Correlated force and contact resonance versus displacement responses have been resolved using load-dependent contact-resonance atomic force microscopy (AFM) to determine the elastic modulus of low-k dielectric thin films. The measurements consisted of recording simultaneously both the deflection and resonance frequency shift of an AFM cantilever probe as the probe was gradually brought in and out of contact. As the applied forces were restricted to the range of adhesive forces, low-k dielectric films of elastic modulus varying from GPa to hundreds of GPa were measurable in this investigation. Over this elastic modulus range, the reliability of load-dependent contact-resonance AFM measurements was confirmed by comparing these results with those from picosecond laser acoustic measurements.

In this work, the correlation between magnetic-domain structure and microstructure in combined reaction-processed equiatomic L10 FePd has been investigated using magnetic force microscopy. The microstructure consisted of approximately equiaxed grains with an average grain size of ∼1 μm and a grain size distribution ranging from below the theoretical critical domain size (Dcrit∼0.2–0.3 μm) up to approximately 5 μm in diameter. The domain structure was characterized as “mixed” in nature, consisting of smaller single-domain grains, larger multidomain grains, and a larger scale interaction domain structure encompassing many grains. The domain boundaries separating interaction domains tended to lie along grain boundaries, and it is proposed that the observed interaction domains should be considered in descriptions of the magnetization and magnetization reversal behavior of this material. In particular, pinning of interaction domain walls by intragranular features of the microstructure such as grain boundaries and single-domain grains could play a role in the measured coercivities.

This article presents an experimental procedure to perform highly localized compression tests on nanoscale structures/features, such as nanospheres and nanopillars, via standard nanoindentation equipment. Current manufacturing capabilities, such as focused ion beam (FIB), lend themselves well to the creation of micron-spaced nanostructures, but it is fundamental to target an individual instance with little or no damage to the surrounding ones. The procedure successfully addresses the problem of locating and testing purposely designed nanostructures of order of 50 nm or less. The technique is illustrated for the case of closely spaced arrays of nanopillars, which were successfully manufactured, characterized, and tested through several pieces of equipment. For the purposes of compression, along with a traditional Berkovich tip, a new multifunctional (MF) tip was devised. This last tip is endowed with a complex contact geometry enabling both atomic force microscope (AFM) scanning and flat punch compression of the nanostructure. The levels of accuracy in tip positioning as well as robustness to alignment errors are unprecedented in comparison with previous in situ compression tests. As a consequence, the MF tip becomes a versatile tool that can be used beyond uniform compression. As an example, ancillary shear tests in controlled conditions are reported. Such results may lay the bases for metal-forming processes at the nanoscale, such as nanoforging or cutting operations, which are relevant to MEMS design and manufacturing.

Measurements of single asperity wear on oxidized silicon surface in aqueous potassium hydroxide (KOH) using atomic force microscopy (AFM), where the single crystal silicon tip was used both to tribologically load and image the surface, is presented. AFM was also operating in the lateral (frictional) force mode to investigate the pH dependence of kinetic friction between the tip and the SiO2 surface. It was shown that the Si tip wear amount strongly depended on the solution pH value and was at a maximum at around pH 10. It was also found that the Si removal volume in mol was approximately equal to that of SiO2 irrespective of the solution pH value. This equality implies that the formation of the Si–O–Si bridge between one Si atom of the tip and one SiO2 molecule of the specimen at the wear interface. The surface of the Si tip is then oxidized. Finally, the bond rupture by the tip movement will occur, the dimeric silica (OH)3Si–O–Si(OH)3, including the Si–O–Si bridge, is dissolved in the KOH solution. The frictional signal is also sensitive to the pH values of the solution and peaked at around pH 10. These results indicate that the removal behavior of the Si tip and SiO2 surface would be affected by the frictional force between the Si and the SiO2, because of an increased liquid temperature and a compressive stress in Si and SiO2 networks. Strong influence is observed by the pH of the ambient solution confirming the important role of the OH− in the wear mechanism. Pressure dependence of the microwear behavior under aqueous electrolyte solutions has also been investigated. A microscopic removal mechanism, which is determined by interplay of the diffusion of water in Si and SiO2, is presented.

