Detection of secondary phases in duplex stainless steel by magnetic force microscopy and scanning Kelvin probe force microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ramírez-Salgado, J.; Domínguez-Aguilar, M.A., E-mail: madoming@imp.mx; Castro-Domínguez, B.

2013-12-15

The secondary phase transformations in a commercial super duplex stainless steel were investigated by micro-chemical analyses and high resolution scanning probe microscopy. Energy dispersive X-ray and electron probe detected ferrite and austenite as well as secondary phases in unetched aged duplex stainless steel type 25Cr-7Ni-3Mo. Volta potential indicated that nitride and sigma appeared more active than ferrite, while secondary austenite and austenite presented a nobler potential. Reversal order in nobility is thought to be attributable to the potential ranking provided by oxide nature diversity as a result of secondary phase surface compositions on steel. After eutectoid transformation, secondary austenite wasmore » detected by electron probe microanalysis, whereas atomic force microscopy distinguished this phase from former austenite by image contrast. Magnetic force microscopy revealed a “ghosted” effect on the latter microstructure probably derived from metal memory reminiscence of mechanical polishing at passivity and long range magnetic forces of ferrite phase. - Highlights: • Nobility detection of secondary phases by SKPFM in DSS particles is not a straightforward procedure. • As Volta potential and contrast are not always consistent SKPFM surface oxides is thought played an important role in detection. • AFM distinguished secondary austenite from former austenite by image contrast though SEM required EPMA.« less

Electrical characterization of grain boundaries of CZTS thin films using conductive atomic force microscopy techniques

DOE Office of Scientific and Technical Information (OSTI.GOV)

Muhunthan, N.; Singh, Om Pal; Toutam, Vijaykumar, E-mail: toutamvk@nplindia.org

2015-10-15

Graphical abstract: Experimental setup for conducting AFM (C-AFM). - Highlights: • Cu{sub 2}ZnSnS{sub 4} (CZTS) thin film was grown by reactive co-sputtering. • The electronic properties were probed using conducting atomic force microscope, scanning Kelvin probe microscopy and scanning capacitance microscopy. • C-AFM current flow mainly through grain boundaries rather than grain interiors. • SKPM indicated higher potential along the GBs compared to grain interiors. • The SCM explains that charge separation takes place at the interface of grain and grain boundary. - Abstract: Electrical characterization of grain boundaries (GB) of Cu-deficient CZTS (Copper Zinc Tin Sulfide) thin films wasmore » done using atomic force microscopic (AFM) techniques like Conductive atomic force microscopy (CAFM), Kelvin probe force microscopy (KPFM) and scanning capacitance microscopy (SCM). Absorbance spectroscopy was done for optical band gap calculations and Raman, XRD and EDS for structural and compositional characterization. Hall measurements were done for estimation of carrier mobility. CAFM and KPFM measurements showed that the currents flow mainly through grain boundaries (GB) rather than grain interiors. SCM results showed that charge separation mainly occurs at the interface of grain and grain boundaries and not all along the grain boundaries.« less

Force modulation and electrochemical gating of conductance in a cytochrome

NASA Astrophysics Data System (ADS)

Davis, Jason J.; Peters, Ben; Xi, Wang

2008-09-01

Scanning probe methods have been used to measure the effect of electrochemical potential and applied force on the tunnelling conductance of the redox metalloprotein yeast iso-1-cytochrome c (YCC) at a molecular level. The interaction of a proximal probe with any sample under test will, at this scale, be inherently perturbative. This is demonstrated with conductive probe atomic force microscopy (CP-AFM) current-voltage spectroscopy in which YCC, chemically adsorbed onto pristine Au(111) via its surface cysteine residue, is observed to become increasingly compressed as applied load is increased, with concomitant decrease in junction resistance. Electrical contact at minimal perturbation, where probe-molecule coupling is comparable to that in scanning tunnelling microscopy, brings with it the observation of negative differential resistance, assigned to redox-assisted probe-substrate tunnelling. The role of the redox centre in conductance is also resolved in electrochemical scanning tunnelling microscopy assays where molecular conductance is electrochemically gateable through more than an order of magnitude.

Characterization of magnetic force microscopy probe tip remagnetization for measurements in external in-plane magnetic fields

DOE Office of Scientific and Technical Information (OSTI.GOV)

Weis, Tanja; Engel, Dieter; Ehresmann, Arno

2008-12-15

A quantitative analysis of magnetic force microscopy (MFM) images taken in external in-plane magnetic fields is difficult because of the influence of the magnetic field on the magnetization state of the magnetic probe tip. We prepared calibration samples by ion bombardment induced magnetic patterning with a topographically flat magnetic pattern magnetically stable in a certain external magnetic field range for a quantitative characterization of the MFM probe tip magnetization in point-dipole approximation.

Growth of carbon nanofibers on tipless cantilevers: process development and applications in scanning probe microscopy

NASA Astrophysics Data System (ADS)

Cui, Hongtao; Kalinin, Sergei; Yang, Xiaojing; Lowndes, Douglas

2005-03-01

Carbon nanofibers (CNFs) are grown on tipless cantilevers as probe tips for scanning probe microscopy. A catalyst dot pattern is formed on the surface of the tipless cantilever using electron beam lithography and CNF growth is performed in a direct-current plasma enhanced chemical vapor deposition reactor. Because the CNF is aligned with the electric field near the edge of the cantilever during growth, it is tilted with respect to the cantilever surface, which compensates partially for the probe tilt introduced when used in scanning probe microscopy. CNFs with different shapes and tip radii can be produced by variation of experimental conditions. The tip geometries of the CNF probes are defined by their catalyst particles, whose magnetic nature also imparts a capability for imaging magnetic samples. We have demonstrated their use in both atomic force and magnetic force surface imaging. These probe tips may provide information on magnetic phenomena at the nanometer scale in connection with the drive for ever-increasing storage density of magnetic hard disks.

Distributed force probe bending model of critical dimension atomic force microscopy bias

NASA Astrophysics Data System (ADS)

Ukraintsev, Vladimir A.; Orji, Ndubuisi G.; Vorburger, Theodore V.; Dixson, Ronald G.; Fu, Joseph; Silver, Rick M.

2013-04-01

Critical dimension atomic force microscopy (CD-AFM) is a widely used reference metrology technique. To characterize modern semiconductor devices, small and flexible probes, often 15 to 20 nm in diameter, are used. Recent studies have reported uncontrolled and significant probe-to-probe bias variation during linewidth and sidewall angle measurements. To understand the source of these variations, tip-sample interactions between high aspect ratio features and small flexible probes, and their influence on measurement bias, should be carefully studied. Using theoretical and experimental procedures, one-dimensional (1-D) and two-dimensional (2-D) models of cylindrical probe bending relevant to carbon nanotube (CNT) AFM probes were developed and tested. An earlier 1-D bending model was refined, and a new 2-D distributed force (DF) model was developed. Contributions from several factors were considered, including: probe misalignment, CNT tip apex diameter variation, probe bending before snapping, and distributed van der Waals-London force. A method for extracting Hamaker probe-surface interaction energy from experimental probe-bending data was developed. Comparison of the new 2-D model with 1-D single point force (SPF) model revealed a difference of about 28% in probe bending. A simple linear relation between biases predicted by the 1-D SPF and 2-D DF models was found. The results suggest that probe bending can be on the order of several nanometers and can partially explain the observed CD-AFM probe-to-probe variation. New 2-D and three-dimensional CD-AFM data analysis software is needed to take full advantage of the new bias correction modeling capabilities.

Examination of biogenic selenium-containing nanosystems based on polyelectrolyte complexes by atomic force, Kelvin probe force and electron microscopy methods

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sukhanova, T. E., E-mail: tat-sukhanova@mail.ru; Vylegzhanina, M. E.; Valueva, S. V.

The morphology and electrical properties of biogenic selenium-containing nanosystems based on polyelectrolyte complexes (PECs) were examined using AFM, Kelvin Probe Force and electron microscopy methods. It has been found, that prepared nanostructures significantly differed in their morphological types and parameters. In particular, multilayers capsules can be produced via varying synthesis conditions, especially, the selenium–PEC mass ratio ν. At the “special point” (ν = 0.1), filled and hollow nano- and microcapsules are formed in the system. The multilayer character of the capsules walls is visible in the phase images. Kelvin Probe Force images showed the inhomogeneity of potential distribution in capsulesmore » and outside them.« less

Cross-Sectional Investigations on Epitaxial Silicon Solar Cells by Kelvin and Conducting Probe Atomic Force Microscopy: Effect of Illumination.

PubMed

Narchi, Paul; Alvarez, Jose; Chrétien, Pascal; Picardi, Gennaro; Cariou, Romain; Foldyna, Martin; Prod'homme, Patricia; Kleider, Jean-Paul; I Cabarrocas, Pere Roca

2016-12-01

Both surface photovoltage and photocurrent enable to assess the effect of visible light illumination on the electrical behavior of a solar cell. We report on photovoltage and photocurrent measurements with nanometer scale resolution performed on the cross section of an epitaxial crystalline silicon solar cell, using respectively Kelvin probe force microscopy and conducting probe atomic force microscopy. Even though two different setups are used, the scans were performed on locations within 100-μm distance in order to compare data from the same area and provide a consistent interpretation. In both measurements, modifications under illumination are observed in accordance with the theory of PIN junctions. Moreover, an unintentional doping during the deposition of the epitaxial silicon intrinsic layer in the solar cell is suggested from the comparison between photovoltage and photocurrent measurements.

In-Process Atomic-Force Microscopy (AFM) Based Inspection

PubMed Central

Mekid, Samir

2017-01-01

A new in-process atomic-force microscopy (AFM) based inspection is presented for nanolithography to compensate for any deviation such as instantaneous degradation of the lithography probe tip. Traditional method used the AFM probes for lithography work and retract to inspect the obtained feature but this practice degrades the probe tip shape and hence, affects the measurement quality. This paper suggests a second dedicated lithography probe that is positioned back-to-back to the AFM probe under two synchronized controllers to correct any deviation in the process compared to specifications. This method shows that the quality improvement of the nanomachining, in progress probe tip wear, and better understanding of nanomachining. The system is hosted in a recently developed nanomanipulator for educational and research purposes. PMID:28561747

DC thermal microscopy: study of the thermal exchange between a probe and a sample

NASA Astrophysics Data System (ADS)

Gomès, Séverine; Trannoy, Nathalie; Grossel, Philippe

1999-09-01

The Scanning Thermal Microscopic (SThM) probe, a thin Pt resistance wire, is used in the constant force mode of an Atomic Force Microscope (AFM). Thermal signal-distance curves for differing degrees of relative humidity and different surrounding gases demonstrate how heat is transferred from the heated probe to the sample. It is known that water affects atomic force microscopy and thermal measurements; we report here on the variation of the water interaction on the thermal coupling versus the probe temperature. Measurements were taken for several solid materials and show that the predominant heat transfer mechanisms taking part in thermal coupling are dependent on the thermal conductivity of the sample. The results have important implications for any quantitative interpretation of thermal images made in air.

Crystallographic order and decomposition of [MnIII 6CrIII]3+ single-molecule magnets deposited in submonolayers and monolayers on HOPG studied by means of molecular resolved atomic force microscopy (AFM) and Kelvin probe force microscopy in UHV

NASA Astrophysics Data System (ADS)

Gryzia, Aaron; Volkmann, Timm; Brechling, Armin; Hoeke, Veronika; Schneider, Lilli; Kuepper, Karsten; Glaser, Thorsten; Heinzmann, Ulrich

2014-02-01

Monolayers and submonolayers of [Mn III 6 Cr III ] 3+ single-molecule magnets (SMMs) adsorbed on highly oriented pyrolytic graphite (HOPG) using the droplet technique characterized by non-contact atomic force microscopy (nc-AFM) as well as by Kelvin probe force microscopy (KPFM) show island-like structures with heights resembling the height of the molecule. Furthermore, islands were found which revealed ordered 1D as well as 2D structures with periods close to the width of the SMMs. Along this, islands which show half the heights of intact SMMs were observed which are evidences for a decomposing process of the molecules during the preparation. Finally, models for the structure of the ordered SMM adsorbates are proposed to explain the observations.

Quantification of in-contact probe-sample electrostatic forces with dynamic atomic force microscopy.

PubMed

Balke, Nina; Jesse, Stephen; Carmichael, Ben; Okatan, M Baris; Kravchenko, Ivan I; Kalinin, Sergei V; Tselev, Alexander

2017-01-04

Atomic force microscopy (AFM) methods utilizing resonant mechanical vibrations of cantilevers in contact with a sample surface have shown sensitivities as high as few picometers for detecting surface displacements. Such a high sensitivity is harnessed in several AFM imaging modes. Here, we demonstrate a cantilever-resonance-based method to quantify electrostatic forces on a probe in the probe-sample junction in the presence of a surface potential or when a bias voltage is applied to the AFM probe. We find that the electrostatic forces acting on the probe tip apex can produce signals equivalent to a few pm of surface displacement. In combination with modeling, the measurements of the force were used to access the strength of the electrical field at the probe tip apex in contact with a sample. We find an evidence that the electric field strength in the junction can reach ca. 1 V nm -1 at a bias voltage of a few volts and is limited by non-ideality of the tip-sample contact. This field is sufficiently strong to significantly influence material states and kinetic processes through charge injection, Maxwell stress, shifts of phase equilibria, and reduction of energy barriers for activated processes. Besides, the results provide a baseline for accounting for the effects of local electrostatic forces in electromechanical AFM measurements as well as offer additional means to probe ionic mobility and field-induced phenomena in solids.

Molecular Imaging of Ultrathin Pentacene Films: Evidence for Homoepitaxy

NASA Astrophysics Data System (ADS)

Wu, Yanfei; Haugstad, Greg; Frisbie, C. Daniel

2013-03-01

Ultrathin polycrystalline films of organic semiconductors have received intensive investigations due to the critical role they play in governing the performance of organic thin film transistors. In this work, a variety of scanning probe microscopy (SPM) techniques have been employed to investigate ultrathin polycrystalline films (1-3 nm) of the benchmark organic semiconductor pentacene. By using spatially resolved Friction Force Microscopy (FFM), Kelvin Probe Force Microscopy (KFM) and Electrostatic Force Microscopy (EFM), an interesting multi-domain structure is revealed within the second layer of the films, characterized as two distinct friction and surface potential domains correlating with each other. The existence of multiple homoepitaxial modes within the films is thus proposed and examined. By employing lattice-revolved imaging using contact mode SPM, direct molecular evidence for the unusual homoepitaxy is obtained.

Identification of nanoparticles and nanosystems in biological matrices with scanning probe microscopy.

PubMed

Angeloni, Livia; Reggente, Melania; Passeri, Daniele; Natali, Marco; Rossi, Marco

2018-04-17

Identification of nanoparticles and nanosystems into cells and biological matrices is a hot research topic in nanobiotechnologies. Because of their capability to map physical properties (mechanical, electric, magnetic, chemical, or optical), several scanning probe microscopy based techniques have been proposed for the subsurface detection of nanomaterials in biological systems. In particular, atomic force microscopy (AFM) can be used to reveal stiff nanoparticles in cells and other soft biomaterials by probing the sample mechanical properties through the acquisition of local indentation curves or through the combination of ultrasound-based methods, like contact resonance AFM (CR-AFM) or scanning near field ultrasound holography. Magnetic force microscopy can detect magnetic nanoparticles and other magnetic (bio)materials in nonmagnetic biological samples, while electric force microscopy, conductive AFM, and Kelvin probe force microscopy can reveal buried nanomaterials on the basis of the differences between their electric properties and those of the surrounding matrices. Finally, scanning near field optical microscopy and tip-enhanced Raman spectroscopy can visualize buried nanostructures on the basis of their optical and chemical properties. Despite at a still early stage, these methods are promising for detection of nanomaterials in biological systems as they could be truly noninvasive, would not require destructive and time-consuming specific sample preparation, could be performed in vitro, on alive samples and in water or physiological environment, and by continuously imaging the same sample could be used to dynamically monitor the diffusion paths and interaction mechanisms of nanomaterials into cells and biological systems. This article is categorized under: Diagnostic Tools > In Vivo Nanodiagnostics and Imaging Nanotechnology Approaches to Biology > Nanoscale Systems in Biology. © 2018 Wiley Periodicals, Inc.

VEDA: a web-based virtual environment for dynamic atomic force microscopy.

PubMed

Melcher, John; Hu, Shuiqing; Raman, Arvind

2008-06-01

We describe here the theory and applications of virtual environment dynamic atomic force microscopy (VEDA), a suite of state-of-the-art simulation tools deployed on nanoHUB (www.nanohub.org) for the accurate simulation of tip motion in dynamic atomic force microscopy (dAFM) over organic and inorganic samples. VEDA takes advantage of nanoHUB's cyberinfrastructure to run high-fidelity dAFM tip dynamics computations on local clusters and the teragrid. Consequently, these tools are freely accessible and the dAFM simulations are run using standard web-based browsers without requiring additional software. A wide range of issues in dAFM ranging from optimal probe choice, probe stability, and tip-sample interaction forces, power dissipation, to material property extraction and scanning dynamics over hetereogeneous samples can be addressed.

Invited Article: VEDA: A web-based virtual environment for dynamic atomic force microscopy

NASA Astrophysics Data System (ADS)

Melcher, John; Hu, Shuiqing; Raman, Arvind

2008-06-01

We describe here the theory and applications of virtual environment dynamic atomic force microscopy (VEDA), a suite of state-of-the-art simulation tools deployed on nanoHUB (www.nanohub.org) for the accurate simulation of tip motion in dynamic atomic force microscopy (dAFM) over organic and inorganic samples. VEDA takes advantage of nanoHUB's cyberinfrastructure to run high-fidelity dAFM tip dynamics computations on local clusters and the teragrid. Consequently, these tools are freely accessible and the dAFM simulations are run using standard web-based browsers without requiring additional software. A wide range of issues in dAFM ranging from optimal probe choice, probe stability, and tip-sample interaction forces, power dissipation, to material property extraction and scanning dynamics over hetereogeneous samples can be addressed.

Three-dimensional atomic force microscopy mapping at the solid-liquid interface with fast and flexible data acquisition

DOE Office of Scientific and Technical Information (OSTI.GOV)

Söngen, Hagen, E-mail: soengen@uni-mainz.de; Graduate School Materials Science in Mainz, Staudinger Weg 9, 55128 Mainz; Nalbach, Martin

2016-06-15

We present the implementation of a three-dimensional mapping routine for probing solid-liquid interfaces using frequency modulation atomic force microscopy. Our implementation enables fast and flexible data acquisition of up to 20 channels simultaneously. The acquired data can be directly synchronized with commercial atomic force microscope controllers, making our routine easily extendable for related techniques that require additional data channels, e.g., Kelvin probe force microscopy. Moreover, the closest approach of the tip to the sample is limited by a user-defined threshold, providing the possibility to prevent potential damage to the tip. The performance of our setup is demonstrated by visualizing themore » hydration structure above the calcite (10.4) surface in water.« less

Probing Membrane Order and Topography in Supported Lipid Bilayers by Combined Polarized Total Internal Reflection Fluorescence-Atomic Force Microscopy

PubMed Central

Oreopoulos, John; Yip, Christopher M.

