Tapping Mode Atomic Force Microscopy Phase Images Research Articles

Characterization of reliability of anti-soiling coatings using tapping mode-AFM phase imaging

Power loss due to dust deposition on photovoltaic (PV) modules (also referred to as soiling) is a severe challenge to the economic viability of PV deployment in sunbelt countries like India and the Middle East. Anti-soiling coatings are nano/micrometer thick transparent coatings, which mitigate dust deposition on PV module. In this study, Tapping Mode Atomic Force Microscopy (TM-AFM) phase imaging was used to characterize the surface changes of four different commercial hydrophobic anti-soiling coatings as they were subjected to outdoor field exposure tests and three different indoor accelerated stress tests. The anti-soiling coatings were applied via manual spray coating method on solar glass substrates. The phase angle for not-coated glass shows a tight distribution around zero. The phase angle distribution of coated surface showed a larger spread. When the coatings were subjected to different environmental stressors, the phase angle distributions became tighter and, in some cases, collapsed to tight distributions around zero, indicating that the coatings were partly or completely removed from the glass surface. We demonstrate a correlation of the changes in surface coverage identified from phase angle distributions to contact angle and surface roughness, thus establishing TM-AFM phase imaging as a promising approach to characterize anti-soiling coatings subjected to environmental stress. While the analysis of the phase angle distribution is able to resolve the removal of the coating, contact angle and surface roughness cannot do so unambiguously.

Polyurethane/poly(hydroxyethyl methacrylate) semi-interpenetrating polymer networks for biomedical applications

The thermodynamic miscibility, morphology, phase distribution, mechanical properties, surface properties, water sorption, bacterial adhesion and cytotoxicity of semi-interpenetrating polymer networks (semi-IPNs) based on crosslinked polyurethane (PU) and poly(hydroxyethylmethacrylate) (PHEMA) were studied to give an insight into their structure and properties. The free energies of mixing of the two polymers in semi-IPNs have been determined and it was shown that the values are positive and depend on the amount of PHEMA. This demonstrates that the components are immiscible, the extent of which is dependent upon variations in composition. The morphology of the semi-IPNs was analyzed with scanning electron microscopy and tapping mode atomic force microscopy (TMAFM). The micrographs of the semi-IPNs and TMAFM phase images indicated that distinct phase separation at the nanometer scale is observed. The mechanical properties reflect the changes in structure of semi-IPNs with composition. The stress at break increases from 3.4 MPa to 23.9 MPa, and the Young's modulus from 12.7 MPa up to 658.5 MPa with increasing amounts of PHEMA, but strain at break has a maximum at 40.4% PHEMA. The bacterial adhesion and cytotoxicity data suggest that semi-IPNs with PHEMA content above 22% may be used for biomedical material applications.

Blending of NR/BR/EPDM by reactive processing for tire sidewall applications. II. Characterization

AbstractCure incompatibility in NR/BR/EPDM blends is a crucial problem, affecting blend properties. In a previous study, it was demonstrated that the mechanical properties of such blends can be significantly improved by utilizing a reactive processing technique, in which a pretreated EPDM is first prepared by incorporating all compounding ingredients in the EPDM and subsequent preheating, prior to crossblending with premasticated NR/BR. In the present article, the pretreated EPDM‐moieties are prepared using two different accelerators, N‐cyclohexyl‐2‐benzothiazole sulfenamide (CBS) and 6‐nitro MBTS. The latter was synthesized and applied for the purpose of IR characterization. The infrared (IR) spectra of the pretreated, extracted EPDM demonstrate absorption peaks associated with the IR absorption of the functional groups in the accelerator fragments, attached to the EPDM. NR/BR/EPDM (35/35/30) ternary blends are prepared by reactive mixing of the pretreated EPDM with CBS fragments attached with premasticated NR/BR on a two‐roll mill. Their blend morphological features are studied using the atomic force microscopy (AFM) and transmission electron microscopy (TEM) microscopic techniques, in comparison with those of blends prepared by a conventional straight mixing method. Both the tapping mode AFM phase images and TEM micrographs clearly show that reactive mixing leads to more homogeneous blends. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 103:2547–2554, 2007

Electron holography and AFM studies on styrenic block copolymers and a high impact polystyrene

AbstractMany of the artifacts of conventional electron microscopy can be avoided if the unstained polymers are studied by electron holography and atomic force microscopy (AFM). Holograms of thin sections (50–70 nm) of organic block copolymers were recorded, and the corresponding phase images were reconstructed. In this way, typical structures such as lamellae and cylinders could be imaged without any staining. In addition, we successfully recorded holograms and performed Lorentz microscopy of an impact‐modified polystyrene (high‐impact polystyrene). The results were compared with the tapping mode AFM phase images. Electron holography and AFM have been demonstrated as suitable tools to image unstained heterogeneous polymers, leading to the understanding of their structure. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 96: 1573–1583, 2005

Feature Article: Tapping Mode Atomic Force Microscopy of Surface Morphology of Polymer Blends

Application of tapping mode atomic force microscopy (TMAFM) phase imaging techniques to characterize the morphology of polymeric blends is reviewed. The basic principle of TMAFM phase imaging capability is introduced. A summary of phase contrast applications for various polymeric blend systems such as rubber-rubber, plastic-rubber, and plastic-plastic blends is extensively discussed. The review shows that AFM is a very useful technique in probing micro-phase dispersion, compatibility between blend components, and local mechanical properties in polymeric blend systems.

