Hysteresis loop construction for the metal-semiconductor phase transition in vanadium dioxide films

Thermal hysteresis of the reflectivity of vanadium dioxide films observed upon the metal-semiconductor phase transition is studied. The major hysteresis loop is assumed to form when the phase equilibrium temperature in film grains and the grain size vary and correlate with each other. Within the suggested concept of hysteresis loop formation, it is demonstrated that the major loop may be asymmetric, i.e., broadened (shifted) toward lower temperatures. Unlike hysteresis branches for VO₂ bulk single crystal, those for VO₂ films are extended along the temperature axis and may exhibit a step if the grain size distribution has several maxima. The validity of the concept is verified experimentally. It is also shown that atomic force microscopy (AFM) data for the grain size distribution can serve to determine the distribution parameters from the phase equilibrium temperatures without constructing a complete set of minor hysteresis loops, as was required before.     

Photo-irradiation effects on the surface morphology of poly(p-phenylene vinylene) films

In this work, we have studied the surface morphology of photo-irradiated poly(p-phenylene vinylene) (PPV) thin films by using atomic force microscopy (AFM). We have analyzed the first-order statistical parameters, the height distribution and the distance between selected peaks. The second-order statistical analysis was introduced calculating the auto-covariance function to determine the correlation length between heights. We have observed that the photo-irradiation process produces a surface topology more homogeneous and isotropic such as a normal surface. In addition, the polymer surface irradiation can be used as a new methodology to obtain materials optically modified.     

Atomic force microscopy-based repeated machining theory for nanochannels on silicon oxide surfaces

The atomic force microscopy (AFM)-based repeated nanomachining of nanochannels on silicon oxide surfaces is investigated both theoretically and experimentally. The relationships of the initial nanochannel depth vs. final nanochannel depth at a normal force are systematically studied. Using the derived theory and simulation results, the final nanochannel depth can be predicted easily. Meanwhile, if a nanochannel with an expected depth needs to be machined, a right normal force can be selected simply and easily in order to decrease the wear of the AFM tip. The theoretical analysis and simulation results can be effectively used for AFM-based fabrication of nanochannels.     

Electrochemical,morphological, and spectroscopic study of poly(aniline-co-<Emphasis Type="Italic">o</Emphasis>-bromoaniline) (PA-co-<Emphasis Type="Italic">o</Emphasis>-BrA) conducting copolymer

A series of moderately conducting and soluble copolymers of poly(aniline-co-o-bromoaniline) (PA-co-o-BrA) having different compositions was obtained by in the situ copolymerization method using different concentrations of monomer units of aniline and o-bromoaniline in the feed. The physio-chemical properties of the copolymers have been studied with sophisticated instrumental techniques. The electrochemical study of the copolymers was conducted by cyclic voltammetry. The band gap of the highest occupied molecular orbital (HOMO) and lowest unoccupied molecular orbital (LUMO) of the copolymers was evaluated by UV-vis spectroscopy. The morphological study was conducted by scanning electron microscopy and transmission electron microscopy at high magnification which shows non-uniform tubular to globular morphology of the copolymers. Surface profiles of the polymers were studied by AFM analyses, and it has confirmed the smooth surface of the copolymers while the homopolymers possesses non-uniform surfaces. The particle size distribution curve indicates that the particle sizes vary in the range of 5 to 9000 nm, and a small fraction of particles possess a size in the range of 5–10 nm.     

Understanding tapping-mode atomic force microscopy data on the surface of soft block copolymers

In this paper, we focus on better understanding tapping-mode atomic force microscopy (AFM) data of soft block copolymer materials with regard to: (1) phase attribution; (2) the relationship between topography and inside structure; (3) contrast-reversal artifacts; (4) the influence of annealing treatment on topography. The experiments were performed on the surface of poly(styrene–ethylene/butylene–styrene) (SEBS) triblock copolymer acting as a model system. First, by coupling AFM with transmission electron microscopy (TEM) measurements, the phase attribution for AFM images was determined. Secondly, by imaging an atomically flat SEBS surface as well as an AFM tip-scratched SEBS surface, it was confirmed that the contrast in AFM height images of soft block copolymers is not necessarily the result of surface topography but the result of lateral differences in tip-indentation depth between soft and hard microdomains. It was also found that there is an enlarging effect in AFM images on the domain size of block copolymers due to the tip-indention mechanism. Thirdly, based on the tip-indention mechanism, tentative explanations in some detail for the observed AFM artifacts (a reversal in phase image followed by another reversal in height image) as function of imaging parameters were given. Last, it was demonstrated that the commonly used annealing treatments in AFM sample preparation of block copolymers may in some cases lead to a dramatic topography change due to the unexpected order-to-order structure transition.     

