Abstract

Dynamic mechanical spectroscopy (DMS), which allows measuring frequency-dependent viscoelastic properties, is important to study soft materials, tissues, biomaterials, polymers. However, the existing DMS techniques (nanoindentation) have limited resolution when used on soft materials, preventing them from being used to study mechanics at the nanoscale. The nanoindenters are not capable of measuring cells, nanointerfaces of composite materials. Here we present a highly accurate DMS modality, which is a combination of three different methods: quantitative nanoindentation (nanoDMA), gentle force and fast response of atomic force microscopy (AFM), and Fourier transform (FT) spectroscopy. This new spectroscopy (which we suggest to call FT-nanoDMA) is fast and sensitive enough to allow DMS imaging of nanointerfaces, single cells, while attaining about 100x improvements on polymers in both spatial (to 10–70 nm) and temporal resolution (to 0.7s/pixel) compared to the current art. Multiple frequencies are measured simultaneously. The use of 10 frequencies are demonstrated here (up to 300 Hz which is a rather relevant range for biological materials and polymers, in both ambient conditions and liquid). The method is quantitatively verified on known polymers and demonstrated on cells and polymers blends. Analysis shows that FT-nanoDMA is highly quantitative. The FT-nanoDMA spectroscopy can easily be implemented in the existing AFMs.

Highlights

  • Total measurement time at one point of the surface Time to record 100 × 1 00 pixel map Ability to study individual biological cells Frequency range

  • The measurement time is fundamentally restricted by the need to wait for the creep relaxation to attain a stable contact, and quantitatively accurate measurements

  • The additional substantial acceleration comes from the fact that the decreased measurement time allows avoiding waiting for the creep relaxation, which is substantial for soft materials

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Summary

Minimum vertical indentation

Total measurement time at one point of the surface Time to record 100 × 1 00 pixel map Ability to study individual biological cells Frequency range. The measurement time is fundamentally restricted by the need to wait for the creep relaxation to attain a stable contact, and quantitatively accurate measurements This results in the measurement time per surface point (pixel) of the order of several minutes. We demonstrate recording maps of quantitative mechanical parameters for cells and polymers with lateral resolution of 50–70 nm (theoretical limit is estimated to be ~10 nm) and a temporal resolution of 0.7 sec per a point of the sample surface These values are better than the ones obtained on polymers with the state-of-the art nanoindenter (see, Table 1): 64–150x higher in lateral resolution and 200–280x faster in speed or temporal resolution. Those multifrequency techniques are based on a different physics (multiple resonance responses of the AFM cantilever) and do not allow measuring of DMS spectra for low frequencies

Results and Discussion
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