2009-01-01

Determining the local structure, dynamics, and conformational requirements for protein-protein and protein-lipid interactions in membranes is critical to understanding biological processes ranging from signaling to the translocating and membranolytic action of antimicrobial peptides. We report here the application of a combined polarized total internal reflection fluorescence microscopy-in situ atomic force microscopy platform. This platform's ability to image membrane orientational order was demonstrated on DOPC/DSPC/cholesterol model membranes containing the fluorescent membrane probe, DiI-C20 or BODIPY-PC. Spatially resolved order parameters and fluorophore tilt angles extracted from the polarized total internal reflection fluorescence microscopy images were in good agreement with the topographical details resolved by in situ atomic force microscopy, portending use of this technique for high-resolution characterization of membrane domain structures and peptide-membrane interactions. PMID:19254557

Subatomic-scale force vector mapping above a Ge(001) dimer using bimodal atomic force microscopy

NASA Astrophysics Data System (ADS)

Naitoh, Yoshitaka; Turanský, Robert; Brndiar, Ján; Li, Yan Jun; Štich, Ivan; Sugawara, Yasuhiro

2017-07-01

Probing physical quantities on the nanoscale that have directionality, such as magnetic moments, electric dipoles, or the force response of a surface, is essential for characterizing functionalized materials for nanotechnological device applications. Currently, such physical quantities are usually experimentally obtained as scalars. To investigate the physical properties of a surface on the nanoscale in depth, these properties must be measured as vectors. Here we demonstrate a three-force-component detection method, based on multi-frequency atomic force microscopy on the subatomic scale and apply it to a Ge(001)-c(4 × 2) surface. We probed the surface-normal and surface-parallel force components above the surface and their direction-dependent anisotropy and expressed them as a three-dimensional force vector distribution. Access to the atomic-scale force distribution on the surface will enable better understanding of nanoscale surface morphologies, chemical composition and reactions, probing nanostructures via atomic or molecular manipulation, and provide insights into the behaviour of nano-machines on substrates.

Electromechanical response of amorphous LaAlO{sub 3} thin film probed by scanning probe microscopies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Borowiak, Alexis S.; Baboux, Nicolas; Albertini, David

The electromechanical response of a 3 nm thick amorphous LaAlO{sub 3} layer obtained by molecular beam epitaxy has been studied using scanning probe microscopies. Although this kind of sample is not ferroelectric due to its amorphous nature, the resulting images are identical to what is generally obtained on truly ferroelectric samples probed by piezoresponse force microscopy: domains of apparently opposite polarisation are detected, and perfect, square shaped hysteresis loops are recorded. Moreover, written patterns are stable within 72 h. We discuss in the general case the possible origins of this behaviour in terms of charge injection, ionic conduction and motion ofmore » oxygen vacancies. In the case presented in this paper, since the writing process has been conducted with applied voltages lower than the injection threshold measured by conductive atomic force Microscopy, allowing to withdraw the hypothesis of charge injection in the sample, we propose that a bistable distribution of oxygen vacancies is responsible for this contrast.« less

Electromechanical response of amorphous LaAlO3 thin film probed by scanning probe microscopies

NASA Astrophysics Data System (ADS)

Borowiak, Alexis S.; Baboux, Nicolas; Albertini, David; Vilquin, Bertrand; Saint Girons, Guillaume; Pelloquin, Sylvain; Gautier, Brice

2014-07-01

The electromechanical response of a 3 nm thick amorphous LaAlO3 layer obtained by molecular beam epitaxy has been studied using scanning probe microscopies. Although this kind of sample is not ferroelectric due to its amorphous nature, the resulting images are identical to what is generally obtained on truly ferroelectric samples probed by piezoresponse force microscopy: domains of apparently opposite polarisation are detected, and perfect, square shaped hysteresis loops are recorded. Moreover, written patterns are stable within 72 h. We discuss in the general case the possible origins of this behaviour in terms of charge injection, ionic conduction and motion of oxygen vacancies. In the case presented in this paper, since the writing process has been conducted with applied voltages lower than the injection threshold measured by conductive atomic force Microscopy, allowing to withdraw the hypothesis of charge injection in the sample, we propose that a bistable distribution of oxygen vacancies is responsible for this contrast.

Magnetic resonance force microscopy with a paramagnetic probe

DOE Office of Scientific and Technical Information (OSTI.GOV)

Berman, G. P.; Gorshkov, V. N.; Tsifrinovich, V. I.

Here, we consider theoretically extension of magnetic resonance force microscopy (MRFM) replacing a ferromagnetic probe on a cantilever tip (CT) with a paramagnetic one (PMRFM). The dynamics of the interaction between the paramagnetic probe and a local magnetic moment in a sample is analyzed, using a quasi-classical approach. We show that the application of a proper sequence of electromagnetic pulses provides a significant deflection of the CT from the initial equilibrium position. Periodic application of these sequences of pulses results in quasi-periodic CT deflections from the equilibrium, which can be used for detection of the magnetic moment in a sample.

Magnetic resonance force microscopy with a paramagnetic probe

NASA Astrophysics Data System (ADS)

Berman, G. P.; Gorshkov, V. N.; Tsifrinovich, V. I.

2017-04-01

We consider theoretically extension of magnetic resonance force microscopy (MRFM) replacing a ferromagnetic probe on a cantilever tip (CT) with a paramagnetic one (PMRFM). The dynamics of the interaction between the paramagnetic probe and a local magnetic moment in a sample is analyzed, using a quasi-classical approach. We show that the application of a proper sequence of electromagnetic pulses provides a significant deflection of the CT from the initial equilibrium position. Periodic application of these sequences of pulses results in quasi-periodic CT deflections from the equilibrium, which can be used for detection of the magnetic moment in a sample.

Magnetic resonance force microscopy with a paramagnetic probe

DOE PAGES

Berman, G. P.; Gorshkov, V. N.; Tsifrinovich, V. I.

2017-04-01

Here, we consider theoretically extension of magnetic resonance force microscopy (MRFM) replacing a ferromagnetic probe on a cantilever tip (CT) with a paramagnetic one (PMRFM). The dynamics of the interaction between the paramagnetic probe and a local magnetic moment in a sample is analyzed, using a quasi-classical approach. We show that the application of a proper sequence of electromagnetic pulses provides a significant deflection of the CT from the initial equilibrium position. Periodic application of these sequences of pulses results in quasi-periodic CT deflections from the equilibrium, which can be used for detection of the magnetic moment in a sample.

Development of carbon electrodes for electrochemistry, solid-state electronics and multimodal atomic force microscopy imaging

NASA Astrophysics Data System (ADS)

Morton, Kirstin Claire

Carbon is one of the most remarkable elements due to its wide abundance on Earth and its many allotropes, which include diamond and graphite. Many carbon allotropes are conductive and in recent decades scientists have discovered and synthesized many new forms of carbon, including graphene and carbon nanotubes. The work in this thesis specifically focuses on the fabrication and characterization of pyrolyzed parylene C (PPC), a conductive pyrocarbon, as an electrode material for diodes, as a conductive coating for atomic force microscopy (AFM) probes and as an ultramicroelectrode (UME) for the electrochemical interrogation of cellular systems in vitro. Herein, planar and three-dimensional (3D) PPC electrodes were microscopically, spectroscopically and electrochemically characterized. First, planar PPC films and PPC-coated nanopipettes were utilized to detect a model redox species, Ru(NH3) 6Cl3. Then, free-standing PPC thin films were chemically doped, with hydrazine and concentrated nitric acid, to yield p- and n-type carbon films. Doped PPC thin films were positioned in conjunction with doped silicon to create Schottky and p-n junction diodes for use in an alternating current half-wave rectifier circuit. Pyrolyzed parylene C has found particular merit as a 3D electrode coating of AFM probes. Current sensing-atomic force microscopy imaging in air of nanoscale metallic features was undertaken to demonstrate the electronic imaging applicability of PPC AFM probes. Upon further insulation with parylene C and modification with a focused ion beam, a PPC UME was microfabricated near the AFM probe apex and utilized for electrochemical imaging. Subsequently, scanning electrochemical microscopy-atomic force microscopy imaging was undertaken to electrochemically quantify and image the spatial location of dopamine exocytotic release, elicited mechanically via the AFM probe itself, from differentiated pheochromocytoma 12 cells in vitro.

Probing the stochastic, motor-driven properties of the cytoplasm using force spectrum microscopy

PubMed Central

Guo, Ming; Ehrlicher, Allen J.; Jensen, Mikkel H.; Renz, Malte; Moore, Jeffrey R.; Goldman, Robert D.; Lippincott-Schwartz, Jennifer; Mackintosh, Frederick C.; Weitz, David A.

2014-01-01

SUMMARY Molecular motors in cells typically produce highly directed motion; however, the aggregate, incoherent effect of all active processes also creates randomly fluctuating forces, which drive diffusive-like, non-thermal motion. Here we introduce force-spectrum-microscopy (FSM) to directly quantify random forces within the cytoplasm of cells and thereby probe stochastic motor activity. This technique combines measurements of the random motion of probe particles with independent micromechanical measurements of the cytoplasm to quantify the spectrum of force fluctuations. Using FSM, we show that force fluctuations substantially enhance intracellular movement of small and large components. The fluctuations are three times larger in malignant cells than in their benign counterparts. We further demonstrate that vimentin acts globally to anchor organelles against randomly fluctuating forces in the cytoplasm, with no effect on their magnitude. Thus, FSM has broad applications for understanding the cytoplasm and its intracellular processes in relation to cell physiology in healthy and diseased states. PMID:25126787

True Tapping Mode Scanning Near-Field Optical Microscopy with Bent Glass Fiber Probes.

PubMed

Smirnov, A; Yasinskii, V M; Filimonenko, D S; Rostova, E; Dietler, G; Sekatskii, S K

2018-01-01

In scanning near-field optical microscopy, the most popular probes are made of sharpened glass fiber attached to a quartz tuning fork (TF) and exploiting the shear force-based feedback. The use of tapping mode feedback could be preferable. Such an approach can be realized, for example, using bent fiber probes. Detailed analysis of fiber vibration modes shows that realization of truly tapping mode of the probe dithering requires an extreme caution. In case of using the second resonance mode, probes vibrate mostly in shear force mode unless the bending radius is rather small (ca. 0.3 mm) and the probe's tip is short. Otherwise, the shear force character of the dithering persists. Probes having these characteristics were prepared by irradiation of a tapered etched glass fiber with a CW CO 2 laser. These probes were attached to the TF in double resonance conditions which enables achieving significant quality factor (4000-6000) of the TF + probe system (Cherkun et al., 2006). We also show that, to achieve a truly tapping character, dithering, short, and not exceeding 3 mm lengths of a freestanding part of bent fiber probe beam should also be used in the case of nonresonant excitation.

Use of Kelvin probe force microscopy for identification of CVD grown graphene flakes on copper foil

NASA Astrophysics Data System (ADS)

Kumar, Rakesh; Mehta, B. R.; Kanjilal, D.

2017-05-01

Graphene flakes have been grown by chemical vapour deposition (CVD) method on Cu foils. The obtained graphene flakes have been characterized by optical microscopy, field emission scanning electron microscopy, Kelvin probe force microscopy (KPFM) and Raman spectroscopy. The graphene flakes grown on Cu foil comprise mainly single layer graphene and confirm that the nucleation for graphene growth starts very quickly. Moreover, KPFM has been found to be a valuable technique to differentiate between covered and uncovered portion of Cu foil by graphene flakes deposited for shorter duration. The results show that KPFM can be a very useful technique in understanding the mechanism of graphene growth.

Kelvin Probe Force Microscopy in liquid using Electrochemical Force Microscopy

DOE PAGES

Collins, Liam; Jesse, Stephen; Kilpatrick, J.; ...

2015-01-19

Conventional closed loop-Kelvin probe force microscopy (KPFM) has emerged as a powerful technique for probing electric and transport phenomena at the solid-gas interface. The extension of KPFM capabilities to probe electrostatic and electrochemical phenomena at the solid–liquid interface is of interest for a broad range of applications from energy storage to biological systems. However, the operation of KPFM implicitly relies on the presence of a linear lossless dielectric in the probe-sample gap, a condition which is violated for ionically-active liquids (e.g., when diffuse charge dynamics are present). Here, electrostatic and electrochemical measurements are demonstrated in ionically-active (polar isopropanol, milli-Q watermore » and aqueous NaCl) and ionically-inactive (non-polar decane) liquids by electrochemical force microscopy (EcFM), a multidimensional (i.e., bias- and time-resolved) spectroscopy method. In the absence of mobile charges (ambient and non-polar liquids), KPFM and EcFM are both feasible, yielding comparable contact potential difference (CPD) values. In ionically-active liquids, KPFM is not possible and EcFM can be used to measure the dynamic CPD and a rich spectrum of information pertaining to charge screening, ion diffusion, and electrochemical processes (e.g., Faradaic reactions). EcFM measurements conducted in isopropanol and milli-Q water over Au and highly ordered pyrolytic graphite electrodes demonstrate both sample- and solvent-dependent features. Finally, the feasibility of using EcFM as a local force-based mapping technique of material-dependent electrostatic and electrochemical response is investigated. The resultant high dimensional dataset is visualized using a purely statistical approach that does not require a priori physical models, allowing for qualitative mapping of electrostatic and electrochemical material properties at the solid–liquid interface.« less

Quantification of in-contact probe-sample electrostatic forces with dynamic atomic force microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Balke, Nina Wisinger; Jesse, Stephen; Carmichael, Ben D.

Here, atomic force microscopy (AFM) methods utilizing resonant mechanical vibrations of cantilevers in contact with a sample surface have shown sensitivities as high as few picometers for detecting surface displacements. Such a high sensitivity is harnessed in several AFM imaging modes. Here, we demonstrate a cantilever-resonance-based method to quantify electrostatic forces on a probe in the probe-sample junction in the presence of a surface potential or when a bias voltage is applied to the AFM probe. We find that the electrostatic forces acting on the probe tip apex can produce signals equivalent to a few pm of surface displacement. Inmore » combination with modeling, the measurements of the force were used to access the strength of the electrical field at the probe tip apex in contact with a sample. We find an evidence that the electric field strength in the junction can reach ca. 1 V nm –1 at a bias voltage of a few volts and is limited by non-ideality of the tip-sample contact. This field is sufficiently strong to significantly influence material states and kinetic processes through charge injection, Maxwell stress, shifts of phase equilibria, and reduction of energy barriers for activated processes. Besides, the results provide a baseline for accounting for the effects of local electrostatic forces in electromechanical AFM measurements as well as offer additional means to probe ionic mobility and field-induced phenomena in solids.« less

Quantification of In-Contact Probe-Sample Electrostatic Forces with Dynamic Atomic Force Microscopy.

PubMed

Balke, Nina; Jesse, Stephen; Carmichael, Ben; Okatan, M; Kravchenko, Ivan; Kalinin, Sergei; Tselev, Alexander

2016-12-13

Atomic Force Microscopy (AFM) methods utilizing resonant mechanical vibrations of cantilevers in contact with a sample surface have shown sensitivities as high as few picometers for detecting surface displacements. Such a high sensitivity is harnessed in several AFM imaging modes. Here, we demonstrate a cantilever-resonance-based method to quantify electrostatic forces on a probe in the probe-sample junction in the presence of a surface potential or when a bias voltage is applied to the AFM probe. We find that the electrostatic forces acting on the probe tip apex can produce signals equivalent to a few pm of surface displacement. In combination with modeling, the measurements of the force were used to access the strength of the electrical field at the probe tip apex in contact with a sample. We find an evidence that the electric field strength in the junction can reach ca. 1 V/nm at a bias voltage of a few volts and is limited by non-ideality of the tip-sample contact. This field is sufficiently strong to significantly influence material states and kinetic processes through charge injection, Maxwell stress, shifts of phase equilibria, and reduction of energy barriers for activated processes. Besides, the results provide a baseline for accounting for the effects of local electrostatic forces in electromechanical AFM measurements as well as offer additional means to probe ionic mobility and field-induced phenomena in solids. Copyright 2016 IOP Publishing Ltd.

Quantification of in-contact probe-sample electrostatic forces with dynamic atomic force microscopy

DOE PAGES

Balke, Nina Wisinger; Jesse, Stephen; Carmichael, Ben D.; ...

2017-01-04

Here, atomic force microscopy (AFM) methods utilizing resonant mechanical vibrations of cantilevers in contact with a sample surface have shown sensitivities as high as few picometers for detecting surface displacements. Such a high sensitivity is harnessed in several AFM imaging modes. Here, we demonstrate a cantilever-resonance-based method to quantify electrostatic forces on a probe in the probe-sample junction in the presence of a surface potential or when a bias voltage is applied to the AFM probe. We find that the electrostatic forces acting on the probe tip apex can produce signals equivalent to a few pm of surface displacement. Inmore » combination with modeling, the measurements of the force were used to access the strength of the electrical field at the probe tip apex in contact with a sample. We find an evidence that the electric field strength in the junction can reach ca. 1 V nm –1 at a bias voltage of a few volts and is limited by non-ideality of the tip-sample contact. This field is sufficiently strong to significantly influence material states and kinetic processes through charge injection, Maxwell stress, shifts of phase equilibria, and reduction of energy barriers for activated processes. Besides, the results provide a baseline for accounting for the effects of local electrostatic forces in electromechanical AFM measurements as well as offer additional means to probe ionic mobility and field-induced phenomena in solids.« less

Nanoscale Investigation of Grain Growth in RF-Sputtered Indium Tin Oxide Thin Films by Scanning Probe Microscopy

NASA Astrophysics Data System (ADS)

Lamsal, B. S.; Dubey, M.; Swaminathan, V.; Huh, Y.; Galipeau, D.; Qiao, Q.; Fan, Q. H.

2014-11-01

This work studied the electronic characteristics of the grains and grain boundaries of indium tin oxide (ITO) thin films using electrostatic and Kelvin probe force microscopy. Two types of ITO films were compared, deposited using radiofrequency magnetron sputtering in pure argon or 99% argon + 1% oxygen, respectively. The average grain size and surface roughness increased with substrate temperature for the films deposited in pure argon. With the addition of 1% oxygen, the increase in the grain size was inhibited above 150°C, which was suggested to be due to passivation of the grains by the excess oxygen. Electrostatic force microscopy and Kelvin probe force microscopy (KPFM) images confirmed that the grain growth was defect mediated and occurred at defective interfaces at high temperatures. Films deposited at room temperature with 1% oxygen showed crystalline nature, while films deposited with pure argon at room temperature were amorphous as observed from KPFM images. The potential drop across the grain and grain boundary was determined by taking surface potential line profiles to evaluate the electronic properties.

