X-ray reflectivity measurement of interdiffusion in metallic multilayers during rapid heating.

A technique for measuring interdiffusion in multilayer materials during rapid heating using X-ray reflectivity is described. In this technique the sample is bent to achieve a range of incident angles simultaneously, and the scattered intensity is recorded on a fast high-dynamic-range mixed-mode pixel array detector. Heating of the multilayer is achieved by electrical resistive heating of the silicon substrate, monitored by an infrared pyrometer. As an example, reflectivity data from Al/Ni heated at rates up to 200 K s-1 are presented. At short times the interdiffusion coefficient can be determined from the rate of decay of the reflectivity peaks, and it is shown that the activation energy for interdiffusion is consistent with a grain boundary diffusion mechanism. At longer times the simple analysis no longer applies because the evolution of the reflectivity pattern is complicated by other processes, such as nucleation and growth of intermetallic phases.

The effect of prism orientation on the indentation testing of human molar enamel.

Recent nanoindentation studies have demonstrated that the hardness and Young's modulus of human molar enamel decreases by more than 50% on moving from the occlusal surface to the dentine-enamel junction on cross-sectional samples. Possible sources of these variations are changes in local chemistry, microstructure, and prism orientation. This study investigates the latter source by performing nanoindentation tests at two different orientations relative to the hydroxyapatite prisms: parallel and perpendicular. A single sample volume was tested in order to maintain a constant chemistry and microstructure. The resulting data show very small differences between the two orientations for both hardness and Young's modulus. The 1.5-3.0% difference is significantly less than the standard deviations found within the data set. Thus, the variations in hardness and Young's modulus on cross-sectional samples of human molar are attributed to changes in local chemistry (varying levels of mineralization, organic matter, and water content) and changes in microstructure (varying volume fractions of inorganic crystals and organic matrix). The impact of prism orientation on mechanical properties measured at this scale by nanoindentation appears to be minimal.

Nanoindentation mapping of the mechanical properties of human molar tooth enamel.

The mechanical behavior of dental enamel has been the subject of many investigations. Initial studies assumed that it was a more or less homogeneous material with uniform mechanical properties. Now it is generally recognized that the mechanical response of enamel depends upon location, chemical composition, and prism orientation. This study used nanoindentation to map out the properties of dental enamel over the axial cross-section of a maxillary second molar (M(2)). Local variations in mechanical characteristics were correlated with changes in chemical content and microstructure across the entire depth and span of a sample. Microprobe techniques were used to examine changes in chemical composition and scanning electron microscopy was used to examine the microstructure. The range of hardness (H) and Young's modulus (E) observed over an individual tooth was found to be far greater than previously reported. At the enamel surface H>6GPa and E>115GPa, while at the enamel-dentine junction H<3GPa and E<70GPa. These variations corresponded to the changes in chemistry, microstructure, and prism alignment but showed the strongest correlations with changes in the average chemistry of enamel. For example, the concentrations of the constituents of hydroxyapatite (P(2)O(5) and CaO) were highest at the hard occlusal surface and decreased on moving toward the softer enamel-dentine junction. Na(2)O and MgO showed the opposite trend. The mechanical properties of the enamel were also found to differ from the lingual to the buccal side of the molar. At the occlusal surface the enamel was harder and stiffer on the lingual side than on the buccal side. The interior enamel, however, was softer and more compliant on the lingual than on the buccal side, a variation that also correlated with differences in average chemistry and might be related to differences in function.

Preparation of multilayered materials in cross-section for in situ TEM tensile deformation studies.

The success of in situ transmission electron microscopy experimentation is often dictated by proper specimen preparation and sample design procedures. We have developed a novel technique permitting the production of tensile specimens of multilayered films in cross-section for in situ deformation studies. Of primary, importance in the development of this technique is the production of an electron transparent micro-gauge section. This micro-gauge section predetermines the position at which plastic deformation, crack nucleation and growth, and failure are observed. In short, we report in detail, a unique combination of specimen preparation procedural steps and the design of a multilayer foil sample. The ability of these procedures to facilitate the success of in situ TEM tensile studies of layered materials in cross-section is demonstrated using a Cu-Zr multilayer foil.

Atomic force microscope measurements of the hardness and elasticity of peritubular and intertubular human dentin.

An atomic force microscope was used to measure the hardness and elasticity of fully-hydrated peritubular and intertubular human dentin. The standard silicon nitride AFM tip and silicon cantilever assembly were replaced with a diamond tip and stainless steel cantilever having significantly higher stiffness. Hardness was measured as the ratio of the applied force to the projected indentation area for indentations with depths from 10-20 nm. The sample stiffness was measured by imaging specimens in a force-modulated mode. Hardness values of 2.3 +/- 0.3 GPa and 0.5 +/- 0.1 GPa were measured for the peritubular and intertubular dentin, respectively. Stiffness imaging revealed that the elastic modulus of the peritubular dentin was spatially homogeneous; whereas, there was considerable spatial variation in the elasticity of the intertubular dentin. The atomic force microscope can be used to measure the mechanical properties of fully hydrated calcified tissues at the submicron level of spatial resolution, thus augmenting more traditional depth sensing probes.

Hardness and Young's modulus of human peritubular and intertubular dentine.

A specially modified atomic-force microscope was used to measure the hardness of fully hydrated peritubular and intertubular dentine at two locations within unerupted human third molars: within 1 mm of the dentine enamel junction and within 1 mm of the pulp. The hardness of fully hydrated peritubular dentine was independent of location, and ranged from 2.23 to 2.54 GPa. The hardness of fully hydrated intertubular dentine did depend upon location, and was significantly greater near the dentine enamel junction (values ranged from 0.49 to 0.52 GPa) than near the pulp (0.12-0.18 GPa). A Nanoindenter was used to estimate the Young's modulus of dehydrated peritubular and intertubular dentine from the unloading portion of the load displacement curve. The modulus values averaged 29.8 GPa for the peritubular dentine (considered to be a lower limit), and ranged from 17.7 to 21.1 GPa for the intertubular dentine, with the lower values obtained for dentine near the pulp.