Ultrathin films (6–10 nm) of silver and nickel were deposited by pulsed laser deposition (PLD) in high vacuum (1 × 10−6 mbar). Microstructural evolution of these films as function of incident laser energy, substrate temperature, substrate material [borosilicate glass, fused silica, MgO(100) and Si (311)] and target–substrate distance was studied in detail using dynamic force microscopy. It is shown that with increase in laser energy incident on the target, there is a substantial increase in particle size in the film. The effect of increased laser energy on microstructure is much more drastic than that for the increase of substrate temperature. In general, denser packing of nanoparticles and increased clustering have been observed at elevated substrate temperature. Increase in laser energy gives rise to higher average grain size, packing density, and clustering in comparison to substrate temperature. It is observed that the aspect ratio of grains is dependent on incident laser fluence and substrate temperature, but more drastically on the substrate material. Substrate coverage and aspect ratio of the grains are particularly dependent on the nature of crystallinity of the substrates. It is demonstrated that PLD provides a greater degree of microstructural manipulation than other physical vapor deposition techniques.

We show that friction anisotropy is an intrinsic property of the atomic structure of Al–Ni–Co decagonal quasicrystals and not only of clean and well-ordered surfaces that can be prepared in vacuum [J.Y. Park et al., Science309, 1354 (2005)]. Friction anisotropy is manifested in both nanometer-size contacts obtained with sharp atomic force microscope tips and macroscopic contacts produced in pin-on-disk tribometers. We show that the friction anisotropy, which is not observed when an amorphous oxide film covers the surface, is recovered when the film is removed due to wear. Equally important is the loss of the friction anisotropy when the quasicrystalline order is destroyed due to cumulative wear. These results reveal the intimate connection between the mechanical properties of these materials and their peculiar atomic structure.

Much has been learned from electrochemical properties of boron-doped diamond (BDD) thin films synthesized using microwave plasma-assisted chemical vapor deposition about the factors influencing electrochemical activity, but some characteristics are still not entirely understood, such as its electrical conductivity in relation with microscale structure. Therefore, to effectively utilize these materials, understanding both the microscopic structure and physical (electrical, in particular) properties becomes indispensable. In addition to topography using atomic force microscopy, electrostatic force microscopy (EFM) in phase mode measuring the long-range electrostatic force gradients, helps to map the electrical conductivity heterogeneity of boron-doped micro-/nanocrystalline diamond surfaces. The mapping of electrical conductivity on boron doping and bias voltage is investigated. Experimental results showed that the BDD films’ surfaces were partially rougher with contrast of conductive regions (areas much less than 1 μm2 in diameter), which were uniformly distributed. Usually, the EFM signal is a convolution of topography and electrostatic force, and the phase contrast was increased with boron doping. At the highest boron doping level, the conductive regions exhibited quasi-metallic electrical properties. Moreover, the presence of a “positive–negative–positive” phase shift along the line section indicates the presence of “insulating–conducting–insulating” phases, although qualitative. Furthermore, the electrical properties, such as capacitance and dielectric constants at operating frequency, were quantitatively evaluated through modeling the bias-dependent phase measurements using simple and approximate geometries. It was found that decreasing grain size (or increasing the boron concentration) lowers the dielectric constant, which is attributed to the change in the crystal field caused by surface bond contraction of the nanosized crystallites. These findings are complemented and validated with scanning electron microscopy, x-ray diffraction, and “visible” Raman spectroscopy revealing their morphology, structure, and carbon-bonding configuration (sp3 versus sp2), respectively. These results are significant in the development of electrochemical nano-/microelectrodes and diamond-based electronics.

A new bulge testing setup for the measurement of the mechanical properties of thin films is presented. This self-built device can be incorporated in an atomic force microscope (AFM), which allows the recording of topographic images of the observed sample membranes under load conditions. Bulge test experiments on different silicon nitride films are presented and compared to nanoindentation experiments. The measured elastic moduli from nanoindentation and bulge testing are in good agreement. Apart from that, the ability to extract stress–strain data from AFM scans is shown, and the results are compared to standard bulge testing experiments. Imaging of the sample microstructure under load conditions is demonstrated on a thin Cu film.

Piezoresponse mode atomic force microscopy was used to induce a dynamic polarization reversal process and to characterize domain configuration behavior in BaMgF4 single crystal. Triangular reversed domains observed on the polar and non-polar surface demonstrate a sideways domain wall motion mechanism prevailing in the switching process of the bulk BaMgF4 crystal. The domain wall bowing phenomenon due to the strong pinning of the crystal defects was first visualized in the piezoresponse image of the engineering domain pattern in BaMgF4 crystal.