An atomic-force-microscopy study of the structure of surface layers of intact fibroblasts

NASA Astrophysics Data System (ADS)

Khalisov, M. M.; Ankudinov, A. V.; Penniyaynen, V. A.; Nyapshaev, I. A.; Kipenko, A. V.; Timoshchuk, K. I.; Podzorova, S. A.; Krylov, B. V.

2017-02-01

Intact embryonic fibroblasts on a collagen-treated substrate have been studied by atomic-force microscopy (AFM) using probes of two types: (i) standard probes with tip curvature radii of 2-10 nm and (ii) special probes with a calibrated 325-nm SiO2 ball radius at the tip apex. It is established that, irrespective of probe type, the average maximum fibroblast height is on a level of 1.7 μm and the average stiffness of the probe-cell contact amounts to 16.5 mN/m. The obtained AFM data reveal a peculiarity of the fibroblast structure, whereby its external layers move as a rigid shell relative to the interior and can be pressed inside to a depth dependent on the load only.

Scanning Probe Microscopy and Electrical Transport Studies of Ferroelectric Thin Films and 2D van der Waals Materials

NASA Astrophysics Data System (ADS)

Xiao, Zhiyong

In this dissertation, I present the scanning microscopy and electrical transport studies of ferroelectric thin films and ferroic/2D van der Waals heterostructures. Based on the conducting probe atomic force microscopy and piezo-response force microscopy (PFM) studies of the static and dynamic behavior of ferroelectric domain walls (DW), we found that the ferroelectric polymer poly(vinylidene-fluoride-trifluorethylene) P(VDF-TrFE) is composed of two-dimensional (2D) ferroelectric monolayers (MLs) that are weakly coupled to each other. We also observed polarization asymmetry in epitaxial thin films of ferroelectric Pb(Zr,Ti)O3, which is attributed to the screening properties of the underlying conducting oxide. PFM studies also reveal ferroelectric relaxor-type behavior in ultrathin Sr(Zr,Ti)O3 films epitaxially deposited on Ge. We exploited scanning-probe-controlled domain patterning in a P(VDF-TrFE) top layer to induce nonvolatile modulation of the conduction characteristic of ML molybdenum disulfide (MoS2) between a transistor and a junction state. In the presence of a DW, MoS2 exhibits rectified Ids-Vds (IV) characteristics that are well described by the thermionic emission model. This approach can be applied to a wide range of van der Waals materials to design various functional homojunctions and nanostructures. We also studied the interfacial charge transfer effect between graphene and magnetoelectric Cr2O3 via electrostatic force microscopy and Kelvin probe force microscopy, which reveal p-type doping with up to 150 meV shift of the Fermi level. The graphene/Cr2O3 heterostructure is promising for developing magnetoelectric graphene transistors for spintronic applications.

Recent Progress in Nanoelectrical Characterizations of CdTe and Cu(In,Ga)Se2

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jiang, Chun-Sheng; To, Bobby; Glynn, Stephen

2016-11-21

We report two recent nanoelectrical characterizations of CdTe and Cu(In, Ga)Se2 (CIGS) thin-film solar cells by developing atomic force microscopy-based nanoelectrical probes. Charges trapped at defects at the CdS/CdTe interface were probed by Kelvin probe force microscopy (KPFM) potential mapping and by ion-milling the CdTe superstrate device in a bevel glancing angle of ~0.5 degrees. The results show randomly distributed donor-like defects at the interface. The effect of K post-deposition treatment on the near-surface region of the CIGS film was studied by KPFM potential and scanning spreading resistance microscopy (SSRM) resistivity mapping, which shows passivation of grain-boundary potential and improvementmore » of resistivity uniformity by the K treatment.« less

Work function of few layer graphene covered nickel thin films measured with Kelvin probe force microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Eren, B.; Material Sciences Division, Lawrence Berkeley National Laboratory, 1 Cyclotron Road, Berkeley, California 94720; Gysin, U.

2016-01-25

Few layer graphene and graphite are simultaneously grown on a ∼100 nm thick polycrystalline nickel film. The work function of few layer graphene/Ni is found to be 4.15 eV with a variation of 50 meV by local measurements with Kelvin probe force microscopy. This value is lower than the work function of free standing graphene due to peculiar electronic structure resulting from metal 3d-carbon 2p(π) hybridization.

Final Technical Report for Award DESC0011912, "Trimodal Tapping Mode Atomic Force Microscopy: Simultaneous 4D Mapping of Conservative and Dissipative Probe-Sample Interactions of Energy-Relevant Materials”

DOE Office of Scientific and Technical Information (OSTI.GOV)

Solares, Santiago D.

The final project report covering the period 7/1/14-6/30/17 provides an overview of the technical accomplishments in the areas of (i) fundamental viscoelasticity, (ii) multifrequency atomic force microscopy, and (iii) characterization of energy-relevant materials with atomic force microscopy. A list of publications supported by the project is also provided.

Interpretation of frequency modulation atomic force microscopy in terms of fractional calculus

NASA Astrophysics Data System (ADS)

Sader, John E.; Jarvis, Suzanne P.

2004-07-01

It is widely recognized that small amplitude frequency modulation atomic force microscopy probes the derivative of the interaction force between tip and sample. For large amplitudes, however, such a physical connection is currently lacking, although it has been observed that the frequency shift presents a quantity intermediate to the interaction force and energy for certain force laws. Here we prove that these observations are a universal property of large amplitude frequency modulation atomic force microscopy, by establishing that the frequency shift is proportional to the half-fractional integral of the force, regardless of the force law. This finding indicates that frequency modulation atomic force microscopy can be interpreted as a fractional differential operator, where the order of the derivative/integral is dictated by the oscillation amplitude. We also establish that the measured frequency shift varies systematically from a probe of the force gradient for small oscillation amplitudes, through to the measurement of a quantity intermediate to the force and energy (the half-fractional integral of the force) for large oscillation amplitudes. This has significant implications to measurement sensitivity, since integrating the force will smooth its behavior, while differentiating it will enhance variations. This highlights the importance in choice of oscillation amplitude when wishing to optimize the sensitivity of force spectroscopy measurements to short-range interactions and consequently imaging with the highest possible resolution.

Exploring Local Electrostatic Effects with Scanning Probe Microscopy: Implications for Piezoresponse Force Microscopy and Triboelectricity

DOE PAGES

Balke, Nina; Maksymovych, Petro; Jesse, Stephen; ...

2014-09-25

The implementation of contact mode Kelvin probe force microscopy (KPFM) utilizes the electrostatic interactions between tip and sample when the tip and sample are in contact with each other. Surprisingly, the electrostatic forces in contact are large enough to be measured even with tips as stiff as 4.5 N/m. As for traditional non-contact KPFM, the signal depends strongly on electrical properties of the sample, such as the dielectric constant, and the tip-properties, such as the stiffness. Since the tip is in contact with the sample, bias-induced changes in the junction potential between tip and sample can be measured with highermore » lateral and temporal resolution compared to traditional non-contact KPFM. Significant and reproducible variations of tip-surface capacitance are observed and attributed to surface electrochemical phenomena. Lastly, observations of significant surface charge states at zero bias and strong hysteretic electromechanical responses at non-ferroelectric surface have significant implications for fields such as triboelectricity and piezoresponse force microscopy.« less

Characterization of Antisticking Layers for UV Nanoimprint Lithography Molds with Scanning Probe Microscopy

NASA Astrophysics Data System (ADS)

Masaaki Kurihara,; Sho Hatakeyama,; Noriko Yamada,; Takeya Shimomura,; Takaharu Nagai,; Kouji Yoshida,; Tatsuya Tomita,; Morihisa Hoga,; Naoya Hayashi,; Hiroyuki Ohtani,; Masamichi Fujihira,

2010-06-01

Antisticking layers (ASLs) on UV nanoimprint lithography (UV-NIL) molds were characterized by scanning probe microscopies (SPMs) in addition to macroscopic analyses of work of adhesion and separation force. Local physical properties of the ASLs were measured by atomic force microscopy (AFM) and friction force microscopy (FFM). The behavior of local adhesive forces measured with AFM on several surfaces was consistent with that of work of adhesion obtained from contact angle. The ASLs were coated by two different processes, i.e., one is a vapor-phase process and the other a spin-coating process. The homogeneity of the ASLs prepared by the vapor-phase process was better than that of those prepared by the spin-coating process. In addition, we measured the thicknesses of ASL patterns prepared by a lift-off method to investigate the effect of the ASL thicknesses on critical dimensions of the molds with ASLs and found that this effect is not negligible.

Surface potential measurement of n-type organic semiconductor thin films by mist deposition via Kelvin probe microscopy

NASA Astrophysics Data System (ADS)

Odaka, Akihiro; Satoh, Nobuo; Katori, Shigetaka

2017-08-01

We partially deposited fullerene (C60) and phenyl-C61-butyric acid methyl ester thin films that are typical n-type semiconductor materials on indium-tin oxide by mist deposition at various substrate temperatures. The topographic and surface potential images were observed via dynamic force microscopy/Kelvin probe force microscopy with the frequency modulation detection method. We proved that the area where a thin film is deposited depends on the substrate temperature during deposition from the topographic images. It was also found that the surface potential depends on the substrate temperature from the surface potential images.

True Tapping Mode Scanning Near-Field Optical Microscopy with Bent Glass Fiber Probes

PubMed Central

Yasinskii, V. M.; Filimonenko, D. S.; Rostova, E.; Dietler, G.; Sekatskii, S. K.

2018-01-01

In scanning near-field optical microscopy, the most popular probes are made of sharpened glass fiber attached to a quartz tuning fork (TF) and exploiting the shear force-based feedback. The use of tapping mode feedback could be preferable. Such an approach can be realized, for example, using bent fiber probes. Detailed analysis of fiber vibration modes shows that realization of truly tapping mode of the probe dithering requires an extreme caution. In case of using the second resonance mode, probes vibrate mostly in shear force mode unless the bending radius is rather small (ca. 0.3 mm) and the probe's tip is short. Otherwise, the shear force character of the dithering persists. Probes having these characteristics were prepared by irradiation of a tapered etched glass fiber with a CW CO2 laser. These probes were attached to the TF in double resonance conditions which enables achieving significant quality factor (4000–6000) of the TF + probe system (Cherkun et al., 2006). We also show that, to achieve a truly tapping character, dithering, short, and not exceeding 3 mm lengths of a freestanding part of bent fiber probe beam should also be used in the case of nonresonant excitation. PMID:29849857

Probing of multiple magnetic responses in magnetic inductors using atomic force microscopy.

PubMed

Park, Seongjae; Seo, Hosung; Seol, Daehee; Yoon, Young-Hwan; Kim, Mi Yang; Kim, Yunseok

2016-02-08

Even though nanoscale analysis of magnetic properties is of significant interest, probing methods are relatively less developed compared to the significance of the technique, which has multiple potential applications. Here, we demonstrate an approach for probing various magnetic properties associated with eddy current, coil current and magnetic domains in magnetic inductors using multidimensional magnetic force microscopy (MMFM). The MMFM images provide combined magnetic responses from the three different origins, however, each contribution to the MMFM response can be differentiated through analysis based on the bias dependence of the response. In particular, the bias dependent MMFM images show locally different eddy current behavior with values dependent on the type of materials that comprise the MI. This approach for probing magnetic responses can be further extended to the analysis of local physical features.

Photoassisted Kelvin probe force microscopy at GaN surfaces: The role of polarity

NASA Astrophysics Data System (ADS)

Wei, J. D.; Li, S. F.; Atamuratov, A.; Wehmann, H.-H.; Waag, A.

2010-10-01

The behavior of GaN surfaces during photoassisted Kelvin probe force microscopy is demonstrated to be strongly dependant on surface polarity. The surface photovoltage of GaN surfaces illuminated with above-band gap light is analyzed as a function of time and light intensity. Distinct differences between Ga-polar and N-polar surfaces could be identified, attributed to photoinduced chemisorption of oxygen during illumination. These differences can be used for a contactless, nondestructive, and easy-performable analysis of the polarity of GaN surfaces.

Note: Switching crosstalk on and off in Kelvin probe force microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Polak, Leo, E-mail: l.polak@vu.nl; Wijngaarden, Rinke J.; Man, Sven de

2014-04-15

In Kelvin Probe Force Microscopy (KPFM) electronic crosstalk can occur between the excitation signal and probe deflection signal. Here, we demonstrate how a small modification to our commercial instrument enables us to literally switch the crosstalk on and off. We study in detail the effect of crosstalk on open-loop KPFM and compare with closed-loop KPFM. We measure the pure crosstalk signal and verify that we can correct for it in the data-processing required for open-loop KPFM. We also demonstrate that open-loop KPFM results are independent of the frequency and amplitude of the excitation signal, provided that the influence of crosstalkmore » has been eliminated.« less

Application of atomic force microscopy to microbial surfaces: from reconstituted cell surface layers to living cells.

PubMed

Dufrêne, Y F

2001-02-01

The application of atomic force microscopy (AFM) to probe the ultrastructure and physical properties of microbial cell surfaces is reviewed. The unique capabilities of AFM can be summarized as follows: imaging surface topography with (sub)nanometer lateral resolution; examining biological specimens under physiological conditions; measuring local properties and interaction forces. AFM is being used increasingly for: (i) visualizing the surface ultrastructure of microbial cell surface layers, including bacterial S-layers, purple membranes, porin OmpF crystals and fungal rodlet layers; (ii) monitoring conformational changes of individual membrane proteins; (iii) examining the morphology of bacterial biofilms, (iv) revealing the nanoscale structure of living microbial cells, including fungi, yeasts and bacteria, (v) mapping interaction forces at microbial surfaces, such as van der Waals and electrostatic forces, solvation forces, and steric/bridging forces; and (vi) probing the local mechanical properties of cell surface layers and of single cells.

Effect of tip polarity on Kelvin probe force microscopy images of thin insulator CaF2 films on Si(111)

NASA Astrophysics Data System (ADS)

Yurtsever, Ayhan; Sugimoto, Yoshiaki; Fukumoto, Masaki; Abe, Masayuki; Morita, Seizo

2012-08-01

We investigate thin insulating CaF2 films on a Si (111) surface using a combination of noncontact atomic force microscopy (NC-AFM) and Kelvin probe force microscopy (KPFM). Atomic-scale NC-AFM and KPFM images are obtained in different imaging modes by employing two different tip polarities. The KPFM image contrast and the distance-dependent variation of the local contact potential difference (LCPD) give rise to a tip-polarity-dependent contrast inversion. Ca2+ cations had a higher LCPD contrast than F- anions for a positively terminated tip, while the LCPD provided by a negatively charged tip gave a higher contrast for F- anions. Thus, this result implies that it is essential to determine the tip apex polarity to correctly interpret LCPD signals acquired by KPFM.

Elemental Identification by Combining Atomic Force Microscopy and Kelvin Probe Force Microscopy.

PubMed

Schulz, Fabian; Ritala, Juha; Krejčí, Ondrej; Seitsonen, Ari Paavo; Foster, Adam S; Liljeroth, Peter

2018-06-01

There are currently no experimental techniques that combine atomic-resolution imaging with elemental sensitivity and chemical fingerprinting on single molecules. The advent of using molecular-modified tips in noncontact atomic force microscopy (nc-AFM) has made it possible to image (planar) molecules with atomic resolution. However, the mechanisms responsible for elemental contrast with passivated tips are not fully understood. Here, we investigate elemental contrast by carrying out both nc-AFM and Kelvin probe force microscopy (KPFM) experiments on epitaxial monolayer hexagonal boron nitride (hBN) on Ir(111). The hBN overlayer is inert, and the in-plane bonds connecting nearest-neighbor boron and nitrogen atoms possess strong covalent character and a bond length of only ∼1.45 Å. Nevertheless, constant-height maps of both the frequency shift Δ f and the local contact potential difference exhibit striking sublattice asymmetry. We match the different atomic sites with the observed contrast by comparison with nc-AFM image simulations based on the density functional theory optimized hBN/Ir(111) geometry, which yields detailed information on the origin of the atomic-scale contrast.

Fourier Transform Infrared (FTIR) Spectroscopy, Ultraviolet Resonance Raman (UVRR) Spectroscopy, and Atomic Force Microscopy (AFM) for Study of the Kinetics of Formation and Structural Characterization of Tau Fibrils.

PubMed

Ramachandran, Gayathri

2017-01-01

Kinetic studies of tau fibril formation in vitro most commonly employ spectroscopic probes such as thioflavinT fluorescence and laser light scattering or negative stain transmission electron microscopy. Here, I describe the use of Fourier transform infrared (FTIR) spectroscopy, ultraviolet resonance Raman (UVRR) spectroscopy, and atomic force microscopy (AFM) as complementary probes for studies of tau aggregation. The sensitivity of vibrational spectroscopic techniques (FTIR and UVRR) to secondary structure content allows for measurement of conformational changes that occur when the intrinsically disordered protein tau transforms into cross-β-core containing fibrils. AFM imaging serves as a gentle probe of structures populated over the time course of tau fibrillization. Together, these assays help further elucidate the structural and mechanistic complexity inherent in tau fibril formation.