Identifying bacterial fragments on morphologically similar substrate using UAFM

The ultrasonic atomic force microscopy (UAFM) can be used effectively to map the elasticity of a surface. Using this technique we have demonstrated that biological fragments on a substrate can be easily identified which is otherwise difficult using only an AFM image. We have shown that AFM image can falsely interpret the surface morphological features on the substrate. We have taken the bacteria Pseudomonas sp. as a case study to demonstrate that UAFM technique is a powerful tool to study biological samples and differentiate morphological features on the substrate.     

Studying the structure of siloxane-urethane-ethylene oxide block copolymers

The structure of siloxane-urethane-ethylene oxide block copolymers is studied by means of atom force microscopy (AFM) and scanning electron microscopy (SEM). The degree of copolymer crystallinity is determined by X-ray diffraction. A correlation between the obtained results is established.     

Asymmetric magnetization reversal behavior and noncollinear anisotropies in exchange-bias system

The effect of noncollinearity between unidirectional and uniaxial anisotropies on asymmetric magnetization reversal of ferromagnet/antiferromagnet (FM/AFM) bilayer has been investigated. The results show the emergence of noncollinear anisotropies comes from the competition among applied magnetic field, magnetic anisotropy and exchange coupling in FM/AFM interface. The noncollinearity can lead to the asymmetry of hysteresis loop of FM/AFM bilayer. However, when the magnetic field is applied along the uniaxial anisotropy axis of FM layer, the hysteresis loop of FM/AFM bilayer is always symmetry independence of the noncollinear angle. Our results indicate that the asymmetry not only originates from the noncollinearity but also depends on the applied magnetic field orientation. Moreover, the asymmetry of hysteresis loop is always along with the appearance of unequivalence for magnetization reversal of FM/AFM bilayer, and there is a periodicity of π with orientation of applied field for its periodicity independence of the angle of the noncollinearity between the uniaxial and unidirectional anisotropies. The results can help us to open additional avenues to tailor the future advance magnetic device.     

Scanning near-field optical/atomic force microscopy for fluorescence imaging and spectroscopy of biomaterials in air and liquid: Observation of recombinantEscherichia coli with gene coding to green fluorescent protein

We have developed a system of scanning near-field optical/atomic force microscopy (SNOM/AFM) for fluorescence imaging and spectroscopy of biomaterials in air and liquid. SNOM/AFM uses a bent optical fiber simultaneously as a dynamic force AFM cantilever and a SNOM probe. Optical resolution of SNOM images shows about 50 nm in an illumination mode for a standard sample of a patterned chromium layer of 20 nm thickness on a quartz glass plate. The SNOM/AFM system contains a photon counting system and polychrometer/ICCD (intensified charge coupled device) system for observation of the fluorescence image and spectrograph of micro areas, respectively. The gene coding to green fluorescence protein (GFP) was cloned in recombinantEscherichia coli (E. coli). Topography, fluorescence image and spectrograph of recombinantE. coli by SNOM/AFM showed a difference in fluorescence in individualE. coli. Fluorescence activity of GFP can thus be used as a convenient indicator of transformation. SNOM/AFM is also applicable to observe immobilizedE. coli on a glass plate in water with a liquid chamber and may allow the viewing of observation of floating organisms.     

Investigation of phase separation in multiblock copolymers consisting of polysulfone and a liquid crystalline polymer

Multiblock copolymers (MBCPs) consisting of polysulfone (PSU) segments and segments of the liquid crystalline poly(ethyleneterephthalate-co-oxybenzoate) (PET/HBA) form rather complex morphologies. Scanning electron microscopy (SEM), small-angle X-ray scattering (SAXS), and atomic force microscopy (AFM) investigations of two block copolymers with significantly different block molecular weights proved the existence of both macro-and microphase separation. These morphologies, existing on different length scales, were found to be superimposed in the samples. A suitable fractionation procedure was used to suppress macrophase separation. Then, it was found that microphase separation is controlled by the segment molecular weights.     

Tribological properties of silicate materials on nano and microscale

We studied the friction properties of four model silicate materials at the nanoscale and microscale. From nanotribology, we characterized the tribological properties at single asperity contact scale and from microtribology, we characterized the tribological properties at multi asperity contact scale. First, for each material we measured chemical composition by XPS, Young's modulus by acoustical microscopy and roughness σ by atomic force microscopy (AFM). Second, we measured the nanofriction coefficients with an AFM and the microfriction coefficients with a ball probe tribometer, for three hardnesses of the ball probe. We identified one friction mechanism at the nanoscale (sliding friction) and two friction mechanisms at the microscale (sliding friction and yielding friction). Comparison of the nano and microfriction coefficients at the same sliding friction regime shown, that the tribological properties of these materials didn’t depend on roughness.     