The secondary osteon is the fundamental building block of compact cortical bone at the tissue level. Light and scanning electron microscopy have shown that the osteon consists of a laminated cylindrical composite of mineralized collagen fibril lamellae ∼5–7 μm thick. Using scanning nanoindentation and quantitative backscattered electron imaging on secondary osteons from the human femoral midshaft, we found that the indentation modulus shows a periodic variation between ∼24 GPa and ∼27 GPa within a single lamella. The average lamellar value remains nearly constant across the osteon and increases abruptly to more than 30 GPa at the interstitial bone interface. The local mineral content, determined from quantitative backscattered electron imaging at the indented locations, shows also a lamellar level modulation and is positively correlated with the indentation modulus at the same tissue position. We propose that such a mechanically and compositionally modulated structure may be an effective crack-stopping mechanism in bone.

Spider silk is a material with unique mechanical properties under tension. In this study, we explore the anisotropic mechanical properties of spider silk using instrumented indentation. Both quasistatic indentation and dynamic stiffness imaging techniques were used to measure the mechanical properties in transverse and longitudinal sections of silk fibers. Quasistatic indentation yielded moduli of 10 ± 2 GPa in transverse sections and moduli of 6.4 ± 0.5 GPa in longitudinal sections, demonstrating mechanical anisotropy in the fiber. This result was supported by dynamic stiffness imaging, which also showed the average reduced modulus measured in the transverse section to be slightly higher than that of the longitudinal section. Stiffness imaging further revealed an oriented microstructure in the fiber, showing microfibrils aligned with the drawing axis of the fiber. No spatial distribution of modulus across the silk sections was observed by either quasistatic or stiffness imaging mechanics.

A single elastic modulus is not sufficient for describing the mechanical behavior of a living cell due to its viscoelastic nature and heterogeneity beneath the membrane. In this paper, the nanoscale elastic and viscoelastic behavior of individual living Chinese hamster ovary (CHO-K1) cells in a physiological environment were probed by atomic force microscopy (AFM) indentations at various loading rates. Based on Hertzian fits of the force–distance curves, the apparent elastic modulus of the cells was determined and found to be a function of the loading rate as well as the indentation depth. Notably, contributions from the substrate were negligible up to 50% of the cell thickness. For increased indentation rates and depths, healthy spindle-shaped CHO-K1 cells were found to exhibit an increased change of stiffness, whereas for unhealthy oval- shaped CHO-K1 cells there was little stiffening at equivalent loading rates and depths. Furthermore, a larger hysteresis between the loading and unloading curves was observed with increasing loading rates, which was related to the viscoelastic behavior of CHO-K1 cells. This work demonstrates differences in the rate- and depth-dependent elastic behavior at the nanoscale level between healthy and unhealthy mammalian cells.

Acquired salivary pellicle is a thin protein-rich film formed by the adsorption of saliva onto teeth. It plays important roles in lubrication during mastication and protecting the teeth from chemical attack. Pellicle can become colonized by bacteria to form dental plaque which can lead to dental caries if the bacteria are acidogenic. Abrasive polishing with a dentrifice is used periodically to remove the pellicle from teeth. Pellicle can interact with dietary polyphenolic compounds (tannins) to create extrinsic stains on the tooth surface. The staining can modify the pellicle's mechanical properties and change its morphology resulting in a “squeaky” feeling when the tongue is rubbed over the teeth. Atomic force microscopy imaging and nanoscale mechanical measurements show that unstained pellicle has a dense undulating morphology and is a surprisingly stiff, viscoelastic solid. In contrast, tannin-stained pellicle has fewer but larger surface undulations and exhibits substantial viscous creep.

In this paper, we describe the application of thin film combinatorial deposition methods to systematically control the microstructure of AlxSi(1−x) alloys through variations in composition and growth temperature. Discrete libraries of compositionally graded films have been sputter deposited onto silicon substrates to produce two structural phase regions: amorphous a-(Al–Si) and amorphous a-Si plus crystalline c-Al. The microstructure was investigated using x-ray diffraction while atomic force microscopy techniques were used to obtain surface morphology and phase distribution.