The surface microtopographic observations and analyses of Izumiyama hydrothermal illite particles were made by utilizing tapping-mode atomic force microscopy (TMAFM). The Izumiyama illite particles showed platy to lath shapes. Platy particles exhibited various spiral growth patterns, i.e. circular, malformed circular, or polygonal single unit-cell layer spirals, polygonal parallel step spiral, or interlaced spiral patterns. The polygonal parallel step spiral and interlaced spiral patterns are formed by two single unit-cell layers rotated by 180° and 120° arising from a single screw dislocation point, respectively. The spiral patterns indicate that the illite particles have 1M, 2O and 2M1 polytypes. Lath-shaped particles show only interlacing patterns supporting the formation of 2M1 structures.

Particles showing circular or malformed circular spirals were found to be thinner and to have narrower step separations than particles showing polygonal spirals. Polygonal platy and lath-shaped particles showing interlaced patterns tended to be thicker and to have wider step separations than the other polygonal platy particles.

These results suggest that the Izumiyama illites crystallize as the result of a mechanism involving solution-mediated polytypes and spiral-type transformations of illite. The mechanism involves the Ostwald ripening process, i.e. a transformation of the polytype and spiral shape. The sequence of crystallization of the Izumiyama illite is: 1M circular spirals → 1M, 2O polygonal spirals → 2M1 polygonal spirals occurring during crystal growth and sequentially overgrowing on the initial particle surfaces. The super-saturation of the hydrothermal solution probably decreases gradually during the transformation, and this decrease may cause not only the transformation from a circular to a polygonal crystal morphology but also the development of a lath habit due to the inhibition of the growth rate in the [010] direction of the particle.

Atomic force microscopy (AFM) is a novel method for measuring changes in clay swelling in situ at the tactoid level in an aqueous environment. While the swelling process has been directly observed at the mesoscale level for multi-tactoid aggregates and the associated pores, no method to date has allowed the direct observation of swelling dynamics at the nanoscale. In initial proof-of-concept studies, individual tactoids of a Na-exchanged nontronite (NAu-1) were imaged in a solution of 5 mM NaCl. When multiple line profiles were examined on the same tactoid, the changes in height varied and depended on which layers of the profile were transected, and demonstrated that AFM analyses can be used to directly probe intratactoid heterogeneity in the swelling process. To better visualize this heterogeneity, a method was developed to restrict AFM images to include only the portions of a tactoid above a threshold height. A comparison of the changes in these images for multiple threshold values revealed that swelling in one part of a tactoid may occur simultaneously with compression in another portion, which suggests that the encroachment of layers into intra-tactoid micropores can partially compensate for the overall volume change. Finally, to demonstrate the ability of this technique to monitor in situ swelling changes as the surrounding aqueous environment is modified, a tactoid of K-montmorillonite (SWy-2) was monitored during cation exchange as a KCl solution was replaced with NaCl. After exchange, a transition from the crystalline swelling regime to the osmotic regime was observed. Subsequent height profiles were unchanged for a period of several hours and indicated that the AFM measurements were stable in the absence of changes to the aqueous phase composition. Because this technique is the first method that allows the swelling of a single tactoid to be monitored in an aqueous solution, it complements the ensemble-averaged data obtained from diffraction and scattering techniques.

The surging interest in manipulating the polarization of piezo/ferroelectric materials by means of light has driven an increasing number of studies toward their light-polarization interaction. One way to investigate such interaction is by performing piezoresponse force microscopy (PFM) while/after the sample is exposed to light illumination. However, caution must be exercised when analyzing and interpreting the data, as demonstrated in this paper, because sizeable photo-response observed in the PFM amplitude image of the sample is shown to be caused by the electrostatic interaction between the photo-induced surface charge and tip. Through photo-assisted Kelvin probe force microscopy (KPFM), positive surface potential is found to be developed near the sample's surface under 405 nm light illumination, whose effects on the measured PFM signal is revealed by the comparative studies on its amplitude curves that are obtained using PFM spectroscopy mode with/without illumination. This work exemplifies the need for complementary use of KPFM, PFM imaging mode, and PFM spectroscopy mode in order to distinguish real behavior from artifacts.