In pursuit of photo-induced magnetic and chiral microscopy

NASA Astrophysics Data System (ADS)

Zeng, Jinwei; Kamandi, Mohammad; Darvishzadeh-Varcheie, Mahsa; Albooyeh, Mohammad; Veysi, Mehdi; Guclu, Caner; Hanifeh, Mina; Rajaei, Mohsen; Potma, Eric O.; Wickramasinghe, H. Kumar; Capolino, Filippo

2018-06-01

Light-matter interactions enable the perception of specimen properties such as its shape and dimensions by measuring the subtle differences carried by an illuminating beam after interacting with the sample. However, major obstacles arise when the relevant properties of the specimen are weakly coupled to the incident beam, for example when measuring optical magnetism and chirality. To address this challenge we propose the idea of detecting such weakly-coupled properties of matter through the photo-induced force, aiming at developing photo-induced magnetic or chiral force microscopy. Here we review our pursuit consisting of the following steps: (1) Development of a theoretical blueprint of a magnetic nanoprobe to detect a magnetic dipole oscillating at an optical frequency when illuminated by an azimuthally polarized beam via the photo-induced magnetic force; (2) Conducting an experimental study using an azimuthally polarized beam to probe the near fields and axial magnetism of a Si disk magnetic nanoprobe, based on photo-induced force microscopy; (3) Extending the concept of force microscopy to probe chirality at the nanoscale, enabling enantiomeric detection of chiral molecules. Finally, we discuss difficulties and how they could be overcome, as well as our plans for future work. Invited Paper

Electrical Study of Trapped Charges in Copper-Doped Zinc Oxide Films by Scanning Probe Microscopy for Nonvolatile Memory Applications

PubMed Central

Su, Ting; Zhang, Haifeng

2017-01-01

Charge trapping properties of electrons and holes in copper-doped zinc oxide (ZnO:Cu) films have been studied by scanning probe microscopy. We investigated the surface potential dependence on the voltage and duration applied to the copper-doped ZnO films by Kelvin probe force microscopy. It is found that the Fermi Level of the 8 at.% Cu-doped ZnO films shifted by 0.53 eV comparing to undoped ZnO films. This shift indicates significant change in the electronic structure and energy balance in Cu-doped ZnO films. The Fermi Level (work function) of zinc oxide films can be tuned by Cu doping, which are important for developing this functional material. In addition, Kelvin probe force microscopy measurements demonstrate that the nature of contact at Pt-coated tip/ZnO:Cu interface is changed from Schottky contact to Ohmic contact by increasing sufficient amount of Cu ions. The charge trapping property of the ZnO films enhance greatly by Cu doping (~10 at.%). The improved stable bipolar charge trapping properties indicate that copper-doped ZnO films are promising for nonvolatile memory applications. PMID:28135335

The importance of cantilever dynamics in the interpretation of Kelvin probe force microscopy.

PubMed

Satzinger, Kevin J; Brown, Keith A; Westervelt, Robert M

2012-09-15

A realistic interpretation of the measured contact potential difference (CPD) in Kelvin probe force microscopy (KPFM) is crucial in order to extract meaningful information about the sample. Central to this interpretation is a method to include contributions from the macroscopic cantilever arm, as well as the cone and sharp tip of a KPFM probe. Here, three models of the electrostatic interaction between a KPFM probe and a sample are tested through an electrostatic simulation and compared with experiment. In contrast with previous studies that treat the KPFM cantilever as a rigid object, we allow the cantilever to bend and rotate; accounting for cantilever bending provides the closest agreement between theory and experiment. We demonstrate that cantilever dynamics play a major role in CPD measurements and provide a simulation technique to explore this phenomenon.

Breaking the Time Barrier in Kelvin Probe Force Microscopy: Fast Free Force Reconstruction Using the G-Mode Platform

DOE Office of Scientific and Technical Information (OSTI.GOV)

Collins, Liam; Ahmadi, Mahshid; Wu, Ting

The atomic force microscope (AFM) offers unparalleled insight into structure and material functionality across nanometer length scales. However, the spatial resolution afforded by the AFM tip is counterpoised by slow detection speeds compared to other common microscopy techniques (e.g. optical, scanning electron microscopy etc.). In this work, we develop an AFM imaging approach allowing ultrafast reconstruction of the tip-sample forces having ~2 orders of magnitude higher time resolution than standard detection methods. Fast free force recovery (F3R) overcomes the widely-viewed temporal bottleneck in AFM, i.e. the mechanical bandwidth of the cantilever, enabling time-resolved imaging at sub-bandwidth speeds. We demonstrate quantitativemore » recovery of electrostatic forces with ~10 µs temporal resolution, free from cantilever ring-down effects. We further apply the F3R method to Kelvin probe force microscopy (KPFM) measurements. F3R-KPFM is an open loop imaging approach (i.e. no bias feedback), allowing ultrafast surface potential measurements (e.g. < 20 µs) to be performed at regular KPFM scan speeds. F3R-KPFM is demonstrated for exploration of ion migration in organometallic halide perovskites materials and shown to allow spatio-temporal imaging of positively charged ion migration under applied electric field, as well as subsequent formation of accumulated charges at the perovskite/electrode interface. In this work we demonstrate quantitative F3R-KPFM measurements – however, we fully expect the F3R approach to be valid for all modes of non-contact AFM operation, including non-invasive probing of ultrafast electrical and magnetic dynamics.« less

Breaking the Time Barrier in Kelvin Probe Force Microscopy: Fast Free Force Reconstruction Using the G-Mode Platform

DOE PAGES

Collins, Liam; Ahmadi, Mahshid; Wu, Ting; ...

2017-08-06

The atomic force microscope (AFM) offers unparalleled insight into structure and material functionality across nanometer length scales. However, the spatial resolution afforded by the AFM tip is counterpoised by slow detection speeds compared to other common microscopy techniques (e.g. optical, scanning electron microscopy etc.). In this work, we develop an AFM imaging approach allowing ultrafast reconstruction of the tip-sample forces having ~2 orders of magnitude higher time resolution than standard detection methods. Fast free force recovery (F3R) overcomes the widely-viewed temporal bottleneck in AFM, i.e. the mechanical bandwidth of the cantilever, enabling time-resolved imaging at sub-bandwidth speeds. We demonstrate quantitativemore » recovery of electrostatic forces with ~10 µs temporal resolution, free from cantilever ring-down effects. We further apply the F3R method to Kelvin probe force microscopy (KPFM) measurements. F3R-KPFM is an open loop imaging approach (i.e. no bias feedback), allowing ultrafast surface potential measurements (e.g. < 20 µs) to be performed at regular KPFM scan speeds. F3R-KPFM is demonstrated for exploration of ion migration in organometallic halide perovskites materials and shown to allow spatio-temporal imaging of positively charged ion migration under applied electric field, as well as subsequent formation of accumulated charges at the perovskite/electrode interface. In this work we demonstrate quantitative F3R-KPFM measurements – however, we fully expect the F3R approach to be valid for all modes of non-contact AFM operation, including non-invasive probing of ultrafast electrical and magnetic dynamics.« less

Physical probing of cells

NASA Astrophysics Data System (ADS)

Rehfeldt, Florian; Schmidt, Christoph F.

2017-11-01

In the last two decades, it has become evident that the mechanical properties of the microenvironment of biological cells are as important as traditional biochemical cues for the control of cellular behavior and fate. The field of cell and matrix mechanics is quickly growing and so is the development of the experimental approaches used to study active and passive mechanical properties of cells and their surroundings. Within this topical review we will provide a brief overview, on the one hand, over how cellular mechanics can be probed physically, how different geometries allow access to different cellular properties, and, on the other hand, how forces are generated in cells and transmitted to the extracellular environment. We will describe the following experimental techniques: atomic force microscopy, traction force microscopy, magnetic tweezers, optical stretcher and optical tweezers pointing out both their advantages and limitations. Finally, we give an outlook on the future of the physical probing of cells.

Analysis and modification of defective surface aggregates on PCDTBT:PCBM solar cell blends using combined Kelvin probe, conductive and bimodal atomic force microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Noh, Hanaul; Diaz, Alfredo J.; Solares, Santiago D.

Organic photovoltaic systems comprising donor polymers and acceptor fullerene derivatives are attractive for inexpensive energy harvesting. Extensive research on polymer solar cells has provided insight into the factors governing device-level efficiency and stability. However, the detailed investigation of nanoscale structures is still challenging. Here we demonstrate the analysis and modification of unidentified surface aggregates. The aggregates are characterized electrically by Kelvin probe force microscopy and conductive atomic force microscopy (C-AFM), whereby the correlation between local electrical potential and current confirms a defective charge transport. Bimodal AFM modification confirms that the aggregates exist on top of the solar cell structure, andmore » is used to remove them and to reveal the underlying active layer. The systematic analysis of the surface aggregates suggests that the structure consists of PCBM molecules.« less

Analysis and modification of defective surface aggregates on PCDTBT:PCBM solar cell blends using combined Kelvin probe, conductive and bimodal atomic force microscopy

DOE PAGES

Noh, Hanaul; Diaz, Alfredo J.; Solares, Santiago D.

2017-03-08

Organic photovoltaic systems comprising donor polymers and acceptor fullerene derivatives are attractive for inexpensive energy harvesting. Extensive research on polymer solar cells has provided insight into the factors governing device-level efficiency and stability. However, the detailed investigation of nanoscale structures is still challenging. Here we demonstrate the analysis and modification of unidentified surface aggregates. The aggregates are characterized electrically by Kelvin probe force microscopy and conductive atomic force microscopy (C-AFM), whereby the correlation between local electrical potential and current confirms a defective charge transport. Bimodal AFM modification confirms that the aggregates exist on top of the solar cell structure, andmore » is used to remove them and to reveal the underlying active layer. The systematic analysis of the surface aggregates suggests that the structure consists of PCBM molecules.« less

Analysis and modification of defective surface aggregates on PCDTBT:PCBM solar cell blends using combined Kelvin probe, conductive and bimodal atomic force microscopy

PubMed Central

Noh, Hanaul; Diaz, Alfredo J

2017-01-01

Organic photovoltaic systems comprising donor polymers and acceptor fullerene derivatives are attractive for inexpensive energy harvesting. Extensive research on polymer solar cells has provided insight into the factors governing device-level efficiency and stability. However, the detailed investigation of nanoscale structures is still challenging. Here we demonstrate the analysis and modification of unidentified surface aggregates. The aggregates are characterized electrically by Kelvin probe force microscopy and conductive atomic force microscopy (C-AFM), whereby the correlation between local electrical potential and current confirms a defective charge transport. Bimodal AFM modification confirms that the aggregates exist on top of the solar cell structure, and is used to remove them and to reveal the underlying active layer. The systematic analysis of the surface aggregates suggests that the structure consists of PCBM molecules. PMID:28382247

Methods and apparatus of spatially resolved electroluminescence of operating organic light-emitting diodes using conductive atomic force microscopy

NASA Technical Reports Server (NTRS)

Hersam, Mark C. (Inventor); Pingree, Liam S. C. (Inventor)

2008-01-01

A conductive atomic force microscopy (cAFM) technique which can concurrently monitor topography, charge transport, and electroluminescence with nanometer spatial resolution. This cAFM approach is particularly well suited for probing the electroluminescent response characteristics of operating organic light-emitting diodes (OLEDs) over short length scales.

A dark mode in scanning thermal microscopy

NASA Astrophysics Data System (ADS)

Ramiandrisoa, Liana; Allard, Alexandre; Joumani, Youssef; Hay, Bruno; Gomés, Séverine

2017-12-01

The need for high lateral spatial resolution in thermal science using Scanning Thermal Microscopy (SThM) has pushed researchers to look for more and more tiny probes. SThM probes have consequently become more and more sensitive to the size effects that occur within the probe, the sample, and their interaction. Reducing the tip furthermore induces very small heat flux exchanged between the probe and the sample. The measurement of this flux, which is exploited to characterize the sample thermal properties, requires then an accurate thermal management of the probe-sample system and to reduce any phenomenon parasitic to this system. Classical experimental methodologies must then be constantly questioned to hope for relevant and interpretable results. In this paper, we demonstrate and estimate the influence of the laser of the optical force detection system used in the common SThM setup that is based on atomic-force microscopy equipment on SThM measurements. We highlight the bias induced by the overheating due to the laser illumination on the measurements performed by thermoresistive probes (palladium probe from Kelvin Nanotechnology). To face this issue, we propose a new experimental procedure based on a metrological approach of the measurement: a SThM "dark mode." The comparison with the classical procedure using the laser shows that errors between 14% and 37% can be reached on the experimental data exploited to determine the heat flux transferred from the hot probe to the sample.

Experiments in NMR Force Microscopy

NASA Astrophysics Data System (ADS)

Manzanera, Isaac; Cardenas, Rosa; Paster, Jeremy; Turbyfill, Amanda; Markert, John

2012-02-01

We report details of the construction and use of three nuclear magnetic resonance force microscopy (NMRFM) probes, as well as the development of control systems for three-dimensional nanoscale imaging and spectroscopy. Our variable temperature probe performed position-dependent ^1H NMR force measurements on a 25x15x7 μm^3 single crystal of ammonium sulfate (NH4)2SO4 at room temperature in a sample-on-oscillator geometry. Force signals were detected with a signal-to-noise ratio of 6, and 12 μm resolution, in a one-dimensional scan. Measurements of NMR relaxation times T2^*=1.5±0.2 μs, T2= 44±2 μs, and T1=5.6±0.7 s were obtained. We describe the upgrade of our ^3He NMRFM probe for measurements towards the base temperature of 0.3K for investigation of nanoscale structures and metal oxide interfaces using the iOSCAR technique and perpendicular-cantilever geometry. Force-detected ^11B NMR signals in a 30 μm crystal of superconductor MgB2 have also been achieved using this probe. Efforts in the development of our NMRFM probe for the study of biological samples in liquid media are reported. Magnetic field effects on micromagnet films on cantilevers are being studied for the characterization of the mechanical sensors to be used in these liquid experiments.

Separating the influence of electric charges in magnetic force microscopy images of inhomogeneous metal samples

NASA Astrophysics Data System (ADS)

Arenas, Mónica P.; Lanzoni, Evandro M.; Pacheco, Clara J.; Costa, Carlos A. R.; Eckstein, Carlos B.; de Almeida, Luiz H.; Rebello, João M. A.; Deneke, Christoph F.; Pereira, Gabriela R.

2018-01-01

In this study, we investigate artifacts arising from electric charges present in magnetic force microscopy images. Therefore, we use two austenitic steel samples with different microstructural conditions. Furthermore, we examine the influence of the surface preparation, like etching, in magnetic force images. Using Kelvin probe force microscopy we can quantify the charges present on the surface. Our results show that electrical charges give rise to a signature in the magnetic force microscopy, which is indistinguishable from a magnetic signal. Our results on two differently aged steel samples demonstrate that the magnetic force microscopy images need to be interpreted with care and must be corrected due to the influence of electrical charges present. We discuss three approaches, how to identify these artifacts - parallel acquisition of magnetic force and electric force images on the same position, sample surface preparation to decrease the presence of charges and inversion of the magnetic polarization in two succeeding measurement.

Customized atomic force microscopy probe by focused-ion-beam-assisted tip transfer

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Andrew; Butte, Manish J., E-mail: manish.butte@stanford.edu

2014-08-04

We present a technique for transferring separately fabricated tips onto tipless atomic force microscopy (AFM) cantilevers, performed using focused ion beam-assisted nanomanipulation. This method addresses the need in scanning probe microscopy for certain tip geometries that cannot be achieved by conventional lithography. For example, in probing complex layered materials or tall biological cells using AFM, a tall tip with a high-aspect-ratio is required to avoid artifacts caused by collisions of the tip's sides with the material being probed. We show experimentally that tall (18 μm) cantilever tips fabricated by this approach reduce squeeze-film damping, which fits predictions from hydrodynamic theory, andmore » results in an increased quality factor (Q) of the fundamental flexural mode. We demonstrate that a customized tip's well-defined geometry, tall tip height, and aspect ratio enable improved measurement of elastic moduli by allowing access to low-laying portions of tall cells (T lymphocytes). This technique can be generally used to attach tips to any micromechanical device when conventional lithography of tips cannot be accomplished.« less

Nanoscale electrical property studies of individual GeSi quantum rings by conductive scanning probe microscopy.

PubMed

Lv, Yi; Cui, Jian; Jiang, Zuimin M; Yang, Xinju

2012-11-29

The nanoscale electrical properties of individual self-assembled GeSi quantum rings (QRs) were studied by scanning probe microscopy-based techniques. The surface potential distributions of individual GeSi QRs are obtained by scanning Kelvin microscopy (SKM). Ring-shaped work function distributions are observed, presenting that the QRs' rim has a larger work function than the QRs' central hole. By combining the SKM results with those obtained by conductive atomic force microscopy and scanning capacitance microscopy, the correlations between the surface potential, conductance, and carrier density distributions are revealed, and a possible interpretation for the QRs' conductance distributions is suggested.

Probing microbubble targeting with atomic force microscopy.

PubMed

Sboros, V; Glynos, E; Ross, J A; Moran, C M; Pye, S D; Butler, M; McDicken, W N; Brown, S B; Koutsos, V

2010-10-01

Microbubble science is expanding beyond ultrasound imaging applications to biological targeting and drug/gene delivery. The characteristics of molecular targeting should be tested by a measurement system that can assess targeting efficacy and strength. Atomic force microscopy (AFM) is capable of piconewton force resolution, and is reported to measure the strength of single hydrogen bonds. An in-house targeted microbubble modified using the biotin-avidin chemistry and the CD31 antibody was used to probe cultures of Sk-Hep1 hepatic endothelial cells. We report that the targeted microbubbles provide a single distribution of adhesion forces with a median of 93pN. This interaction is assigned to the CD31 antibody-antigen unbinding event. Information on the distances between the interaction forces was obtained and could be important for future microbubble fabrication. In conclusion, the capability of single microbubbles to target cell lines was shown to be feasible with AFM.

Plant cell wall characterization using scanning probe microscopy techniques

PubMed Central

Yarbrough, John M; Himmel, Michael E; Ding, Shi-You

2009-01-01

Lignocellulosic biomass is today considered a promising renewable resource for bioenergy production. A combined chemical and biological process is currently under consideration for the conversion of polysaccharides from plant cell wall materials, mainly cellulose and hemicelluloses, to simple sugars that can be fermented to biofuels. Native plant cellulose forms nanometer-scale microfibrils that are embedded in a polymeric network of hemicelluloses, pectins, and lignins; this explains, in part, the recalcitrance of biomass to deconstruction. The chemical and structural characteristics of these plant cell wall constituents remain largely unknown today. Scanning probe microscopy techniques, particularly atomic force microscopy and its application in characterizing plant cell wall structure, are reviewed here. We also further discuss future developments based on scanning probe microscopy techniques that combine linear and nonlinear optical techniques to characterize plant cell wall nanometer-scale structures, specifically apertureless near-field scanning optical microscopy and coherent anti-Stokes Raman scattering microscopy. PMID:19703302

Scanning probe microscopy in mineralogical studies: about origin of the observed roughness of natural silica-rich glasses

NASA Astrophysics Data System (ADS)

Golubev, Ye A.; Isaenko, S. I.

2017-10-01

We have studied different mineralogical objects: natural glasses of impact (tektites, impactites) and volcanic (obsidians) origin, using atomic force microscopy, X-ray microanalysis, infrared and Raman spectroscopy. The spectroscopy showed the difference in the structure and chemical composition of the glasses of different origin. The analysis of the dependence of nanoscale heterogeneity of the glasses, revealed by the atomic force microscopy, on their structural and chemical features was carried out.

Single molecular dynamic interactions between glycophorin A and lectin as probed by atomic force microscopy.

