Nondestructive depth-resolved imaging of ∼20-nm-thick surface layers of soft polymeric materials is demonstrated using amplitude modulation atomic force microscopy (AM-AFM). From a map of amplitude-phase-distance curves, the tip indentation into the specimen is determined. This serves as a depth coordinate for reconstructing cross sections and volume images of the specimen's mechanical properties. Our method reveals subsurface structures which are not discernible using conventional AM-AFM. Results for surfaces of a block copolymer and a semicrystalline polymer are presented.
This paper reviews our recent work on vibrating sensors for the physical properties of fluids, particularly viscosity and density. Several device designs and the associated properties, specifically with respect to the sensed rheological domain and the onset of non-Newtonian behavior, are discussed.
Miniaturized liquid sensors are essential devices in online process or condition monitoring. In case of viscosity and density sensing, microacoustic sensors such as quartz crystal resonators or SAW devices have proved particularly useful. However, these devices basically measure a thin-film viscosity, which is often not comparable to the macroscopic parameters probed by conventional viscometers. Miniaturized cantilever-based devices are interesting alternatives for such applications, but here the interaction between the liquid and the oscillating beam is more involved. In our contribution, we describe a measurement setup, which allows the investigation of this interaction for different beam cross-sections. We present an analytical model based on an approximation of the immersed cantilever as an oscillating sphere comprising the effective mass and the intrinsic damping of the cantilever and additional mass and damping due to the liquid loading. The model parameters are obtained from measurements with well-known sample liquids by a curve fitting procedure. Finally, we present the measurement of viscosity and density of an unknown sample liquid, demonstrating the feasibility of the model.
High resolution volume images of semicrystalline polypropylene were obtained by stepwise wet-chemical etching followed by atomic force microscopy of the specimen. Enhanced signal-to-noise ratio and spatial resolution were achieved by using the second flexural eigenmode of the cantilever for phase imaging while the amplitude of the first mode was used as feedback signal. The energy dissipated between the tip and the sample revealed characteristic differences between the crystalline and the amorphous regions of the polypropylene after etching, indicating the presence of a thin (<10nm thick) amorphous layer on top of crystalline regions.
We developed MUSIC-mode atomic force microscopy (AFM)
to emulate
intermittent contact mode AFM without a feedback loop and in the absence
of lateral forces. This single-pass approach is based on maps of amplitude-phase-distance
curves and allows the height and phase images to be simultaneously
obtained for almost any amplitude set point. This is advantageous
for determining the shape and nanomechanical properties of very soft
and fragile samples. As an example, we studied supramolecular aggregates
of oligothiophenes, which form ≈15 nm wide fibrils with a rigid
core and a soft shell.
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