Atomic force microscopy (AFM) is a well-known tool for studying surface roughness and to collect depth information about features on the top atomic layers of samples. By combining secondary ion mass spectroscopy (SIMS) with focused ion beam (FIB) milling in a scanning electron microscope (SEM), chemical information of sputtered structures can be visualized and located with high lateral and depth resolution. In this paper, a high vacuum (HV) compatible AFM was installed in a TESCAN FIB-SEM instrument that was equipped with a time-of-flight SIMS (ToF-SIMS) detector. To calibrate the sputtering rate and measure the induced roughness caused by the ToF-SIMS analysis, subsequent AFM measurements were performed on an inorganic multilayer vertical cavity surface-emitting laser sample. Normalized sputtering rates were used to aid the accurate three-dimensional reconstruction of the sputtered volume's chemical composition. Achievable resolution, surface roughness during sputtering, and surface oxidation issues were analyzed. The integration of complementary detectors opens up the ability to determine the sample properties as well as to understand the influence of the Ga+ ion sputtering method on the sample surface during the analysis.

This overview is meant to help newer microscopists decide on an appropriate high-resolution method for nanoscale and microscale materials characterization. The operating principles, capabilities, and resolution of scanning electron microscopy (SEM) and atomic force microscopy (AFM), as well as the needs for sample preparation and the constraints imposed on the sample environment within the microscope, are compared and contrasted. This is followed by a similar assessment of the merits and challenges of transmission electron microscopy (TEM).

Atomic force microscopy (AFM) is used in a wide range of applications for imaging sub-nanometer resolution topography, as well as for analysis of physical characteristics (such as surface stiffness and electromagnetic properties). While surface imaging and characterization on the nanoscale is of great value and is widely used across all fields of science, correlation with other types of microscopy can greatly enhance the value of those measurements. Here, we discuss a new approach that uses a small, ultra-thin AFM, which allows it to be integrated with standard light microscopes. The authors believe the design will allow for a new paradigm in microscopy, by enabling all the advantages of AFM to be combined with the advanced imaging capabilities of research-grade light microscopes.

AFM-based nanoelectrical modes have numerous applications in fields ranging from semiconductors to biology. The data produced have traditionally been in the form of a 2D map, generated in contact mode, with a single electrical data point per XY location. Electrical ramps or spectra would be generated at a few, carefully selected locations. This article discusses a new approach to nanoelectrical imaging that creates an electrical data cube and a correlated nanomechanical data cube while operating at normal imaging speeds. This approach avoids contact mode imaging, thus extending electrical measurements to soft and fragile samples and improving measurement consistency. Moreover, this is a general approach that is applicable to most nanoelectrical modes and applications.

Determining and acting on thermo-physical properties at the nanoscale is essential for understanding/managing heat distribution in micro/nanostructured materials and miniaturized devices. Adequate thermal nano-characterization techniques are required to address thermal issues compromising device performance. Scanning thermal microscopy (SThM) is a probing and acting technique based on atomic force microscopy using a nano-probe designed to act as a thermometer and resistive heater, achieving high spatial resolution. Enabling direct observation and mapping of thermal properties such as thermal conductivity, SThM is becoming a powerful tool with a critical role in several fields, from material science to device thermal management. We present an overview of the different thermal probes, followed by the contribution of SThM in three currently significant research topics. First, in thermal conductivity contrast studies of graphene monolayers deposited on different substrates, SThM proves itself a reliable technique to clarify the intriguing thermal properties of graphene, which is considered an important contributor to improve the performance of downscaled devices and materials. Second, SThM’s ability to perform sub-surface imaging is highlighted by thermal conductivity contrast analysis of polymeric composites. Finally, an approach to induce and study local structural transitions in ferromagnetic shape memory alloy Ni–Mn–Ga thin films using localized nano-thermal analysis is presented.