Calibration of a scanning Joule expansion microscope (SJEM)

Scanning thermal microscopy (SThM) is a scanning probe technique based on atomic force microscopy (AFM) enabling high-resolution topographical imaging together with visualization of the temperature distribution in the studied sample. For the thermal mapping, rather expensive, micro-fabricated cantilevers with integrated thermocouples have to be used. The spatial resolution is typically limited to 100 nm. Scanning Joule expansion microscopy (SJEM) uses an alternative approach to detect the temperature of the sample with a regular silicon cantilever and lock-in detection. By monitoring the thermal expansion of the sample (due to Joule heating), the local temperature can be monitored. The resolution of SJEM is comparable to that of contact AFM, which is an order of magnitude better than for SThM. Our research involves implementing a SJEM for the study of heating phenomena in mesoscopic structures prepared by electron beam lithography and lift-off techniques. In particular, we calibrated our SJEM in order to make quantitative temperature maps of the studied samples.     

Microstructure, optical and static recording properties of AgOx film, and near-field simulation of sub-wavelength aperture based on the AgOx marks’ formation

Structures, spectra and surface topographies of as-deposited and annealed AgO_x films have been investigated by an X-ray diffractometer, a spectrophotometer and an atomic force microscopy (AFM). X-ray diffraction and spectrum results show that the as-deposited AgO_x films with high oxygen ratios (x≥0.5) are in amorphous states and Ag crystalline particles will separate out after annealed. AFM results show that the film surface will become much rougher and film thickness will increase greatly after annealed due to the decomposition of AgO_x with release of oxygen. Static recording results show that two microstructures of the recording marks can be produced: one is the bubble mark at a low recording power and the other is the rupture bubble with an ablated aperture (hole) in the center at a high recording power. Based on the formation of rupture bubble marks, the near-field optical distribution of a focused Gaussian laser beam through a sub-wavelength aperture (200 nm in diameter) has been simulated using finite-difference-time-domain (FDTD) method. Results show that the spot size can be greatly squeezed with still highly transmitted intensity, which may lead to the super-resolution readout.     

Numerical simulation of magnetization process in antiferromagnetic–ferromagnetic bilayer with compensated interface

The properties of antiferromagnetic (AFM)–ferromagnetic (FM) bilayer have been studied using self-consistent mean-field approximation for Heisenberg Hamiltonian. The perpendicular exchange coupling has been revealed in a bilayer with a compensated interface. For a uniform AFM film a symmetrical hysteresis loop has been calculated, because the transverse instability develops within the AFM film at certain critical value of external magnetic field. On the other hand, shifted hysteresis loop with a finite exchange bias field has been obtained for a non-uniform AFM film consisting of various AFM domains with perpendicular directions of the easy anisotropy axes.     

Structure and frictional properties of Langmuir-Blodgett films of Cu nanoparticles modified by dialkyldithiophosphate

Langmuir-Blodgett (LB) films of dialkyldithiophosphate (DDP) modified Cu nanoparticles were prepared. The structure, microfrictional behaviors and adhesion of the LB films were investigated by transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and atomic/friction force microscopy (AFM/FFM). Our results showed that the modified Cu nanoparticles have a typical core-shell structure and fine film-forming ability. The images of AFM/FFM showed that LB films of modified Cu nanoparticles were composed of many nanoparticles arranged closely and orderly and the nanoparticles had favorable behaviors of lower friction. The friction loop of the films indicated that the friction force was affected prominently by the surface slope of the Cu nanoparticles and the microfrictional behaviors showed obvious “ratchet effect”. The adhesion experiment showed that the modified Cu nanoparticle had a very small adhesive force.     

Scanning tunnelling microscopy imaging and modification of hydrogen-passivated Ge(100) surfaces

Scanning tunnelling microscopy (STM) study and modification of hydrogen (H)-passivated Ge(100) surfaces have been investigated. Thermal oxidation procedures were used to minimise surface roughness. Ge samples were passivated in HF solution after thermal oxidation. STM and atomic force microscope (AFM) imaging showed that, using HF etching after thermal oxidation, we can obtain a natural H-passivatedtopographically and chemically flat Ge(100) surface. The root-mean-square (rms) roughness ofa H-passivatedGe(100) surface measured both by STM and AFM is less than 2 ?. Electric properties of H-passivatedGe(100) surfaces were studied by scanning tunnelling spectroscopy (STS) in nitrogen ambient. STS showed that the H-passivated Ge surfaces were not pinned. Modification on H-passivated Ge(100) surfaces was carried out using STM by applying an electric voltage between the sample and tip in air. Modified features were characterised by STM and AFM imaging. On the H-passivated Ge(100) surfaces, stable, low-voltage, nanometer-scale modified features can be produced.     