PubMed

Yan, Chao; Yersin, Alexandre; Afrin, Rehana; Sekiguchi, Hiroshi; Ikai, Atsushi

2009-09-01

Glycophorin A (GpA) is one of the most abundant transmembrane proteins in human erythrocytes and its interaction with lectins has been studied as model systems for erythrocyte related biological processes. We performed a force measurement study using the force mode of atomic force microscopy (AFM) to investigate the single molecular level biophysical mechanisms involved in GpA-lectin interactions. GpA was mounted on a mica surface or natively presented on the erythrocyte membrane and probed with an AFM tip coated with the monomeric but multivalent Psathyrella velutina lectin (PVL) through covalent crosslinkers. A dynamic force spectroscopy study revealed similar interaction properties in both cases, with the unbinding force centering around 60 pN with a weak loading rate dependence. Hence we identified the presence of one energy barrier in the unbinding process. Force profile analysis showed that more than 70% of GpAs are free of cytoskeletal associations in agreement with previous reports.

Near-field deformation of a liquid interface by atomic force microscopy.

PubMed

Mortagne, C; Chireux, V; Ledesma-Alonso, R; Ogier, M; Risso, F; Ondarçuhu, T; Legendre, D; Tordjeman, Ph

2017-07-01

We experiment the interaction between a liquid puddle and a spherical probe by Atomic Force Microscopy (AFM) for a probe radius R ranging from 10 nm to 30 μm. We have developed a new experimental setup by coupling an AFM with a high-speed camera and an inverted optical microscope. Interaction force-distance curves (in contact mode) and frequency shift-distance curves (in frequency modulation mode) are measured for different bulk model liquids for which the probe-liquid Hamaker constant H_{pl} is known. The experimental results, analyzed in the frame of the theoretical model developed in Phys. Rev. Lett. 108, 106104 (2012)PRLTAO0031-900710.1103/PhysRevLett.108.106104 and Phys. Rev. E 85, 061602 (2012)PLEEE81539-375510.1103/PhysRevE.85.061602, allow to determine the "jump-to-contact" critical distance d_{min} below which the liquid jumps and wets the probe. Comparison between theory and experiments shows that the probe-liquid interaction at nanoscale is controlled by the liquid interface deformation. This work shows a very good agreement between the theoretical model and the experiments and paves the way to experimental studies of liquids at the nanoscale.

Near-field deformation of a liquid interface by atomic force microscopy

NASA Astrophysics Data System (ADS)

Mortagne, C.; Chireux, V.; Ledesma-Alonso, R.; Ogier, M.; Risso, F.; Ondarçuhu, T.; Legendre, D.; Tordjeman, Ph.

2017-07-01

We experiment the interaction between a liquid puddle and a spherical probe by Atomic Force Microscopy (AFM) for a probe radius R ranging from 10 nm to 30 μ m . We have developed a new experimental setup by coupling an AFM with a high-speed camera and an inverted optical microscope. Interaction force-distance curves (in contact mode) and frequency shift-distance curves (in frequency modulation mode) are measured for different bulk model liquids for which the probe-liquid Hamaker constant Hp l is known. The experimental results, analyzed in the frame of the theoretical model developed in Phys. Rev. Lett. 108, 106104 (2012), 10.1103/PhysRevLett.108.106104 and Phys. Rev. E 85, 061602 (2012), 10.1103/PhysRevE.85.061602, allow to determine the "jump-to-contact" critical distance dmin below which the liquid jumps and wets the probe. Comparison between theory and experiments shows that the probe-liquid interaction at nanoscale is controlled by the liquid interface deformation. This work shows a very good agreement between the theoretical model and the experiments and paves the way to experimental studies of liquids at the nanoscale.

Quantification of surface displacements and electromechanical phenomena via dynamic atomic force microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Balke, Nina; Jesse, Stephen; Yu, Pu

Detection of dynamic surface displacements associated with local changes in material strain provides access to a number of phenomena and material properties. Contact resonance-enhanced methods of atomic force microscopy (AFM) have been shown capable of detecting ~1–3 pm-level surface displacements, an approach used in techniques such as piezoresponse force microscopy, atomic force acoustic microscopy, and ultrasonic force microscopy. Here, based on an analytical model of AFM cantilever vibrations, we demonstrate a guideline to quantify surface displacements with high accuracy by taking into account the cantilever shape at the first resonant contact mode, depending on the tip–sample contact stiffness. The approachmore » has been experimentally verified and further developed for piezoresponse force microscopy (PFM) using well-defined ferroelectric materials. These results open up a way to accurate and precise measurements of surface displacement as well as piezoelectric constants at the pm-scale with nanometer spatial resolution and will allow avoiding erroneous data interpretations and measurement artifacts. Furthermore, this analysis is directly applicable to all cantilever-resonance-based scanning probe microscopy (SPM) techniques.« less

Quantification of surface displacements and electromechanical phenomena via dynamic atomic force microscopy

DOE PAGES

Balke, Nina; Jesse, Stephen; Yu, Pu; ...

2016-09-15

Detection of dynamic surface displacements associated with local changes in material strain provides access to a number of phenomena and material properties. Contact resonance-enhanced methods of atomic force microscopy (AFM) have been shown capable of detecting ~1–3 pm-level surface displacements, an approach used in techniques such as piezoresponse force microscopy, atomic force acoustic microscopy, and ultrasonic force microscopy. Here, based on an analytical model of AFM cantilever vibrations, we demonstrate a guideline to quantify surface displacements with high accuracy by taking into account the cantilever shape at the first resonant contact mode, depending on the tip–sample contact stiffness. The approachmore » has been experimentally verified and further developed for piezoresponse force microscopy (PFM) using well-defined ferroelectric materials. These results open up a way to accurate and precise measurements of surface displacement as well as piezoelectric constants at the pm-scale with nanometer spatial resolution and will allow avoiding erroneous data interpretations and measurement artifacts. Furthermore, this analysis is directly applicable to all cantilever-resonance-based scanning probe microscopy (SPM) techniques.« less

Investigating biomolecular recognition at the cell surface using atomic force microscopy.

PubMed

Wang, Congzhou; Yadavalli, Vamsi K

2014-05-01

Probing the interaction forces that drive biomolecular recognition on cell surfaces is essential for understanding diverse biological processes. Force spectroscopy has been a widely used dynamic analytical technique, allowing measurement of such interactions at the molecular and cellular level. The capabilities of working under near physiological environments, combined with excellent force and lateral resolution make atomic force microscopy (AFM)-based force spectroscopy a powerful approach to measure biomolecular interaction forces not only on non-biological substrates, but also on soft, dynamic cell surfaces. Over the last few years, AFM-based force spectroscopy has provided biophysical insight into how biomolecules on cell surfaces interact with each other and induce relevant biological processes. In this review, we focus on describing the technique of force spectroscopy using the AFM, specifically in the context of probing cell surfaces. We summarize recent progress in understanding the recognition and interactions between macromolecules that may be found at cell surfaces from a force spectroscopy perspective. We further discuss the challenges and future prospects of the application of this versatile technique. Copyright © 2014 Elsevier Ltd. All rights reserved.

Non-invasive current and voltage imaging techniques for integrated circuits using scanning probe microscopy. Final report, LDRD Project FY93 and FY94

DOE Office of Scientific and Technical Information (OSTI.GOV)

Campbell, A.N.; Cole, E.I. Jr.; Tangyunyong, Paiboon

This report describes the first practical, non-invasive technique for detecting and imaging currents internal to operating integrated circuits (ICs). This technique is based on magnetic force microscopy and was developed under Sandia National Laboratories` LDRD (Laboratory Directed Research and Development) program during FY 93 and FY 94. LDRD funds were also used to explore a related technique, charge force microscopy, for voltage probing of ICs. This report describes the technical work performed under this LDRD as well as the outcomes of the project in terms of publications and awards, intellectual property and licensing, synergistic work, potential future work, hiring ofmore » additional permanent staff, and benefits to DOE`s defense programs (DP).« less

Nanofabrication technique based on localized photocatalytic reactions using a TiO2-coated atomic force microscopy probe

NASA Astrophysics Data System (ADS)

Shibata, Takayuki; Iio, Naohiro; Furukawa, Hiromi; Nagai, Moeto

2017-02-01

We performed a fundamental study on the photocatalytic degradation of fluorescently labeled DNA molecules immobilized on titanium dioxide (TiO2) thin films under ultraviolet irradiation. The films were prepared by the electrochemical anodization of Ti thin films sputtered on silicon substrates. We also confirmed that the photocurrent arising from the photocatalytic oxidation of DNA molecules can be detected during this process. We then demonstrated an atomic force microscopy (AFM)-based nanofabrication technique by employing TiO2-coated AFM probes to penetrate living cell membranes under near-physiological conditions for minimally invasive intracellular delivery.

Characterisation of adhesional properties of lactose carriers using atomic force microscopy.

PubMed

Louey, M D; Mulvaney, P; Stewart, P J

2001-06-01

The atomic force microscopy (AFM) colloid probe technique was investigated as a method for the characterisation of adhesional properties of pharmaceutical powder surfaces. Lactose carriers used in dry powder inhaler (DPI) formulations were chosen for investigation since adhesion between the carrier surface and drug particles has been proposed to affect the dispersion of drug particles. Individual adhesion forces were determined by measuring the detachment forces in air between the colloid probe and the lactose particle surface. The colloid probe consisted of a silica sphere (10 microm diameter) attached to a V-shaped silicon nitride cantilever (spring constant, k=0.42 N/m). Adhesion forces were calculated from individual force-distance curves using Hooke's Law. Individual forces measured at various adhesion sites were observed to be reproducible and stable over 10 min (coefficient of variation, CV below 5%). The adhesion force distribution determined from measurements at multiple sites (n>50) on each sample followed a log-normal relationship (regression coefficient, r(2) ranged between 0.95 and 0.99). This enabled characterisation in terms of the geometric mean adhesion force and a geometric standard deviation (GSD). Significant differences (P<0.001) in adhesion force were observed between samples, ranging from 37.47+/-1.95 to 117.48+/-2.20 nN. This study demonstrates the suitability of AFM as sensitive technique for the characterisation of adhesional properties of pharmaceutical particles.

Effect of the tip state during qPlus noncontact atomic force microscopy of Si(100) at 5 K: Probing the probe

PubMed Central

Jarvis, Sam; Danza, Rosanna; Moriarty, Philip

2012-01-01

Summary Background: Noncontact atomic force microscopy (NC-AFM) now regularly produces atomic-resolution images on a wide range of surfaces, and has demonstrated the capability for atomic manipulation solely using chemical forces. Nonetheless, the role of the tip apex in both imaging and manipulation remains poorly understood and is an active area of research both experimentally and theoretically. Recent work employing specially functionalised tips has provided additional impetus to elucidating the role of the tip apex in the observed contrast. Results: We present an analysis of the influence of the tip apex during imaging of the Si(100) substrate in ultra-high vacuum (UHV) at 5 K using a qPlus sensor for noncontact atomic force microscopy (NC-AFM). Data demonstrating stable imaging with a range of tip apexes, each with a characteristic imaging signature, have been acquired. By imaging at close to zero applied bias we eliminate the influence of tunnel current on the force between tip and surface, and also the tunnel-current-induced excitation of silicon dimers, which is a key issue in scanning probe studies of Si(100). Conclusion: A wide range of novel imaging mechanisms are demonstrated on the Si(100) surface, which can only be explained by variations in the precise structural configuration at the apex of the tip. Such images provide a valuable resource for theoreticians working on the development of realistic tip structures for NC-AFM simulations. Force spectroscopy measurements show that the tip termination critically affects both the short-range force and dissipated energy. PMID:22428093

Bubble colloidal AFM probes formed from ultrasonically generated bubbles.

PubMed

Vakarelski, Ivan U; Lee, Judy; Dagastine, Raymond R; Chan, Derek Y C; Stevens, Geoffrey W; Grieser, Franz

2008-02-05

Here we introduce a simple and effective experimental approach to measuring the interaction forces between two small bubbles (approximately 80-140 microm) in aqueous solution during controlled collisions on the scale of micrometers to nanometers. The colloidal probe technique using atomic force microscopy (AFM) was extended to measure interaction forces between a cantilever-attached bubble and surface-attached bubbles of various sizes. By using an ultrasonic source, we generated numerous small bubbles on a mildly hydrophobic surface of a glass slide. A single bubble picked up with a strongly hydrophobized V-shaped cantilever was used as the colloidal probe. Sample force measurements were used to evaluate the pure water bubble cleanliness and the general consistency of the measurements.

Single-Cell Force Spectroscopy of Probiotic Bacteria

PubMed Central

Beaussart, Audrey; El-Kirat-Chatel, Sofiane; Herman, Philippe; Alsteens, David; Mahillon, Jacques; Hols, Pascal; Dufrêne, Yves F.

2013-01-01

Single-cell force spectroscopy is a powerful atomic force microscopy modality in which a single living cell is attached to the atomic force microscopy cantilever to quantify the forces that drive cell-cell and cell-substrate interactions. Although various single-cell force spectroscopy protocols are well established for animal cells, application of the method to individual bacterial cells remains challenging, mainly owing to the lack of appropriate methods for the controlled attachment of single live cells on cantilevers. We present a nondestructive protocol for single-bacterial cell force spectroscopy, which combines the use of colloidal probe cantilevers and of a bioinspired polydopamine wet adhesive. Living cells from the probiotic species Lactobacillus plantarum are picked up with a polydopamine-coated colloidal probe, enabling us to quantify the adhesion forces between single bacteria and biotic (lectin monolayer) or abiotic (hydrophobic monolayer) surfaces. These minimally invasive single-cell experiments provide novel, to our knowledge, insight into the specific and nonspecific forces driving the adhesion of L. plantarum, and represent a generic platform for studying the molecular mechanisms of cell adhesion in probiotic and pathogenic bacteria. PMID:23663831

Numerical simulations for quantitative analysis of electrostatic interaction between atomic force microscopy probe and an embedded electrode within a thin dielectric: meshing optimization, sensitivity to potential distribution and impact of cantilever contribution

NASA Astrophysics Data System (ADS)

Azib, M.; Baudoin, F.; Binaud, N.; Villeneuve-Faure, C.; Bugarin, F.; Segonds, S.; Teyssedre, G.

2018-04-01

Recent experimental results demonstrated that an electrostatic force distance curve (EFDC) can be used for space charge probing in thin dielectric layers. A main advantage of the method is claimed to be its sensitivity to charge localization, which, however, needs to be substantiated by numerical simulations. In this paper, we have developed a model which permits us to compute an EFDC accurately by using the most sophisticated and accurate geometry for the atomic force microscopy probe. To avoid simplifications and in order to reproduce experimental conditions, the EFDC has been simulated for a system constituted of a polarized electrode embedded in a thin dielectric layer (SiN x ). The individual contributions of forces on the tip and on the cantilever have been analyzed separately to account for possible artefacts. The EFDC sensitivity to potential distribution is studied through the change in electrode shape, namely the width and the depth. Finally, the numerical results have been compared with experimental data.

Sensing mode atomic force microscope

DOEpatents

Hough, Paul V. C.; Wang, Chengpu

2006-08-22

An atomic force microscope is described having a cantilever comprising a base and a probe tip on an end opposite the base; a cantilever drive device connected to the base; a magnetic material coupled to the probe tip, such that when an incrementally increasing magnetic field is applied to the magnetic material an incrementally increasing force will be applied to the probe tip; a moveable specimen base; and a controller constructed to obtain a profile height of a specimen at a point based upon a contact between the probe tip and a specimen, and measure an adhesion force between the probe tip and the specimen by, under control of a program, incrementally increasing an amount of a magnetic field until a release force, sufficient to break the contact, is applied. An imaging method for atomic force microscopy involving measuring a specimen profile height and adhesion force at multiple points within an area and concurrently displaying the profile and adhesion force for each of the points is also described. A microscope controller is also described and is constructed to, for a group of points, calculate a specimen height at a point based upon a cantilever deflection, a cantilever base position and a specimen piezo position; calculate an adhesion force between a probe tip and a specimen at the point by causing an incrementally increasing force to be applied to the probe tip until the probe tip separates from a specimen; and move the probe tip to a new point in the group.

Sensing mode atomic force microscope

DOEpatents

Hough, Paul V.; Wang, Chengpu

2004-11-16

An atomic force microscope is described having a cantilever comprising a base and a probe tip on an end opposite the base; a cantilever drive device connected to the base; a magnetic material coupled to the probe tip, such that when an incrementally increasing magnetic field is applied to the magnetic material an incrementally increasing force will be applied to the probe tip; a moveable specimen base; and a controller constructed to obtain a profile height of a specimen at a point based upon a contact between the probe tip and a specimen, and measure an adhesion force between the probe tip and the specimen by, under control of a program, incrementally increasing an amount of a magnetic field until a release force, sufficient to break the contact, is applied. An imaging method for atomic force microscopy involving measuring a specimen profile height and adhesion force at multiple points within an area and concurrently displaying the profile and adhesion force for each of the points is also described. A microscope controller is also described and is constructed to, for a group of points, calculate a specimen height at a point based upon a cantilever deflection, a cantilever base position and a specimen piezo position; calculate an adhesion force between a probe tip and a specimen at the point by causing an incrementally increasing force to be applied to the probe tip until the probe tip separates from a specimen; and move the probe tip to a new point in the group.

Learning about Modes in Atomic Force Microscopy by Means of Hands-On Activities Based on a Simple Apparatus

ERIC Educational Resources Information Center

Phuapaiboon, Unchada; Panijpan, Bhinyo; Osotchan, Tanakorn

2009-01-01

This study was conducted to examine the results of using a low-cost hands-on setup in combination with accompanying activities to promote understanding of the contact mode of atomic force microscopy (AFM). This contact mode setup enabled learners to study how AFM works by hand scanning using probing cantilevers with different characteristics on…

Corrosion study of AA2024-T3 by scanning Kelvin probe force microscopy and in situ atomic force microscopy scratching

DOE Office of Scientific and Technical Information (OSTI.GOV)

Schmutz, P.; Frankel, G.S.

1998-07-01

The localized corrosion of AA2024-T3, and the behavior of intermetallic particles in particular, were studied using different capabilities of the atomic force microscope (AFM). The role of intermetallic particles in determining the locations and rates of localized corrosion was determined using scanning Kelvin probe force microscopy in air after exposure to chloride solutions. Al-Cu-Mg particles, which have a noble Volta potential in air because of an altered surface film, are actively dissolved in chloride solution after a certain induction time. Al-Cu(Fe, Mn) particles are heterogeneous in nature and exhibit nonuniform dissolution in chloride solution as well as trenching of themore » matrix around the particles. Light scratching of the surface by rastering with the AFM tip in contact mode in chloride solution results in accelerated dissolution of both pure Al and alloy 2024-T3. The abrasion associated with contact AFM in situ resulted in the immediate dissolution of the Al-Cu-Mg particles because of a destabilization of the surface film.« less

Single-molecule height measurements on microsomal cytochrome P450 in nanometer-scale phospholipid bilayer disks

NASA Astrophysics Data System (ADS)

Bayburt, Timothy H.; Sligar, Stephen G.

