Atomic force microscopy (AFM) has evolved to be one of the most powerful tools for the characterization of material surfaces especially at the nanoscale. Recent development of AFM has incorporated a ...suite of analytical techniques including surface‐enhanced Raman scattering (SERS) technique and infrared (IR) spectroscopy to further reveal chemical composition and map the chemical distribution. This incorporation not only elevates the functionality of AFM but also increases the resolution limitation of conventional IR and Raman spectroscopy. Despite the rapid development of such hybrid AFM techniques, many unique features, principles, applications, potential pitfalls or artifacts are not well known to the community. This review systematically summarizes the recent relevant literature on hybrid AFM principles and applications. It focuses specially on AFM‐IR and AFM‐Raman techniques. Various applications in different research fields are critically reviewed and discussed, highlighting the potentials of these hybrid AFM techniques. Here, the major drawbacks and limitations of these two hybrid AFM techniques are presented. The intentions of this article are to shed new light on the future research and achieve improvements in stability and reliability of the measurements.
Hybrid atomic force microscopy (AFM) combines AFM with spectroscopic techniques such as infrared (IR), Raman and confocal. Hybrid AFM techniques can achieve nanoscale physicochemical characterization of material surfaces with high spatial resolutions. Recent developments and applications of hybrid AFM are summarized with a focus on AFM‐IR and AFM‐Raman and their existing drawbacks and limitations.
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BFBNIB, FZAB, GIS, IJS, KILJ, NLZOH, NUK, OILJ, SBCE, SBMB, UL, UM, UPUK
Poly(vinylidene fluoride-co-trifluoroethylene) (P(VDF-co-TrFE)) copolymer and poly(vinylidene fluoride-ter-trifluoroethylene-ter-chlorotrifluoroethylene) P(VDF-ter-TrFE-ter-CTFE) terpolymer thin ...films are usually produced by solvent-casting followed by annealing to enhance their electroactive properties in electronic devices. In this study, we investigate the effect of a different thermal treatment, namely crystallization from the melt, on the crystalline structure and morphology of P(VDF-ter-TrFE-ter-CTFE) terpolymers with varying CTFE content (ranging from 0 to 8.3 mol %) using a combination of different in-situ techniques. First, in-situ Wide-Angle X-Ray Scattering (WAXS) shows the different crystal-crystal transitions during cooling for all the samples. For the terpolymers, two sharp Bragg peaks ((110) and (200) family of planes) of the low temperature crystalline phase can be detected. Their sharpness reflects a high lateral extension of the crystalline domains. Moreover, coupled morphological studies by in-situ Small-Angle X-Ray Scattering (SAXS) and Atomic Force Microscopy (AFM) show that the crystallization starts with the formation of very extended semi-crystalline domains with a sub-micrometric thickness that contributes to the SAXS signal. For significant amounts of CTFE, crystallization is spread out, leading to the appearance of increasingly finer lamellar stacks during cooling, filling the spaces left unoccupied during crystallization at higher temperatures. This contrasts with the very rapid crystallization observed in the polymer with 0 mol % of CTFE. Finally, the Curie transition is clearly visible in the AFM mechanical images, providing an original method for detecting the structural transitions occurring in these polymers.
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•Structural/morphological study of the melt-crystallization of P(VDF-TrFE-CTFE).•Coupled in-situ WAXS, SAXS, and AFM analyses during cooling from the melt.•During crystallization, extended semi-crystalline domains (SCD) appear first.•The sub-micrometric thickness of the extended SCD induces a specific SAXS profile.•The Curie transition is surprisingly highlighted also in AFM mechanical images.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NLZOH, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UILJ, UL, UM, UPCLJ, UPUK, ZAGLJ, ZRSKP
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•A new approach to test inflammatory-induced corrosion of biomedical Ti was presented.•Corrosion was monitored in the PBS + H2O2 in the real-time using in situ AFM and AESEC.•Both ...oxide film growth and dissolution contributes to corrosion of commercially pure Ti.•Oxide film growth in PBS + H2O2 is suppressed for Ti-29Nb-13Ta-4.6Zr (TNTZ).•Roughness rather than chemical composition determines oxide film growth on TNTZ in PBS + H2O2.
