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      Reflectance in AFM-IR: Implications for Interpretation and Remote Analysis of the Buried Interface

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          AFM-IR combines the chemical sensitivity of infrared spectroscopy with the lateral resolution of scanning probe microscopy, allowing nanoscale chemical analysis of almost any organic material under ambient conditions. As a result, this versatile technique is rapidly gaining popularity among materials scientists. Here, we report a previously overlooked source of data and artifacts in AFM-IR analysis; reflection from the buried interface. Periodic arrays of gold on glass are used to show that the overall signal in AFM-IR is affected by the wavelength-dependent reflectivity and thermal response of the underlying substrate. Excitingly, this demonstrates that remote analysis of heterogeneities at the buried interface is possible alongside that of an overlying organic film. On the other hand, AFM-IR users should carefully consider the composition and topography of underlying substrates when interpreting nanoscale infrared data. The common practice of generating ratio images, or indeed the normalization of AFM-IR spectra, should be approached with caution in the presence of substrate heterogeneity or variable sample thickness.

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          We describe ultraresolution microscopy far beyond the classical Abbe diffraction limit of one half wavelength (lambda/2), and also beyond the practical limit (ca. lambda/10) of aperture-based scanning near-field optical microscopy (SNOM). The 'apertureless' SNOM discussed here uses light scattering from a sharp tip (hence scattering-type or s-SNOM) and has no lambda-related resolution limit. Rather, its resolution is approximately equal to the radius a of the probing tip (for commercial tips, a < 20 nm) so that 10 nm is obtained in the visible (lambda/60). A resolution of lambda/500 has been obtained in the mid-infrared at lambda = 10 microm. The advantage of infrared, terahertz and even microwave illumination is that specific excitations can be exploited to yield specific contrast, e.g. the molecular vibration offering a spectroscopic fingerprint to identify chemical composition. S-SNOM can routinely acquire simultaneous amplitude and phase images to obtain information on refractive and absorptive properties. Plasmon- or phonon-resonant materials can be highlighted by their particularly high near-field signal level. Furthermore, s-SNOM can map the characteristic optical eigenfields of small, optically resonant particles. Lastly, we describe theoretical modelling that explains and predicts s-SNOM contrast on the basis of the local dielectric function.
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            AFM-IR: combining atomic force microscopy and infrared spectroscopy for nanoscale chemical characterization.

            Polymer and life science applications of a technique that combines atomic force microscopy (AFM) and infrared (IR) spectroscopy to obtain nanoscale IR spectra and images are reviewed. The AFM-IR spectra generated from this technique contain the same information with respect to molecular structure as conventional IR spectroscopy measurements, allowing significant leverage of existing expertise in IR spectroscopy. The AFM-IR technique can be used to acquire IR absorption spectra and absorption images with spatial resolution on the 50 to 100 nm scale, versus the scale of many micrometers or more for conventional IR spectroscopy. In the life sciences, experiments have demonstrated the capacity to perform chemical spectroscopy at the sub-cellular level. Specifically, the AFM-IR technique provides a label-free method for mapping IR-absorbing species in biological materials. On the polymer side, AFM-IR was used to map the IR absorption properties of polymer blends, multilayer films, thin films for active devices such as organic photovoltaics, microdomains in a semicrystalline polyhydroxyalkanoate copolymer, as well as model pharmaceutical blend systems. The ability to obtain spatially resolved IR spectra as well as high-resolution chemical images collected at specific IR wavenumbers was demonstrated. Complementary measurements mapping variations in sample stiffness were also obtained by tracking changes in the cantilever contact resonance frequency. Finally, it was shown that by taking advantage of the ability to arbitrarily control the polarization direction of the IR excitation laser, it is possible to obtain important information regarding molecular orientation in electrospun nanofibers.
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              Theory of infrared nanospectroscopy by photothermal induced resonance


                Author and article information

                Anal Chem
                Anal. Chem
                Analytical Chemistry
                American Chemical Society
                15 May 2020
                16 June 2020
                : 92
                : 12
                : 8117-8124
                []School of Materials, The University of Manchester , The Mill, Sackville St, Manchester M13 9PL, United Kingdom
                []AkzoNobel , Stoneygate Lane, Felling, Gateshead, Tyne and Wear NE10 0JY, United Kingdom
                Author notes
                [* ]Email: Suzanne.morsch@ . Tel: +44 161 306 2914.
                Copyright © 2020 American Chemical Society

                This is an open access article published under a Creative Commons Attribution (CC-BY) License, which permits unrestricted use, distribution and reproduction in any medium, provided the author and source are cited.

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                Analytical chemistry


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