2002-05-01

The architecture of membrane proteins in their native environment of the phospholipid bilayer is critical for understanding physiological function, but has been difficult to realize experimentally. In this communication we describe the incorporation of a membrane-anchored protein into a supported phospholipid bilayer. Cytochrome P450 2B4 solubilized and purified from the hepatic endoplasmic reticulum was incorporated into phospholipid bilayer nanostructures and oriented on a surface for visualization by atomic force microscopy. Individual P450 molecules were observed protruding from the bilayer surface. Problems associated with deformation of the protein by the atomic force microscopy probe were avoided by analyzing force-dependent height measurements to quantitate the height of the protein above the bilayer surface. Measurements of the atomic force microscopy cantilever deflection as a function of probe-sample separation reveal that the top of the P450 opposite the N-terminal membrane anchor region sits 3.5 nanometers above the phospholipid-water boundary. Models of the orientation of the enzyme are presented and discussed in relation to membrane interactions and interaction with cytochrome P450 reductase.

Real-space measurement of potential distribution in PECVD ONO electrets by Kelvin probe force microscopy.

PubMed

Emmerich, F; Thielemann, C

2016-05-20

Multilayers of silicon oxide/silicon nitride/silicon oxide (ONO) are known for their good electret properties due to deep energy traps near the material interfaces, facilitating charge storage. However, measurement of the space charge distribution in such multilayers is a challenge for conventional methods if layer thickness dimensions shrink below 1 μm. In this paper, we propose an atomic force microscope based method to determine charge distributions in ONO layers with spatial resolution below 100 nm. By applying Kelvin probe force microscopy (KPFM) on freshly cleaved, corona-charged multilayers, the surface potential is measured directly along the z-axis and across the interfaces. This new method gives insights into charge distribution and charge movement in inorganic electrets with a high spatial resolution.

Study of electromechanical and mechanical properties of bacteria using force microscopy

NASA Astrophysics Data System (ADS)

Reukov, Vladimir; Thompson, Gary; Nikiforov, Maxim; Guo, Senli; Ovchinnikov, Oleg; Jesse, Stephen; Kalinin, Sergei; Vertegel, Alexey

2010-03-01

The application of scanning probe microscopy (SPM) to biological systems has evolved over the past decade into a multimodal and spectroscopic instrument that provides multiple information channels at each spatial pixel acquired. Recently, functional recognition imaging based on differing electromechanical properties between Gram negative and Gram positive bacteria was achieved using artificial neural network analysis of band excitation piezoresponse force microscopy (BEPFM) data. The immediate goal of this project was to study mechanical and electromechanical properties of bacterial systems physiologically-relevant solutions using Band-width Excitation Piezoresponce Force Microscopy (BE PFM) in combination with Force Mapping. Electromechanical imaging in physiological environments will improve the versatility of functional recognition imaging and open the way for application of the rapid BEPFM line mode method to other living cell systems.

Direct determination of the local Hamaker constant of inorganic surfaces based on scanning force microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Krajina, Brad A.; Kocherlakota, Lakshmi S.; Overney, René M., E-mail: roverney@u.washington.edu

The energetics involved in the bonding fluctuations between nanometer-sized silicon dioxide (SiO{sub 2}) probes and highly oriented pyrolytic graphite (HOPG) and molybdenum disulfide (MoS{sub 2}) could be quantified directly and locally on the submicron scale via a time-temperature superposition analysis of the lateral forces between scanning force microscopy silicon dioxide probes and inorganic sample surfaces. The so-called “intrinsic friction analysis” (IFA) provided direct access to the Hamaker constants for HOPG and MoS{sub 2}, as well as the control sample, calcium fluoride (CaF{sub 2}). The use of scanning probe enables nanoscopic analysis of bonding fluctuations, thereby overcoming challenges associated with largermore » scale inhomogeneity and surface roughness common to conventional techniques used to determine surface free energies and dielectric properties. A complementary numerical analysis based on optical and electron energy loss spectroscopy and the Lifshitz quantum electrodynamic theory of van der Waals interactions is provided and confirms quantitatively the IFA results.« less

Direct determination of the local Hamaker constant of inorganic surfaces based on scanning force microscopy

NASA Astrophysics Data System (ADS)

Krajina, Brad A.; Kocherlakota, Lakshmi S.; Overney, René M.

2014-10-01

The energetics involved in the bonding fluctuations between nanometer-sized silicon dioxide (SiO2) probes and highly oriented pyrolytic graphite (HOPG) and molybdenum disulfide (MoS2) could be quantified directly and locally on the submicron scale via a time-temperature superposition analysis of the lateral forces between scanning force microscopy silicon dioxide probes and inorganic sample surfaces. The so-called "intrinsic friction analysis" (IFA) provided direct access to the Hamaker constants for HOPG and MoS2, as well as the control sample, calcium fluoride (CaF2). The use of scanning probe enables nanoscopic analysis of bonding fluctuations, thereby overcoming challenges associated with larger scale inhomogeneity and surface roughness common to conventional techniques used to determine surface free energies and dielectric properties. A complementary numerical analysis based on optical and electron energy loss spectroscopy and the Lifshitz quantum electrodynamic theory of van der Waals interactions is provided and confirms quantitatively the IFA results.

Direct determination of the local Hamaker constant of inorganic surfaces based on scanning force microscopy.

PubMed

Krajina, Brad A; Kocherlakota, Lakshmi S; Overney, René M

2014-10-28

The energetics involved in the bonding fluctuations between nanometer-sized silicon dioxide (SiO2) probes and highly oriented pyrolytic graphite (HOPG) and molybdenum disulfide (MoS2) could be quantified directly and locally on the submicron scale via a time-temperature superposition analysis of the lateral forces between scanning force microscopy silicon dioxide probes and inorganic sample surfaces. The so-called "intrinsic friction analysis" (IFA) provided direct access to the Hamaker constants for HOPG and MoS2, as well as the control sample, calcium fluoride (CaF2). The use of scanning probe enables nanoscopic analysis of bonding fluctuations, thereby overcoming challenges associated with larger scale inhomogeneity and surface roughness common to conventional techniques used to determine surface free energies and dielectric properties. A complementary numerical analysis based on optical and electron energy loss spectroscopy and the Lifshitz quantum electrodynamic theory of van der Waals interactions is provided and confirms quantitatively the IFA results.

Transfer doping of single isolated nanodiamonds, studied by scanning probe microscopy techniques.

PubMed

Bolker, Asaf; Saguy, Cecile; Kalish, Rafi

2014-09-26

The transfer doping of diamond surfaces has been applied in various novel two-dimensional electronic devices. Its extension to nanodiamonds (ND) is essential for ND-based applications in many fields. In particular, understanding the influence of the crystallite size on transfer doping is desirable. Here, we report the results of a detailed study of the electronic energetic band structure of single, isolated transfer-doped nanodiamonds with nanometric resolution using a combination of scanning tunneling spectroscopy and Kelvin force microscopy measurements. The results show how the band gap, the valence band maximum, the electron affinity and the work function all depend on the ND's size and nanoparticle surface properties. The present analysis, which combines information from both scanning tunneling spectroscopy and Kelvin force microscopy, should be applicable to any nanoparticle or surface that can be measured with scanning probe techniques.

The application of atomic force microscopy in mineral flotation.

PubMed

Xing, Yaowen; Xu, Mengdi; Gui, Xiahui; Cao, Yijun; Babel, Bent; Rudolph, Martin; Weber, Stefan; Kappl, Michael; Butt, Hans-Jürgen

2018-06-01

During the past years, atomic force microscopy (AFM) has matured to an indispensable tool to characterize nanomaterials in colloid and interface science. For imaging, a sharp probe mounted near to the end of a cantilever scans over the sample surface providing a high resolution three-dimensional topographic image. In addition, the AFM tip can be used as a force sensor to detect local properties like adhesion, stiffness, charge etc. After the invention of the colloidal probe technique it has also become a major method to measure surface forces. In this review, we highlight the advances in the application of AFM in the field of mineral flotation, such as mineral morphology imaging, water at mineral surface, reagent adsorption, inter-particle force, and bubble-particle interaction. In the coming years, the complementary characterization of chemical composition such as using infrared spectroscopy and Raman spectroscopy for AFM topography imaging and the synchronous measurement of the force and distance involving deformable bubble as a force sensor will further assist the fundamental understanding of flotation mechanism. Copyright © 2018 Elsevier B.V. All rights reserved.

Scanning Probe Microscopies and Their Applications Towards the Study of Superconductors

NASA Astrophysics Data System (ADS)

Helfrich, Jennifer Ann

1995-11-01

The invention of the scanning tunneling microscope (STM) in 1982 made it possible to study surfaces and structures at resolutions previously believed unattainable. Adapting the STM for low temperatures makes it possible to study superconductors with new methods and to obtain valuable information. This thesis describes a novel low temperature STM (LTSTM) that was designed and built at Northwestern University for the purpose of studying superconductors in the mixed state. At low temperatures, this LTSTM has a scan range an order of magnitude larger than other LTSTM's designed elsewhere. It is capable of low temperature imaging and obtaining dI/dV vs. V curves. A detailed study of magnetic force microscopy (MFM) probes is also presented. The fields and forces between probe and surface were computer modeled. These results are compared with results from electron holographs of MFM probes. The final section of the thesis describes an a.c. susceptibility measurement on a UPt_3 sphere. Results are presented and discussed.

Thermally oxidized Inconel 600 and 690 nickel-based alloys characterizations by combination of global photoelectrochemistry and local near-field microscopy techniques (STM, STS, AFM, SKPFM)

NASA Astrophysics Data System (ADS)

Mechehoud, F.; Benaioun, N. E.; Hakiki, N. E.; Khelil, A.; Simon, L.; Bubendorff, J. L.

2018-03-01

Thermally oxidized nickel-based alloys are studied by scanning tunnelling microscopy (STM), scanning tunnelling spectroscopy (STS), atomic force microscopy (AFM), scanning kelvin probe force microscopy (SKPFM) and photoelectro-chemical techniques as a function of oxidation time at a fixed temperature of 623 K. By photoelectrochemistry measurements we identify the formation of three oxides NiO, Fe2O3, Cr2O3 and determine the corresponding gap values. We use these values as parameter for imaging the surface at high bias voltage by STM allowing the spatial localization and identification of both NiO, Fe2O3 oxide phases using STS measurements. Associated to Kelvin probe measurements we show also that STS allow to distinguished NiO from Cr2O3 and confirm that the Cr2O3 is not visible at the surface and localized at the oxide/steel interface.

Iron-platinum-coated carbon nanocone probes on tipless cantilevers for high resolution magnetic force imaging.

PubMed

Chen, I-Chen; Chen, Li-Han; Gapin, Andrew; Jin, Sungho; Yuan, Lu; Liou, Sy-Hwang

2008-02-20

High coercivity iron-platinum-coated carbon nanocones (CNCs) have been fabricated for magnetic force microscopy (MFM) by direct-current plasma-enhanced chemical vapor deposition growth of nanocones on tipless cantilevers followed by sputtering and annealing of the FePt film. The FePt-coated CNC probe has many localized magnetic stray fields due to the high-aspect-ratio geometry and small radius of the tip. The MFM imaging on magnetic recording media was performed using CNC probes and compared with the imaging by FePt-coated silicon probes. An image with 20 nm lateral resolution has been demonstrated.

Attachment of micro- and nano-particles on tipless cantilevers for colloidal probe microscopy.

PubMed

D'Sa, Dexter J; Chan, Hak-Kim; Chrzanowski, Wojciech

2014-07-15

Current colloidal probe preparation techniques face several challenges in the production of functional probes using particles ⩽5 μm. Challenges include: glue encapsulated particles, glue altered particle properties, improper particle or agglomerate attachment, and lengthy procedures. We present a method to rapidly and reproducibly produce functional micro and nano-colloidal probes. Using a six-step procedure, cantilevers mounted on a custom designed 45° holder were used to approach and obtain a minimal amount of epoxy resin (viscosity of ∼14,000 cP) followed by a single micron/nano particle on the apex of a tipless cantilever. The epoxy and particles were prepared on individual glass slides and subsequently affixed to a 10× or 40× optical microscope lens using another custom designed holder. Scanning electron microscopy and comparative glue-colloidal probe measurements were used to confirm colloidal probe functionality. The method presented allowed rapid and reproducible production of functional colloidal probes (80% success). Single nano-particles were prominently affixed to the apex of the cantilever, unaffected by the epoxy. Nano-colloidal probes were used to conduct topographical, instantaneous force, and adhesive force mapping measurements in dry and liquid media conveying their versatility and functionality in studying nano-colloidal systems. Copyright © 2014 Elsevier Inc. All rights reserved.

Multifrequency spectrum analysis using fully digital G Mode-Kelvin probe force microscopy.

PubMed

Collins, Liam; Belianinov, Alex; Somnath, Suhas; Rodriguez, Brian J; Balke, Nina; Kalinin, Sergei V; Jesse, Stephen

2016-03-11

Since its inception over two decades ago, Kelvin probe force microscopy (KPFM) has become the standard technique for characterizing electrostatic, electrochemical and electronic properties at the nanoscale. In this work, we present a purely digital, software-based approach to KPFM utilizing big data acquisition and analysis methods. General mode (G-Mode) KPFM works by capturing the entire photodetector data stream, typically at the sampling rate limit, followed by subsequent de-noising, analysis and compression of the cantilever response. We demonstrate that the G-Mode approach allows simultaneous multi-harmonic detection, combined with on-the-fly transfer function correction-required for quantitative CPD mapping. The KPFM approach outlined in this work significantly simplifies the technique by avoiding cumbersome instrumentation optimization steps (i.e. lock in parameters, feedback gains etc), while also retaining the flexibility to be implemented on any atomic force microscopy platform. We demonstrate the added advantages of G-Mode KPFM by allowing simultaneous mapping of CPD and capacitance gradient (C') channels as well as increased flexibility in data exploration across frequency, time, space, and noise domains. G-Mode KPFM is particularly suitable for characterizing voltage sensitive materials or for operation in conductive electrolytes, and will be useful for probing electrodynamics in photovoltaics, liquids and ionic conductors.

Multifrequency spectrum analysis using fully digital G Mode-Kelvin probe force microscopy

DOE PAGES

Collins, Liam F.; Jesse, Stephen; Belianinov, Alex; ...

2016-02-11

Since its inception over two decades ago, Kelvin probe force microscopy (KPFM) has become the standard technique for characterizing electrostatic, electrochemical and electronic properties at the nanoscale. In this work, we present a purely digital, software-based approach to KPFM utilizing big data acquisition and analysis methods. General Mode (G-Mode) KPFM, works by capturing the entire photodetector data stream, typically at the sampling rate limit, followed by subsequent de-noising, analysis and compression of the cantilever response. We demonstrate that the G-Mode approach allows simultaneous multi-harmonic detection, combined with on-the-fly transfer function correction required for quantitative CPD mapping. The KPFM approach outlinedmore » in this work significantly simplifies the technique by avoiding cumbersome instrumentation optimization steps (i.e. lock in parameters, feedback gains etc.), while also retaining the flexibility to be implemented on any atomic force microscopy platform. We demonstrate the added advantages of G-Mode KPFM by allowing simultaneous mapping of CPD and capacitance gradient (C') channels as well as increased flexibility in data exploration across frequency, time, space, and noise domains. As a result, G-Mode KPFM is particularly suitable for characterizing voltage sensitive materials or for operation in conductive electrolytes, and will be useful for probing electrodynamics in photovoltaics, liquids and ionic conductors.« less

Scanning probe microscopy for the analysis of composite Ti/hydrocarbon plasma polymer thin films

NASA Astrophysics Data System (ADS)

Choukourov, A.; Grinevich, A.; Slavinska, D.; Biederman, H.; Saito, N.; Takai, O.

2008-03-01

Composite Ti/hydrocarbon plasma polymer films with different Ti concentration were deposited on silicon by dc magnetron sputtering of titanium in an atmosphere of argon and hexane. As measured by Kelvin force microscopy and visco-elastic atomic force microscopy, respectively, surface potential and hardness increase with increasing Ti content. Adhesion force to silicon and to fibrinogen molecules was stronger for the Ti-rich films as evaluated from the AFM force-distance curves. Fibrinogen forms a very soft layer on these composites with part of the protein molecules embedded in the outermost region of the plasma polymer. An increase of the surface charge due to fibrinogen adsorption has been observed and attributed to positively charged αC domains of fibrinogen molecule.

Characterisation of dry powder inhaler formulations using atomic force microscopy.

PubMed

Weiss, Cordula; McLoughlin, Peter; Cathcart, Helen

2015-10-15

Inhalation formulations are a popular way of treating the symptoms of respiratory diseases. The active pharmaceutical ingredient (API) is delivered directly to the site of action within the deep lung using an inhalation device such as the dry powder inhaler (DPI). The performance of the formulation and the efficiency of the treatment depend on a number of factors including the forces acting between the components. In DPI formulations these forces are dominated by interparticulate interactions. Research has shown that adhesive and cohesive forces depend on a number of particulate properties such as size, surface roughness, crystallinity, surface energetics and combinations of these. With traditional methods the impact of particulate properties on interparticulate forces could be evaluated by examining the bulk properties. Atomic force microscopy (AFM), however, enables the determination of local surface characteristics and the direct measurement of interparticulate forces using the colloidal probe technique. AFM is considered extremely useful for evaluating the surface topography of a substrate (an API or carrier particle) and even allows the identification of crystal faces, defects and polymorphs from high-resolution images. Additionally, information is given about local mechanical properties of the particles and changes in surface composition and energetics. The assessment of attractive forces between two bodies is possible by using colloidal probe AFM. This review article summarises the application of AFM in DPI formulations while specifically focussing on the colloidal probe technique and the evaluation of interparticulate forces. Copyright © 2015 Elsevier B.V. All rights reserved.

Electrochemically assisted localized etching of ZnO single crystals in water using a catalytically active Pt-coated atomic force microscopy probe

NASA Astrophysics Data System (ADS)

Shibata, Takayuki; Yamamoto, Kota; Sasano, Junji; Nagai, Moeto

2017-09-01

This paper presents a nanofabrication technique based on the electrochemically assisted chemical dissolution of zinc oxide (ZnO) single crystals in water at room temperature using a catalytically active Pt-coated atomic force microscopy (AFM) probe. Fabricated grooves featured depths and widths of several tens and several hundreds of nanometers, respectively. The material removal rate of ZnO was dramatically improved by controlling the formation of hydrogen ions (H+) on the surface of the catalytic Pt-coated probe via oxidation of H2O molecules; this reaction can be enhanced by applying a cathodic potential to an additional Pt-wire working electrode in a three-electrode configuration. Consequently, ZnO can be dissolved chemically in water as a soluble Zn2+ species via a reaction with H+ species present in high concentrations in the immediate vicinity of the AFM tip apex.