This study offers a new approach to analyze surface behavior of titanium biomaterials during their exposure to the H2O2-enriched fluid which simulates post-operative inflammatory conditions. In this work in situ AFM and AESEC tests were exploited to study the origin of initial inflammatory-induced degradation for commercially pure Ti (CP-Ti) and Ti-29Nb-13Ta-4.6Zr (TNTZ) alloy. Overall results indicate that initial interaction between H2O2 and TNTZ surface results only in dissolution of the alloy, while for CP-Ti both oxide formation and dissolution give important contribution to the degradation process. Proposed methodology yields insight into the origin of corrosion properties registered during standard electrochemical tests that are used to evaluate biomaterials.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NLZOH, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UILJ, UL, UM, UPCLJ, UPUK, ZAGLJ, ZRSKP
The colloidal probe (CP) technique is an essential tool for quantitative direct force measurements by atomic force microscopy (AFM). By attaching a colloidal particle to the free end of an ...AFM-cantilever, not only a defined interaction geometry can be accomplished, but also a nearly arbitrary surface chemistry becomes possible. Commonly, the CP-technique is utilized for spherical particles in the sphere/sphere or sphere/plane interaction geometry. Here, the CP-technique has been extended to rod-shaped colloids with diameters well below one micrometer, thus preparing ‘rod probes’ based on a procedure similar to that known from DNA combing, allowing for a controlled alignment between these rods and the rod probe. In combination with AFM-imaging by the rod on the probe, sufficiently orthogonally aligned pairs of rods can be identified, and direct force measurements in the crossed-cylinder geometry, similar to the surface force apparatus (SFA), can be accomplished. A proof-of-concept of direct force measurements between silica rods with diameters of 270 ± 50 nm has been presented. The acquired interaction force profiles have been quantitatively evaluated within the framework of the full solutions of the Poisson-Boltzmann equation, including charge regulation.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NLZOH, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UILJ, UL, UM, UPCLJ, UPUK, ZAGLJ, ZRSKP
The corrosion inhibition performance of two pyrimidine derivatives namely 5-styryl-2,7-dithioxo-2,3,5,6,7,8-hexahydropyrimido4,5-d pyrimidin-4(1H) one (PP-1) and ...5-(2-hydroxyphenyl)-2,7-dithioxo-2,3,5,6,7,8-hexahydropyrimido4,5-d-pyrimidin-4(1H) one (PP-2) on N80 steel corrosion in 15% HCl has been studied using gravimetric method, electrochemical impedance spectroscopy (EIS), potentiodynamic polarization, atomic force microscopy (AFM), scanning electron microscopy (SEM), DFT, molecular electrostatic potential and Monte Carlo simulation. The corrosion inhibition efficiencies at optimum concentration (250mg/L) are 89.1% (PP-1) and 73.1% (PP-2) respectively at 308K. The corrosion inhibition efficiency increases with increase in concentration and decreases with temperature. PPs obeyed Langmuir adsorption isotherm. AFM and SEM analyses supported formation of protective film on N80 steel in presence of inhibitors. DFT and Monte Carlo simulation calculations supported experimental results.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UL, UM, UPCLJ, UPUK, ZRSKP
Supercritical carbon dioxide (ScCO2) fracturing technology has been increasingly emphasized in the development of unconventional oil and gas resources due to its advantages of anhydrous fabrication ...of complex seam networks and geological sequestration of CO2. However, previous studies have mostly focused on the geometry, number, and type of inorganic mineral fractures, and rarely paid attention to the changes in the seepage structure within organic matter (OM). To characterize the nanoscale microstructural changes of OM induced by H2O-ScCO2, this study obtained the variation rule of mechanical properties of OM with adsorbed water saturation based on nanoindentation test, and the continuous change of elastic modulus and morphology of the OM in the same region after dry, water-wet, and water-ScCO2 treatments was compared by atomic force microscopy (AFM). Elastic modulus and hardness of OM were calculated by Oliver-Pharr and Hertz methods, and the average roughness, root mean square roughness, and kurtosis were obtained based on 3D morphology. The results showed that elastic modulus and hardness were negatively and nonlinearly correlated with water saturation. Although the AFM-measured elastic modulus of OM microphases of the dry, water-wet, and water-ScCO2-treated shale were all highly discrete and non-homogeneous, they were generally normally distributed, and the mean values of the elastic modulus decreased sequentially. It is determined that water-ScCO2 coupling make OM matrix undergo superimposed dissolution. It is shown that ScCO2 and water synergistically change the microstructure of shale OM, and the weakening of mechanical properties and the increase of surface roughness are very favorable for geological sequestration and long-term storage of CO2.
