded 220%. The large fiber stretch ratios were the result of a cascade of periodic necks that formed during cold drawing of the nanofibers.