On the basis of the suggestion that bone nanostructure bears “tissue age” information and may reflect surface deposition/modification processes, we performed nanoscale characterization of the external cortical bone surface at the femoral neck in women using atomic force microscopy (AFM). The specific aims were to assess age-related differences in bone nanostructure and explore the existence of nanostructural traces of potential bone apposition at this surface. Our findings revealed that the external cortical surface represents a continuous phase composed of densely packed mineral grains. Although the grains varied in size and shape, there was a domination of small grains indicative of freshly deposited bone (mean grain size: young, 35 nm; old, 37 nm; p > 0.05). Advanced quantitative analysis of surface morphological patterns revealed comparable roughness and complexity of the surface, suggesting a similar rate of mineral particle deposition at the surface in both groups. Calcium/phosphorus ratio, a measure of bone tissue age, was within the same range in both groups. In summary, our AFM analyses showed consistent nanostructural and compositional bone features, suggesting existence of new bone at the periosteal bone surface in both young and elderly women. Considering observed age-related increase in the neck diameter, AFM findings may support the theory of continuous bone apposition at the periosteal surface.

Carbon nanotubes (CNT) are proper tips for atomic force microscopes (AFMs) as a result of their small tip diameter, high aspect ratio, and high flexibility. For nanoscale imaging of soft biological specimens, a CNT tipped AFM is an ideal tool. In this article we review the application of CNTs as AFM tips and present related research about the forces applied from liquids on nanotubes. Then a dynamic mode CNT tipped AFM in liquid is modeled and simulated. The simulation results are compared with experimental results. For modeling and simulation, a continuous beam model and a forward-time simulation method are used. The simulation results show that when a CNT tip vibrates in liquid, the oscillation amplitude and resonance frequency are changed compared to the state of oscillation in air. The small structure of CNTs reduces the hydrodynamic forces, and the liquid environment reduces the adhesive forces between the CNT tip and the sample. These two factors make CNTs a good choice as an AFM tip.

A gray cast iron specimen was investigated by color and chemical etching with optical and atomic force microscopy, and the effect of grain orientation on the effectiveness of etching was examined. It was proven that the grain orientation dependence of chemical and color etching is just the opposite, and that the specimen surface after color etching is not uniformly smooth. Explanation for the layer structure of the color etched iron specimen is given.

The adsorption of humic acid (HA) onto highly ordered pyrolytic graphite (HOPG) surfaces at different concentrations has been studied by atomic force microscopy. When HA concentration was increased from 10 to 1,000 mg/L, HA can sequentially form spherical particles, layered structures, and connected blocks on HOPG surfaces. The findings of the layer structures and small amount of fine chains have been verified and discussed. When HA was acidified by addition of acetic acid, it changed into small rigid particles. These results indicated that HA can be considered as supramolecular associations of self-assembling heterogeneous and relatively small molecules, and a small amount of polymers. The present results are important for understanding HA molecular structures and their adsorption characteristic on carbonaceous surfaces.

Atomic force microscopy probe-induced large-area ultrathin SiOx (x ≡ O/Si content ratio and x > 2) protrusions only a few nanometers high on a SiO2 layer were characterized by scanning photoemission microscopy (SPEM) and X-ray photoemission spectroscopy (XPS). SPEM images of the large-area ultrathin SiOx protrusions directly showed the surface chemical distribution and chemical state specifications. The peak intensity ratios of the XPS spectra of the large-area ultrathin SiOx protrusions provided the elemental quantification of the Si 2p core levels and Si oxidation states (such as the Si4+, Si3+, Si2+, and Si1+ species). The O/Si content ratio (x) was evidently determined by the height of the large-area ultrathin SiOx protrusions.

Quantification of very low density molecular coatings on large (60 nm) gold nanoparticles (AuNPs) is demonstrated via the use of antibody-mediated self-limiting self-assembly of small and large AuNPs into raspberry-like structures subsequently imaged by atomic force microscopy (AFM). AFM imaging is proposed as an automated, lower-cost, higher-throughput alternative to immunostaining and imaging by transmission electron microscopy. Synthesis of large AuNPs, containing one of three ligand molecules in one of three stoichiometries (1, 2, or 10 ligands per AuNP), and small probe AuNPs with one of three antibody molecules in a one antibody per AuNP ratio, enabled a range of predicted self-limiting self-assembled structures. A model predicting the probability of observing a given small to large AuNP ratio based on a topography measurement such as AFM is described, in which random orientational deposition is assumed and which accounts for the stochastic synthesis method of the library AuNPs with varied ligand ratios. Experimental data were found to agree very well with the predictive models when using an established AFM sample preparation method that avoids drying-induced aggregation.