Electrocatalysis-induced elasticity modulation in a superionic proton conductor probed by band-excitation atomic force microscopy.

PubMed

Papandrew, A B; Li, Q; Okatan, M B; Jesse, S; Hartnett, C; Kalinin, S V; Vasudevan, R K

2015-12-21

Variable temperature band-excitation atomic force microscopy in conjunction with I-V spectroscopy was used to investigate the crystalline superionic proton conductor CsHSO4 during proton exchange induced by a Pt-coated conductive scanning probe. At a sample temperature of 150 °C and under an applied bias <1 V, reduction currents of up to 1 nA were observed. Simultaneously, we show that the electrochemical reactions are accompanied by a reversible decrease in the elastic modulus of CsHSO4, as seen by a contact resonance shift, and find evidence for superplasticity during scanning. These effects were not observed in the room-temperature phase of CsHSO4 or in the case of catalytically inactive conductive probes, proving the utility of this technique for monitoring electrochemical processes on the nanoscale, as well as the use of local contact stiffness as a sensitive indicator of electrochemical reactions.

Multifunctional hydrogel nano-probes for atomic force microscopy

PubMed Central

Lee, Jae Seol; Song, Jungki; Kim, Seong Oh; Kim, Seokbeom; Lee, Wooju; Jackman, Joshua A.; Kim, Dongchoul; Cho, Nam-Joon; Lee, Jungchul

2016-01-01

Since the invention of the atomic force microscope (AFM) three decades ago, there have been numerous advances in its measurement capabilities. Curiously, throughout these developments, the fundamental nature of the force-sensing probe—the key actuating element—has remained largely unchanged. It is produced by long-established microfabrication etching strategies and typically composed of silicon-based materials. Here, we report a new class of photopolymerizable hydrogel nano-probes that are produced by bottom-up fabrication with compressible replica moulding. The hydrogel probes demonstrate excellent capabilities for AFM imaging and force measurement applications while enabling programmable, multifunctional capabilities based on compositionally adjustable mechanical properties and facile encapsulation of various nanomaterials. Taken together, the simple, fast and affordable manufacturing route and multifunctional capabilities of hydrogel AFM nano-probes highlight the potential of soft matter mechanical transducers in nanotechnology applications. The fabrication scheme can also be readily utilized to prepare hydrogel cantilevers, including in parallel arrays, for nanomechanical sensor devices. PMID:27199165

Transfer doping of single isolated nanodiamonds, studied by scanning probe microscopy techniques

NASA Astrophysics Data System (ADS)

Bolker, Asaf; Saguy, Cecile; Kalish, Rafi

2014-09-01

The transfer doping of diamond surfaces has been applied in various novel two-dimensional electronic devices. Its extension to nanodiamonds (ND) is essential for ND-based applications in many fields. In particular, understanding the influence of the crystallite size on transfer doping is desirable. Here, we report the results of a detailed study of the electronic energetic band structure of single, isolated transfer-doped nanodiamonds with nanometric resolution using a combination of scanning tunneling spectroscopy and Kelvin force microscopy measurements. The results show how the band gap, the valence band maximum, the electron affinity and the work function all depend on the ND’s size and nanoparticle surface properties. The present analysis, which combines information from both scanning tunneling spectroscopy and Kelvin force microscopy, should be applicable to any nanoparticle or surface that can be measured with scanning probe techniques.

Multi-scale Imaging of Cellular and Sub-cellular Structures using Scanning Probe Recognition Microscopy.

NASA Astrophysics Data System (ADS)

Chen, Q.; Rice, A. F.

2005-03-01

Scanning Probe Recognition Microscopy is a new scanning probe capability under development within our group to reliably return to and directly interact with a specific nanobiological feature of interest. In previous work, we have successfully recognized and classified tubular versus globular biological objects from experimental atomic force microscope images using a method based on normalized central moments [ref. 1]. In this paper we extend this work to include recognition schemes appropriate for cellular and sub-cellular structures. Globular cells containing tubular actin filaments are under investigation. Thus there are differences in external/internal shapes and scales. Continuous Wavelet Transform with a differential Gaussian mother wavelet is employed for multi- scale analysis. [ref. 1] Q. Chen, V. Ayres and L. Udpa, ``Biological Investigation Using Scanning Probe Recognition Microscopy,'' Proceedings 3rd IEEE Conference on Nanotechnology, vol. 2, p 863-865 (2003).

Scanning Probe Microscopy of Organic Solar Cells

NASA Astrophysics Data System (ADS)

Reid, Obadiah G.

Nanostructured composites of organic semiconductors are a promising class of materials for the manufacture of low-cost solar cells. Understanding how the nanoscale morphology of these materials affects their efficiency as solar energy harvesters is crucial to their eventual potential for large-scale deployment for primary power generation. In this thesis we describe the use of optoelectronic scanning-probe based microscopy methods to study this efficiency-structure relationship with nanoscale resolution. In particular, our objective is to make spatially resolved measurements of each step in the power conversion process from photons to an electric current, including charge generation, transport, and recombination processes, and correlate them with local device structure. We have achieved two aims in this work: first, to develop and apply novel electrically sensitive scanning probe microscopy experiments to study the optoelectronic materials and processes discussed above; and second, to deepen our understanding of the physics underpinning our experimental techniques. In the first case, we have applied conductive-, and photoconductive atomic force (cAFM & pcAFM) microscopy to measure both local photocurrent collection and dark charge transport properties in a variety of model and novel organic solar cell composites, including polymer/fullerene blends, and polymer-nanowire/fullerene blends, finding that local heterogeneity is the rule, and that improvements in the uniformity of specific beneficial nanostructures could lead to large increases in efficiency. We have used scanning Kelvin probe microscopy (SKPM) and time resolved-electrostatic force microscopy (trEFM) to characterize all-polymer blends, quantifying their sensitivity to photochemical degradation and the subsequent formation of local charge traps. We find that while trEFM provides a sensitive measure of local quantum efficiency, SKPM is generally unsuited to measurements of efficiency, less sensitive than trEFM, and of greater utility in identifying local changes in steady-state charge density that can be associated with charge trapping. In the second case, we have developed a new understanding of charge transport between a sharp AFM tip and planar substrates applicable to conductive and photoconductive atomic force microscopy, and shown that hole-only transport characteristics can be easily obtained including quantitative values of the charge carrier mobility. Finally, we have shown that intensity-dependent photoconductive atomic force microscopy measurements can be used to infer the 3D structure of organic photovoltaic materials, and gained new insight into the influence vertical composition of the these devices can have on their open-circuit voltage and its intensity dependence.

Cell adhesion to borate glasses by colloidal probe microscopy.

PubMed

Wiederhorn, Sheldon M; Chae, Young-Hun; Simon, Carl G; Cahn, Jackson; Deng, Yan; Day, Delbert

2011-05-01

The adhesion of osteoblast-like cells to silicate and borate glasses was measured in cell growth medium using colloidal probe microscopy. The probes consisted of silicate and borate glass spheres, 25-50 μm in diameter, attached to atomic force microscope cantilevers. Variables of the study included glass composition and time of contact of the cell to the glasses. Increasing the time of contact from 15 to 900 s increased the force of adhesion. The data could be plotted linearly on a log-log plot of adhesive force versus time. Of the seven glasses tested, five had slopes close to 0.5, suggesting a square root dependence of the adhesive force on the contact time. Such behavior can be interpreted as a diffusion limited process occurring during the early stages of cell attachment. We suggest that the rate limiting step in the adhesion process is the diffusion of integrins resident in the cell membrane to the area of cell attachment. Data presented in this paper support the hypothesis of Hench et al. that strong adhesion depends on the formation of a calcium phosphate reaction layer on the surfaces of the glass. Glasses that did not form a calcium phosphate layer exhibited a weaker adhesive force relative to those glasses that did form a calcium phosphate layer. Published by Elsevier Ltd.

Resonant antenna probes for tip-enhanced infrared near-field microscopy.

PubMed

Huth, Florian; Chuvilin, Andrey; Schnell, Martin; Amenabar, Iban; Krutokhvostov, Roman; Lopatin, Sergei; Hillenbrand, Rainer

2013-03-13

We report the development of infrared-resonant antenna probes for tip-enhanced optical microscopy. We employ focused-ion-beam machining to fabricate high-aspect ratio gold cones, which replace the standard tip of a commercial Si-based atomic force microscopy cantilever. Calculations show large field enhancements at the tip apex due to geometrical antenna resonances in the cones, which can be precisely tuned throughout a broad spectral range from visible to terahertz frequencies by adjusting the cone length. Spectroscopic analysis of these probes by electron energy loss spectroscopy, Fourier transform infrared spectroscopy, and Fourier transform infrared near-field spectroscopy corroborates their functionality as resonant antennas and verifies the broad tunability. By employing the novel probes in a scattering-type near-field microscope and imaging a single tobacco mosaic virus (TMV), we experimentally demonstrate high-performance mid-infrared nanoimaging of molecular absorption. Our probes offer excellent perspectives for optical nanoimaging and nanospectroscopy, pushing the detection and resolution limits in many applications, including nanoscale infrared mapping of organic, molecular, and biological materials, nanocomposites, or nanodevices.

Scanning probe acceleration microscopy (SPAM) in fluids: Mapping mechanical properties of surfaces at the nanoscale

NASA Astrophysics Data System (ADS)

Legleiter, Justin; Park, Matthew; Cusick, Brian; Kowalewski, Tomasz

2006-03-01

One of the major thrusts in proximal probe techniques is combination of imaging capabilities with simultaneous measurements of physical properties. In tapping mode atomic force microscopy (TMAFM), the most straightforward way to accomplish this goal is to reconstruct the time-resolved force interaction between the tip and surface. These tip-sample forces can be used to detect interactions (e.g., binding sites) and map material properties with nanoscale spatial resolution. Here, we describe a previously unreported approach, which we refer to as scanning probe acceleration microscopy (SPAM), in which the TMAFM cantilever acts as an accelerometer to extract tip-sample forces during imaging. This method utilizes the second derivative of the deflection signal to recover the tip acceleration trajectory. The challenge in such an approach is that with real, noisy data, the second derivative of the signal is strongly dominated by the noise. This problem is solved by taking advantage of the fact that most of the information about the deflection trajectory is contained in the higher harmonics, making it possible to filter the signal by “comb” filtering, i.e., by taking its Fourier transform and inverting it while selectively retaining only the intensities at integer harmonic frequencies. Such a comb filtering method works particularly well in fluid TMAFM because of the highly distorted character of the deflection signal. Numerical simulations and in situ TMAFM experiments on supported lipid bilayer patches on mica are reported to demonstrate the validity of this approach.

EFM data mapped into 2D images of tip-sample contact potential difference and capacitance second derivative.

PubMed

Lilliu, S; Maragliano, C; Hampton, M; Elliott, M; Stefancich, M; Chiesa, M; Dahlem, M S; Macdonald, J E

2013-11-27

We report a simple technique for mapping Electrostatic Force Microscopy (EFM) bias sweep data into 2D images. The method allows simultaneous probing, in the same scanning area, of the contact potential difference and the second derivative of the capacitance between tip and sample, along with the height information. The only required equipment consists of a microscope with lift-mode EFM capable of phase shift detection. We designate this approach as Scanning Probe Potential Electrostatic Force Microscopy (SPP-EFM). An open-source MATLAB Graphical User Interface (GUI) for images acquisition, processing and analysis has been developed. The technique is tested with Indium Tin Oxide (ITO) and with poly(3-hexylthiophene) (P3HT) nanowires for organic transistor applications.

Research Update: Nanoscale surface potential analysis of MoS2 field-effect transistors for biomolecular detection using Kelvin probe force microscopy

NASA Astrophysics Data System (ADS)

Kim, Min Hyung; Park, Heekyeong; Lee, Hyungbeen; Nam, Kihwan; Jeong, Seokhwan; Omkaram, Inturu; Yoon, Dae Sung; Lee, Sei Young; Kim, Sunkook; Lee, Sang Woo

2016-10-01

We used high-resolution Kelvin probe force microscopy (KPFM) to investigate the immobilization of a prostate specific antigen (PSA) antibody by measuring the surface potential (SP) on a MoS2 surface over an extensive concentration range (1 pg/ml-100 μg/ml). After PSA antibody immobilization, we demonstrated that the SP on the MoS2 surface characterized by KPFM strongly correlated to the electrical signal of a MoS2 bioFET. This demonstration can not only be used to optimize the immobilization conditions for captured molecules, but can also be applied as a diagnostic tool to complement the electrical detection of a MoS2 FET biosensor.

An Undergraduate Nanotechnology Engineering Laboratory Course on Atomic Force Microscopy

ERIC Educational Resources Information Center

Russo, D.; Fagan, R. D.; Hesjedal, T.

2011-01-01

The University of Waterloo, Waterloo, ON, Canada, is home to North America's first undergraduate program in nanotechnology. As part of the Nanotechnology Engineering degree program, a scanning probe microscopy (SPM)-based laboratory has been developed for students in their fourth year. The one-term laboratory course "Nanoprobing and…

Local probe microscopic studies on Al-doped ZnO: Pseudoferroelectricity and band bending at grain boundaries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Mohit; Basu, Tanmoy; Som, Tapobrata, E-mail: tsom@iopb.res.in

2016-01-07

In this paper, based on piezoforce measurements, we show the presence of opposite polarization at grains and grain boundaries of Al-doped ZnO (AZO). The polarization can be flipped by 180° in phase by switching the polarity of the applied electric field, revealing the existence of nanoscale pseudoferroelectricity in AZO grown on Pt/TiO{sub 2}/SiO{sub 2}/Si substrate. We also demonstrate an experimental evidence on local band bending at grain boundaries of AZO films using conductive atomic force microscopy and Kelvin probe force microscopy. The presence of an opposite polarization at grains and grain boundaries gives rise to a polarization-driven barrier formation atmore » grain boundaries. With the help of conductive atomic force microscopy, we show that the polarization-driven barrier along with the defect-induced electrostatic potential barrier account for the measured local band bending at grain boundaries. The present study opens a new avenue to understand the charge transport in light of both polarization and electrostatic effects.« less

Self-assembled monolayers of alkyl-thiols on InAs: A Kelvin probe force microscopy study

NASA Astrophysics Data System (ADS)

Szwajca, A.; Wei, J.; Schukfeh, M. I.; Tornow, M.

2015-03-01

We report on the preparation and characterization of self-assembled monolayers from aliphatic thiols with different chain length and termination on InAs (100) planar surfaces. This included as first step the development and investigation of a thorough chemical InAs surface preparation step using a dedicated bromine/NH4OH-based etching process. Ellipsometry, contact angle measurements and atomic force microscopy (AFM) indicated the formation of smooth, surface conforming monolayers. The molecular tilt angles were obtained as 30 ± 10° with respect to the surface normal. Kelvin probe force microscopy (KPFM) measurements in hand with Parameterized Model number 5 (PM5) calculations of the involved molecular dipoles allowed for an estimation of the molecular packing densities on the surface. We obtained values of up to n = 1014 cm- 2 for the SAMs under study. These are close to what is predicted from a simple geometrical model that would calculate a maximum density of about n = 2.7 × 1014 cm- 2. We take this as additional conformation of the substrate smoothness and quality of our InAs-SAM hybrid layer systems.

Surface potential extraction from electrostatic and Kelvin-probe force microscopy images

NASA Astrophysics Data System (ADS)

Xu, Jie; Chen, Deyuan; Li, Wei; Xu, Jun

2018-05-01

A comprehensive comparison study of electrostatic force microscopy (EFM) and Kelvin probe force microscopy (KPFM) is conducted in this manuscript. First, it is theoretically demonstrated that for metallic or semiconductor samples, both the EFM and KPFM signals are a convolution of the sample surface potential with their respective transfer functions. Then, an equivalent point-mass model describing cantilever deflection under distributed loads is developed to reevaluate the cantilever influence on detection signals, and it is shown that the cantilever has no influence on the EFM signal, while it will affect the KPFM signal intensity but not change the resolution. Finally, EFM and KPFM experiments are carried out, and the surface potential is extracted from the EFM and KPFM images by deconvolution processing, respectively. The extracted potential intensity is well consistent with each other and the detection resolution also complies with the theoretical analysis. Our work is helpful to perform a quantitative analysis of EFM and KPFM signals, and the developed point-mass model can also be used for other cantilever beam deflection problems.

Band Excitation Kelvin probe force microscopy utilizing photothermal excitation

DOE PAGES

Collins, Liam; Jesse, Stephen; Balke, Nina; ...

2015-03-13

A multifrequency open loop Kelvin probe force microscopy (KPFM) approach utilizing photothermal as opposed to electrical excitation is developed. Photothermal band excitation (PthBE)-KPFM is implemented here in a grid mode on a model test sample comprising a metal-insulator junction with local charge-patterned regions. Unlike the previously described open loop BE-KPFM, which relies on capacitive actuation of the cantilever, photothermal actuation is shown to be highly sensitive to the electrostatic force gradient even at biases close to the contact potential difference (CPD). PthBE-KPFM is further shown to provide a more localized measurement of true CPD in comparison to the gold standardmore » ambient KPFM approach, amplitude modulated KPFM. In conclusion, PthBE-KPFM data contain information relating to local dielectric properties and electronic dissipation between tip and sample unattainable using conventional single frequency KPFM approaches.« less

Recent advances in micromechanical characterization of polymer, biomaterial, and cell surfaces with atomic force microscopy

NASA Astrophysics Data System (ADS)

Chyasnavichyus, Marius; Young, Seth L.; Tsukruk, Vladimir V.

2015-08-01

Probing of micro- and nanoscale mechanical properties of soft materials with atomic force microscopy (AFM) gives essential information about the performance of the nanostructured polymer systems, natural nanocomposites, ultrathin coatings, and cell functioning. AFM provides efficient and is some cases the exclusive way to study these properties nondestructively in controlled environment. Precise force control in AFM methods allows its application to variety of soft materials and can be used to go beyond elastic properties and examine temperature and rate dependent materials response. In this review, we discuss experimental AFM methods currently used in the field of soft nanostructured composites and biomaterials. We discuss advantages and disadvantages of common AFM probing techniques, which allow for both qualitative and quantitative mappings of the elastic modulus of soft materials with nanosacle resolution. We also discuss several advanced techniques for more elaborate measurements of viscoelastic properties of soft materials and experiments on single cells.