•Young's modulus and hardness of organic matter showed a nonlinear negative correlation with water content.•Young's modulus and morphological changes of organic matter were analyzed at the nanoscale by in-situ AFM.•Water swelling decreased the roughness and Young's modulus of the organic matter.•The coupling of water and ScCO2 complicated the morphology and decreased Young's modulus of the organic matter.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NLZOH, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UILJ, UL, UM, UPCLJ, UPUK, ZAGLJ, ZRSKP
Nanostructural properties impacting ion and electron transfer processes at the electrolyte-electrode interface are of pivotal importance for the overall performance of rechargeable batteries such as ...sodium-ion batteries (SIBs). Compared to lithium-ion batteries (LIBs), less is known about the solid electrolyte interphase (SEI) formation at the negative electrode of SIBs. In this contribution, we present conductive atomic force microscopy (AFM), AFM-based nanomechanical mappings and AFM-scanning electrochemical microscopy (AFM-SECM) measurements addressing the interphase formation on hard carbon (HC) providing insight on the effect of additives like 4-fluoro-1,3-dioxolan-2-one (FEC) and the potential cumulative impact of the electrochemical and nanomechanical properties. The additive strongly influences the adhesion forces, whereas in contrast the Young's modulus appears significantly increased after cycling independent of an added additive to the electrolyte solution. AFM-SECM images before and after cycling clearly indicate the formation of an electrically insulating interphase layer. In addition, the effective heterogeneous rate constant of electron transfer was determined at single HC particles.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NLZOH, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UILJ, UL, UM, UPCLJ, UPUK, ZAGLJ, ZRSKP
This study explores the impact of 60 MeV N5+ ion irradiation on few layer WSe2 systems. The structural analysis exhibit an anomalous variation in crystallite size with increasing grain growth after ...irradiation. Raman spectroscopy study reveals increased disorder, enhanced intensities of prominent modes, and an eight-fold rise in AFM-measured roughness from 27.2 nm to 212.6 nm. HR-TEM shows voids in nanosheets post-irradiation. In addition, DFT calculations on monolayer with vacancy clusters shows modification of WSe2 bandgap from 1.48 eV to 0.37 eV. Interrelated structural, morphological and electronic structure calculations would provide useful insights upon controlled radiation exposure.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NLZOH, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UILJ, UL, UM, UPCLJ, UPUK, ZAGLJ, ZRSKP
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In this paper, the simple and low-cost water extraction way was used to acquisition Betel leaves extracts (BLE). The water as the extraction solvent has the characteristics of low ...price, environmentally friendly, and good solubility for other extraction solvents. BLE was researched as an environmental-friendly inhibitor via various experimental methods and theoretical calculations. Electrochemical experiments manifest that BLE can restrain reactions of the cathode and anode of Q235 steel. The BLE concentration was 400 mg/L, the anti-corrosion efficiency was close to 94%. The experimental data show that BLE can show high-quality anti-corrosion nature for Q235 steel immersing in 1 M hydrochloric acid (HCl) environment at a certain temperature range. The morphology maps of scanning electron microscope (SEM) and atomic force microscopy (AFM) strongly proves the data of electrochemical experiments. In addition, the BLE adsorption at the Q235 steel surface belongs to the Langmuir mono-layer adsorption. Quantum chemical calculations (QCC) and molecular dynamics simulations (MDS) effectually manifest that BLE can show decent anti corrosion character.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NLZOH, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UILJ, UL, UM, UPCLJ, UPUK, ZAGLJ, ZRSKP
Hydration layers are ubiquitous in life and technology. Hence, interfacial aqueous layers have a central role in a wide range of phenomena from materials science to molecular and cell biology. A ...complete understanding of those processes requires, among other things, the development of very-sensitive and high-resolution instruments. Three-dimensional atomic force microscopy (3D-AFM) represents the latest and most successful attempt to generate atomically resolved three-dimensional images of solid–liquid interfaces. This review provides an overview of the 3D-AFM operating principles and its underlying physics. We illustrate and explain the capability of the instrument to resolve atomic defects on crystalline surfaces immersed in liquid. We also illustrate some of its applications to imaging the hydration structures on DNA or proteins. In the last section, we discuss some perspectives on emerging applications in materials science and molecular biology.
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IJS, KILJ, NUK, PNG, UL, UM