Characterization of chemical heterogeneity in polymer systems using hydrolysis and tapping‐mode atomic force microscopy

AbstractCharacterization of polymer coatings microstructure is critical to the fundamental understanding of the corrosion of coated metals. An approach for mapping the chemical heterogeneity of a polymer system using chemical modification and tapping‐mode atomic force microscopy (TMAFM) is demonstrated. This approach is based on the selective degradation of one of the phases in a multiphase polymer blend system and the ability of TMAFM to provide nanoscale lateral information about the different phases in the polymer system. Films made of a 70:30 polyethyl acrylate/polystyrene (PEA/PS) blend were exposed to a hydrolytic acidic environment and analyzed using TMAFM. Pits were observed to form in the PEA/PS blend films, and this degradation behavior was similar to that of the PEA material. Using these results, the domains in the 70:30 blend were identified as the PS‐rich regions and the matrix as the PEA‐rich region. This conclusion was confirmed by Fourier transform infrared‐attenuated total reflection analyses that revealed the hydrolysis of the PEA material. TMAFM phase imaging was also used to follow pit growth of the blend as a function of exposure time. The usefulness of the chemical modification/AFM imaging approach in understanding the degradation process of a coating film is discussed. © 2001 John Wiley & Sons, Inc. J Polym Sci B Part B: Polym Phys 39: 1460–1470, 2001

Imaging of sub-surface nano particles by tapping-mode atomic force microscopy

Time-of-flight secondary ion mass spectrometry (ToF-SIMS), X-ray photoelectron spectroscopy (XPS), and tapping mode atomic force microscopy (TM-AFM) were used to study the surface of a poly( N-vinyl-2-pyrrolidone) thin film containing nano silica particles. ToF-SIMS results illustrate that the topmost layer of the thin film consists of PVP and a small amount of poly(dimethyl siloxane) (PDMS). Nano silica particles are localized underneath this layer. XPS results suggest that the concentration of the silica particles increases as the sampling depth increases from 5.3 to 7.2 nm. TM-AFM phase imaging is shown to be capable of detecting the presence of these sub-surface nano silica particles.

Examination of Butadiene/Styrene-co-butadiene Rubber Blends by Tapping Mode Atomic Force Microscopy. Importance of the Indentation Depth and Reduced Tip−Sample Energy Dissipation in Tapping Mode Atomic Force Microscopy Study of Elastomers

Tapping mode atomic force microscopy (TMAFM) measurements were performed for blends of two elastomers, cis-1,4-butadiene rubber (BR) and styrene-co-butadiene rubber (SBR) containing silica filler particles. To help interpret the TMAFM phase and height images of the BR/SBR blends, transmission electron microscopy (TEM) measurements were carried out for the BR/SBR blends, and dynamic mechanical analysis (DMA) as well as frequency-sweep/force-probe TMAFM measurements were carried out for BR and SBR homopolymers. TEM images show that silica filler particles of BR/SBR blends are present mainly in the SBR component, and DMA results reveal that BR has a lower glass transition temperature than does SBR. In the phase images of BR/SBR blends the less stiff component BR is brighter than is the stiffer component SBR. For the rational interpretation of TMAFM phase images of viscoelastic materials, it is crucial to consider the indentation depth of the tip into samples as well as the reduced tip−sample energy dissipati...

Characterization of the Morphologies and Nanostructures of Blends of Poly(styrene)-block-poly(ethene-co-but-1-ene)-block-poly(styrene) with Isotactic and Atactic Polypropylenes by Tapping-Mode Atomic Force Microscopy

Blends of poly(styrene)-block-poly(ethene-co-but-1-ene)-block-poly(styrene) (SEBS) with isotactic polypropylene (i-PP) and with atactic polypropylene (a-PP) were prepared under different thermal treatments. On the basis of the phase imaging of tapping-mode atomic force microscopy (TMAFM), we investigated the nanostructures and the morphologies of these blends as well as their dependence on blending history. The observed macrophase separation in i-PP/SEBS blends is caused by the incompatibility of the two polymer components. The microphase separation of the SEBS component depends on the thermal treatment. The morphology of a-PP/SEBS blends exhibits domains that span a wide range of sizes from 15 μm down to 15 nm. Our work shows that TMAFM phase imaging is an important and competitive tool for studying the microphase separation of polymers.