The product and direct role of the rssC gene of Serratia marcescens is unknown. For unraveling the role of the rssC gene, atomic force microscopy has been used to identify the surfaces of intact S. marcescens wild-type CH-1 cells and rssC mutant CH-1ΔC cells. The detailed surface topographies were directly visualized, and quantitative measurements of the physical properties of the membrane structures were provided. CH-1 and CH-1ΔC cells were observed before and after treatment with lysozyme, and their topography-related parameters, e.g., a valley-to-peak distance, mean height, surface roughness, and surface root-mean-square values, were defined and compared. The data obtained suggest that the cellular surface topography of mutant CH-1ΔC becomes rougher and more precipitous than that of wild-type CH-1 cells. Moreover, it was found that, compared with native wild-type CH-1, the cellular surface topography of lysozyme-treated CH-1 was not changed profoundly. The product of the rssC gene is thus predicted to be mainly responsible for fatty-acid biosynthesis of the S. marcescens outer membrane. This study represents the first direct observation of the structural changes in membranes of bacterial mutant cells and offers a new prospect for predicting gene expression in bacterial cells.

Adeno-associated virus (AAV) is a defective, nonpathogenic human parvovirus, which coinfects with a helper adenovirus or herpes virus. AAV's unique characteristics have made it an appealing vector system for gene delivery. AAV or recombinant AAV (rAAV) has been widely detected using negative stain transmission electron microscopy (TEM) but little has been detected using atomic force microscopy (AFM). In this article, we used AFM and TEM to observe the recombinant AAV-2 (rAAV-2) virus particles and applied statistical analysis to the AFM and TEM images. The results indicated that the rAAV-2 particle was a slightly elliptic particle close to round when it was detected by TEM (the mean length of major and minor axes of rAAV-2 particles was 24.77 ± 1.78 nm and 21.84 ± 1.57 nm, respectively), whereas when detected by AFM, the rAAV-2 particle was almost round. Even though the dimensions of the rAAV-2 particle exhibited a polymorphous distribution via off-line particle analysis of AFM, most of the rAAV-2 particles had a mean diameter of approximate 22.04 nm, which was similar to the results obtained by TEM. The results above suggested that AFM was important for accurately determining the average dimensions and distributions of virus particles.

With a vertical resolution of 0.1 nm, atomic force microscopy (AFM) height measurements can be used to determine accurately the diameter of single-walled carbon nanotubes (SWNT) with the assumption that they have circular cross sections. The aim of this article is to draw attention to the need to optimize operating parameters in tapping mode for quantitative AFM height (diameter) analysis of SWNTs. Using silicon tip/cantilever assemblies with force constants ranging from 0.9 to 40 N m−1, we examined the effect of applied force on the apparent diameter of SWNT wrapped with a 29-residue amphiphilic α-helical peptide. A decrease in apparent height (SWNT diameter) with increasing applied force was observed for the higher force constant cantilevers. Cantilevers having force constants of 0.9 and 3 N m−1 demonstrated minimal vertical sample compression with increasing applied force. The effects of AFM image pixel density and scan speed on the measured height (diameter) of SWNTs were also assessed.

Atomic force microscopy (AFM) is now well established among the tools of choice for the analysis and characterization of materials.Applications of AFM span many industries including chemicals, plastics, pharmaceuticals, and semiconductors.Advancements in AFM instrumentation over the last five years have expanded the range of application of this technology to investigate thermal and mechanical properties of complex materials at high spatial resolution as well as structural and morphological characterization of materials subjected to thermal and mechanical stresses.In particular, this has been an enabling technology for an improved understanding of structure–property relationships in polymeric materials including homopolymers, blends, impact-modified polymer systems, porous polymer systems, and semicrystalline polymers.Practical examples illustrate applications of contact, tapping-mode, phase-imaging, hot-stage, and scanning thermal methods for the characterization of modern industrial polymer materials.