Tip-surface interactions at redox responsive poly(ferrocenylsilane) (PFS) interface by AFM-based force spectroscopy

Poly(ferrocenylsilanes) (PFS) belong to the class of redox responsive organometallic polymers. Atomic force microscopy (AFM)-based single molecule force spectroscopy (SMFS) was used earlier to study single chain PFS response and redox energy driven single chain PFS molecular motors. Here we present further AFM investigations of force interactions between tip and a grafted PFS surface under potential control in electrochemical redox cycles. Typical tip-Au interaction is considered as reference in the force measurements. First the electrostatic component in the diffused double layer (DL) in NaClO₄ electrolyte environment was considered for a “grafted to” PFS, which dominated the interplay between the tip and sample surface. The DL forces can also hinder the physisorption of PFS chain onto the tip when the voltage was applied at −0.1 V. On the other hand, if the tip contacted the PFS surface prior to the electrochemical process, physisorption of PFS chains governed the overall interaction regardless of subsequently applied surface potential. In addition, prolonged contact time, t_c, may also contribute to the stability of tip-PFS bridging and detection of electrostatic forces between the tip-PFS interface. The results showed that tip-substrate interaction forces without PFS grafts have negligibly small force contributions under similar, electrochemically controlled, conditions used in single PFS chain based molecular motors.     

Mapping charge-mosaic surfaces in electrolyte solutions using surface charge microscopy

A significant limitation of electrokinetic measurements is that only an average value of the zeta potential/streaming potential is measured—regardless of whether the surface charge distribution is homogeneous or otherwise. However, in real-world situations, nearly all solids (and liquids) of technological significance exhibit surface heterogeneities. To detect heterogeneities in surface charge, analytical tools which provide accurate and spatially resolved information about material surface potential—particularly at microscopic and sub-microscopic resolutions—are needed.A novel AFM-based technique for mapping surface charge domains on heterogeneous surfaces, which we call Surface Charge Microscopy (SCM), was recently introduced by our research team. It relies on recording colloidal force curves over multiple locations on the substrate surface using small probes. The surface charge characteristics of the heterogeneous substrate are determined from the recorded colloidal force curves, allowing for the surface charge variation to be mapped. In this communication, we briefly review the SCM technique. Examples of results of measurements of the surface interaction forces that were recorded between a silicon nitride AFM cantilever and a multi-phase volcanic rock and heterogeneous surface of bitumen are also given.     

Size distribution and morphology of nascent soot in premixed ethylene flames with and without benzene doping

Particle size distribution functions of nascent soot formed in four burner-stabilized, premixed ethylene-oxygen-argon flames were studied in a spatially resolved manner by online sampling/scanning mobility particle sizer. Particle morphology was analyzed by atomic force microscopy (AFM) of substrate-deposited samples. Two of the four flames were doped with benzene. An aerosol electrometer is introduced to extend the lower detection limit to around 1.5 nm in diameter. The results show that the bimodal behavior of particle size is applicable to all premixed ethylene flames studied. The variation of the size distribution from flame to flame is conclusively attributed to flame temperature variation. Under the condition of an equal carbon concentration, benzene doping leads to negligible changes in the characteristics of the size distribution. For all flames studied, AFM observations show that nascent soot is liquid-like and spreads extensively upon impact on a substrate surface.     

Fractal analysis and atomic force microscopy measurements of surface roughness for Hastelloy C276 substrates and amorphous alumina buffer layers in coated conductors

In coated conductors, surface roughness of metallic substrates and buffer layers could significantly affect the texture of subsequently deposited buffer layers and the critical current density of superconductor layer. Atomic force microscopy (AFM) is usually utilized to measure surface roughness. However, the roughness values are actually relevant to scan scale. Fractal geometry could be exerted to analyze the scaling performance of surface roughness. In this study, four samples were prepared, which were electro polished Hastelloy C276 substrate, mechanically polished Hastelloy C276 substrate and the amorphous alumina buffer layers deposited on both the substrates by ion beam deposition. The surface roughness, described by root mean squared (RMS) and arithmetic average (R_a) values, was analyzed considering the scan scale of AFM measurements. The surfaces of amorphous alumina layers were found to be fractal in nature because of the scaling performance of roughness, while the surfaces of Hastelloy substrates were not. The flatten modification of AFM images was discussed. And the calculation of surface roughness in smaller parts divided from the whole AFM images was studied, compared with the results of actual AFM measurements of the same scan scales.