EDITORIAL: Scanning probe microscopy: a visionary development Scanning probe microscopy: a visionary development

NASA Astrophysics Data System (ADS)

Demming, Anna

2013-07-01

The development of scanning probe microscopy repositioned modern physics. When Rohrer and Binnig first used electronic tunnelling effects to image atoms and quantum states they did more than pin down theoretical hypotheses to real-world observables; the scanning tunnelling microscope fed imaginations, prompting researchers to consider new directions and possibilities [1]. As Rohrer once commented, 'We could show that you can easily manipulate or position something small in space with an accuracy of 10 pm.... When you can do that, you simply have ideas of what you can do' [2]. The development heralded a cavalry of scanning probe techniques—such as atomic force microscopy (AFM) [3-5], scanning near-field optical microscopy (SNOM) [6-8] and Kelvin probe force microscopy (KPFM) [9, 10]—that still continue to bring nanomaterials and nanoscale phenomena into fresh focus. Not long after the development of scanning tunnelling microscopy, Binnig, Quate and Gerber collaborating in California in the US published work on a new type of microscope also capable of atomic level resolution [3]. The original concept behind scanning tunnelling microscopy uses electrical conductance, which places substantial limitations on the systems that it can image. Binnig, Quate and Gerber developed the AFM to 'feel' the topology of surfaces like the needle of an old fashioned vinyl player. In this way insulators could be imaged as well. The development of a force modulation mode AFM extended the tool's reach to soft materials making images of biological samples accessible with the technique [4]. There have now been a number of demonstrations of image capture at rates that allow dynamics at the nanoscale to be tracked in real time, opening further possibilities in applications of the AFM as described in a recent review by Toshio Ando at Kanazawa University [5]. Researchers also found a way to retrieve optical information at 'super-resolution' [6, 7]. Optical microscopy provides spectral details that harbour a wealth of additional information about the sample and its environment, like switching from black and white to technicolour. With the invention of SNOM these details were no longer restricted by the diffraction limit to a resolution of half the wavelength of the incident light. The principle behind SNOM remains very similar to STM but instead of measuring an electronic current, information is captured from the non-propagating optical near field, where the diffraction limit does not apply. SNOM continues to be an invaluable imaging technique as demonstrated recently by researchers in Spain and Korea, who used it to measure near-infrared-to-visible upconversion and cathodoluminescence emission properties of Ln3+ in nanocrystalline Ln-doped Lu2O3 materials with 1D morphology [8]. Their work holds promise for controlled incorporation of such optically active nanostructures in future photonic structures and applications. The cantilever-probe system provides a number of highly sensitive interactions that can be exploited to extract details of a sample system. The potential offset between the probe and surface manifests itself in a force and this too has been used in KPFM [9]. The finite tip size has a profound effect on the measured image in scanning probe-microscopes in general. In KPFM, as Rosenwaks and colleagues in Israel, US and Germany point out in this issue [10] the influence of the tip and cantilever on measurements is particularly significant because of the long range nature of the electrostatic forces involved. Measurements at any one point provide a weighted average of the contact potential difference of the sample and to obtain a quantitative image this averaging must be taken into account. Rosenwaks and colleagues tackle this challenge in the work reported in this issue, presenting an algorithm for reconstructing a sample surface potential from its KPFM image. Their study also reveals that the averaging effects are far more significant for amplitude modulated KPFM measurements compared with the frequency modulated mode. Rohrer and Binnig shared the Nobel Prize for Physics 'for their design of the scanning tunnelling microscope' [11]. They are widely recognized among the founding fathers of nanoscience. In an interview in 2005 Rohrer once commented on the benefits of changing fields even if it leaves you feeling a little 'lost and lonely' at first. In fact he attributed his ability to contribute his Nobel Prize winning work to science at a comparatively senior age to the fact that he had changed fields. 'You cannot be the star from the beginning, but I think what is important is that you might bring in a different way of thinking. You have a certain lightness to approach something that is the expert opinion' [2]. In nanotechnology where such a formidable range of disciplines seem to feed into the research such words may be particularly encouraging. Rohrer passed away on 16 May 2013, but the awesome legacy of his life's work continues. With the scanning tunnelling microscope the lofty eccentricities of quantum mechanical theory literally came into view, quite an inspiration. References [1] Binning G, Rohrer H, Gerber Ch and Weibel E 1982 Surface studies by scanning tunneling microscopy Phys. Rev. Lett. 49 57-61 [2] Weiss P S 2007 A conversation with Dr. Heinrich Rohrer: STM Co-inventor and one of the founding fathers of nanoscience ACS Nano 1 3-5 [3] Binnig G, Quate C F and Gerber Ch 1986 Atomic force microscope Phys. Rev. Lett. 56 930-3 [4] Maivald P, Butt H J, Gould S A C, Prater C B, Drake B, Gurley J A, Elings V B and Hansma P K 1991 Using force modulation to image surface elasticities with the atomic force microscope Nanotechnology 2 103-6 [5] Ando T 2012 High-speed atomic force microscopy coming of age Nanotechnology 23 062001 [6] Betzig E, Isaacson M, Barshatzky H, Lewis A and Lin K 1988 Super-resolution imaging with near-field scanning optical microscopy (NSOM) Ultramicroscopy 25 155-63 [7] Thio T, Lezec H J, Ebbesen T W, Pellerin K M, Lewen G D, Nahata A and Linke R A 2002 Giant optical transmission of sub-wavelength apertures: physics and applications Nanotechnology 13 429-32 [8] Barrera E W, Pujol M C, Díaz F, Choi S B, Rotermund F, Park K H, Jeong M S and Cascales C 2011 Emission properties of hydrothermal Yb3+, Er3+ and Yb3+, Tm3+-codoped Lu2O3 nanorods: upconversion, cathodoluminescence and assessment of waveguide behaviour Nanotechnology 22 075205 [9] Nonnenmacher M, O'Boyle M P and Wickramasinghe H K 1991 Kelvin probe force microscopy Appl. Phys. Lett. 58 2921-3 [10] Cohen G, Halpern E, Nanayakkara S U, Luther J M, Held C, Bennewitz R, Boag A and Rosenwaks Y 2013 Reconstruction of surface potential from Kelvin probe force microscopy images Nanotechnology 24 295702 [11] 1986 The Nobel Prize in Physics www.nobelprize.org/nobel prizes/physics/laureates/1986/ index.html

A study approach on ferroelectric domains in BaTiO{sub 3}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rocha, L.S.R.; Cavalcanti, C.S.

Atomic Force Acoustic Microscopy (AFAM) and Piezoresponse Force Microscopy (PFM) were used to study local elastic and electromechanical response in BaTiO{sub 3} ceramics. A commercial multi-mode Scanning Probe Microscopy (SPM) and AFAM mode to image contact stiffness were employed to accomplish the aforementioned purposes. Stiffness parameters along with Young's moduli and piezo coefficients were quantitatively determined. PFM studies were based on electrostatic and electromechanical response from localized tip-surface contact. Comparison was made regarding the Young's moduli obtained by AFAM and PFM. In addition, phase and amplitude images were analyzed based on poling behavior, obtained via the application of − 10more » V to + 10 V local voltage. - Highlights: •Nanoscale behavior of piezo domains in BaTiO{sub 3} ferroelectric materials •Use of Atomic Force Acoustic Microscopy (AFAM) and Piezo Force Microscopy (PFM) •Local elastic and electromechanical response in BaTiO{sub 3} ceramics •The young's moduli obtained from AFAM and PFM.« less

Preventing probe induced topography correlated artifacts in Kelvin Probe Force Microscopy.

PubMed

Polak, Leo; Wijngaarden, Rinke J

2016-12-01

Kelvin Probe Force Microscopy (KPFM) on samples with rough surface topography can be hindered by topography correlated artifacts. We show that, with the proper experimental configuration and using homogeneously metal coated probes, we are able to obtain amplitude modulation (AM) KPFM results on a gold coated sample with rough topography that are free from such artifacts. By inducing tip inhomogeneity through contact with the sample, clear potential variations appear in the KPFM image, which correlate with the surface topography and, thus, are probe induced artifacts. We find that switching to frequency modulation (FM) KPFM with such altered probes does not remove these artifacts. We also find that the induced tip inhomogeneity causes a lift height dependence of the KPFM measurement, which can therefore be used as a check for the presence of probe induced topography correlated artifacts. We attribute the observed effects to a work function difference between the tip and the rest of the probe and describe a model for such inhomogeneous probes that predicts lift height dependence and topography correlated artifacts for both AM and FM-KPFM methods. This work demonstrates that using a probe with a homogeneous work function and preventing tip changes is essential for KPFM on non-flat samples. From the three investigated probe coatings, PtIr, Au and TiN, the latter appears to be the most suitable, because of its better resistance against coating damage. Copyright © 2016 Elsevier B.V. All rights reserved.

Characterizing nanoscale scanning probes using electron microscopy: A novel fixture and a practical guide

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jacobs, Tevis D. B., E-mail: tjacobs@pitt.edu; Wabiszewski, Graham E.; Goodman, Alexander J.

2016-01-15

The nanoscale geometry of probe tips used for atomic force microscopy (AFM) measurements determines the lateral resolution, contributes to the strength of the tip-surface interaction, and can be a significant source of uncertainty in the quantitative analysis of results. While inverse imaging of the probe tip has been used successfully to determine probe tip geometry, direct observation of the tip profile using electron microscopy (EM) confers several advantages: it provides direct (rather than indirect) imaging, requires fewer algorithmic parameters, and does not require bringing the tip into contact with a sample. In the past, EM-based observation of the probe tipmore » has been achieved using ad hoc mounting methods that are constrained by low throughput, the risk of contamination, and repeatability issues. We report on a probe fixture designed for use in a commercial transmission electron microscope that enables repeatable mounting of multiple AFM probes as well as a reference grid for beam alignment. This communication describes the design, fabrication, and advantages of this probe fixture, including full technical drawings for machining. Further, best practices are discussed for repeatable, non-destructive probe imaging. Finally, examples of the fixture’s use are described, including characterization of common commercial AFM probes in their out-of-the-box condition.« less

Characterizing nanoscale scanning probes using electron microscopy: A novel fixture and a practical guide

NASA Astrophysics Data System (ADS)

Jacobs, Tevis D. B.; Wabiszewski, Graham E.; Goodman, Alexander J.; Carpick, Robert W.

2016-01-01

The nanoscale geometry of probe tips used for atomic force microscopy (AFM) measurements determines the lateral resolution, contributes to the strength of the tip-surface interaction, and can be a significant source of uncertainty in the quantitative analysis of results. While inverse imaging of the probe tip has been used successfully to determine probe tip geometry, direct observation of the tip profile using electron microscopy (EM) confers several advantages: it provides direct (rather than indirect) imaging, requires fewer algorithmic parameters, and does not require bringing the tip into contact with a sample. In the past, EM-based observation of the probe tip has been achieved using ad hoc mounting methods that are constrained by low throughput, the risk of contamination, and repeatability issues. We report on a probe fixture designed for use in a commercial transmission electron microscope that enables repeatable mounting of multiple AFM probes as well as a reference grid for beam alignment. This communication describes the design, fabrication, and advantages of this probe fixture, including full technical drawings for machining. Further, best practices are discussed for repeatable, non-destructive probe imaging. Finally, examples of the fixture's use are described, including characterization of common commercial AFM probes in their out-of-the-box condition.

High quality-factor quartz tuning fork glass probe used in tapping mode atomic force microscopy for surface profile measurement

NASA Astrophysics Data System (ADS)

Chen, Yuan-Liu; Xu, Yanhao; Shimizu, Yuki; Matsukuma, Hiraku; Gao, Wei

2018-06-01

This paper presents a high quality-factor (Q-factor) quartz tuning fork (QTF) with a glass probe attached, used in frequency modulation tapping mode atomic force microscopy (AFM) for the surface profile metrology of micro and nanostructures. Unlike conventionally used QTFs, which have tungsten or platinum probes for tapping mode AFM, and suffer from a low Q-factor influenced by the relatively large mass of the probe, the glass probe, which has a lower density, increases the Q-factor of the QTF probe unit allowing it to obtain better measurement sensitivity. In addition, the process of attaching the probe to the QTF with epoxy resin, which is necessary for tapping mode AFM, is also optimized to further improve the Q-factor of the QTF glass probe. The Q-factor of the optimized QTF glass probe unit is demonstrated to be very close to that of a bare QTF without a probe attached. To verify the effectiveness and the advantages of the optimized QTF glass probe unit, the probe unit is integrated into a home-built tapping mode AFM for conducting surface profile measurements of micro and nanostructures. A blazed grating with fine tool marks of 100 nm, a microprism sheet with a vertical amplitude of 25 µm and a Fresnel lens with a steep slope of 90 degrees are used as measurement specimens. From the measurement results, it is demonstrated that the optimized QTF glass probe unit can achieve higher sensitivity as well as better stability than conventional probes in the measurement of micro and nanostructures.

Probing fibronectin–antibody interactions using AFM force spectroscopy and lateral force microscopy

PubMed Central

Kulik, Andrzej J; Lee, Kyumin; Pyka-Fościak, Grazyna; Nowak, Wieslaw

2015-01-01

Summary The first experiment showing the effects of specific interaction forces using lateral force microscopy (LFM) was demonstrated for lectin–carbohydrate interactions some years ago. Such measurements are possible under the assumption that specific forces strongly dominate over the non-specific ones. However, obtaining quantitative results requires the complex and tedious calibration of a torsional force. Here, a new and relatively simple method for the calibration of the torsional force is presented. The proposed calibration method is validated through the measurement of the interaction forces between human fibronectin and its monoclonal antibody. The results obtained using LFM and AFM-based classical force spectroscopies showed similar unbinding forces recorded at similar loading rates. Our studies verify that the proposed lateral force calibration method can be applied to study single molecule interactions. PMID:26114080

Low-Temperature Reduction of Graphene Oxide: Electrical Conductance and Scanning Kelvin Probe Force Microscopy

NASA Astrophysics Data System (ADS)

Slobodian, Oleksandr M.; Lytvyn, Peter M.; Nikolenko, Andrii S.; Naseka, Victor M.; Khyzhun, Oleg Yu.; Vasin, Andrey V.; Sevostianov, Stanislav V.; Nazarov, Alexei N.

2018-05-01

Graphene oxide (GO) films were formed by drop-casting method and were studied by FTIR spectroscopy, micro-Raman spectroscopy (mRS), X-ray photoelectron spectroscopy (XPS), four-points probe method, atomic force microscopy (AFM), and scanning Kelvin probe force (SKPFM) microscopy after low-temperature annealing at ambient conditions. It was shown that in temperature range from 50 to 250 °C the electrical resistivity of the GO films decreases by seven orders of magnitude and is governed by two processes with activation energies of 6.22 and 1.65 eV, respectively. It was shown that the first process is mainly associated with water and OH groups desorption reducing the thickness of the film by 35% and causing the resistivity decrease by five orders of magnitude. The corresponding activation energy is the effective value determined by desorption and electrical connection of GO flakes from different layers. The second process is mainly associated with desorption of oxygen epoxy and alkoxy groups connected with carbon located in the basal plane of GO. AFM and SKPFM methods showed that during the second process, first, the surface of GO plane is destroyed forming nanostructured surface with low work function and then at higher temperature a flat carbon plane is formed that results in an increase of the work function of reduced GO.

Carbon Nanotube Tip Probes: Stability and Lateral Resolution in Scanning Probe Microscopy and Application to Surface Science to Semiconductors

NASA Technical Reports Server (NTRS)

Nguyen, Cattien V.; Chao, Kuo-Jen; Stevens, Ramsey M. D.; Delzeit, Lance; Cassell, Alan; Han, Jie; Meyyappan, M.; Arnold, James (Technical Monitor)

2001-01-01

In this paper we present results on the stability and lateral resolution capability of carbon nanotube (CNT) scanning probes as applied to atomic force microscopy (AFM). Surface topography images of ultra-thin films (2-5 nm thickness) obtained with AFM are used to illustrate the lateral resolution capability of single-walled carbon nanotube probes. Images of metal films prepared by ion beam sputtering exhibit grain sizes ranging from greater than 10 nm to as small as approximately 2 nm for gold and iridium respectively. In addition, imaging stability and lifetime of multi-walled carbon nanotube scanning probes are studied on a relatively hard surface of silicon nitride (Si3N4). AFM images Of Si3N4 surface collected after more than 15 hrs of continuous scanning show no detectable degradation in lateral resolution. These results indicate the general feasibility of CNT tips and scanning probe microscopy for examining nanometer-scale surface features of deposited metals as well as non-conductive thin films. AFM coupled with CNT tips offers a simple and nondestructive technique for probing a variety of surfaces, and has immense potential as a surface characterization tool in integrated circuit manufacturing.

Identifying passivated dynamic force microscopy tips on H:Si(100)

NASA Astrophysics Data System (ADS)

Sharp, Peter; Jarvis, Sam; Woolley, Richard; Sweetman, Adam; Kantorovich, Lev; Pakes, Chris; Moriarty, Philip

2012-06-01

The chemical reactivity of the tip plays a central role in image formation in dynamic force microscopy, but in very many cases the state of the probe is a key experimental unknown. We show here that an H-terminated and thus chemically unreactive tip can be readily identified via characteristic imaging and spectroscopic (F(z)) signatures, including, in particular, contrast inversion, on hydrogen-passivated Si(100). We determine the tip apex termination by comparing site-specific difference force curves with the results of density functional theory, providing a clear protocol for the identification of chemically unreactive tips on silicon surfaces.

Distinguishing ferritin from apoferritin using magnetic force microscopy

NASA Astrophysics Data System (ADS)

Nocera, Tanya M.; Zeng, Yuzhi; Agarwal, Gunjan

2014-11-01

Estimating the amount of iron-replete ferritin versus iron-deficient apoferritin proteins is important in biomedical and nanotechnology applications. This work introduces a simple and novel approach to quantify ferritin by using magnetic force microscopy (MFM). We demonstrate how high magnetic moment probes enhance the magnitude of MFM signal, thus enabling accurate quantitative estimation of ferritin content in ferritin/apoferritin mixtures in vitro. We envisage MFM could be adapted to accurately determine ferritin content in protein mixtures or in small aliquots of clinical samples.

Magnetic force microscopy/current contrast imaging: A new technique for internal current probing of ICs

DOE Office of Scientific and Technical Information (OSTI.GOV)

Campbell, A.N.; Cole, E.I. Jr.; Dodd, B.A.

This invited paper describes recently reported work on the application of magnetic force microscopy (MFM) to image currents in IC conductors [1]. A computer model for MFM imaging of IC currents and experimental results demonstrating the ability to determine current direction and magnitude with a resolution of {approximately} 1 mA dc and {approximately} 1 {mu}A ac are presented. The physics of MFM signal generation and applications to current imaging and measurement are described.

Magnetic elements for switching magnetization magnetic force microscopy tips.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cambel, V.; Elias, P.; Gregusova, D.

2010-09-01

Using combination of micromagnetic calculations and magnetic force microscopy (MFM) imaging we find optimal parameters for novel magnetic tips suitable for switching magnetization MFM. Switching magnetization MFM is based on two-pass scanning atomic force microscopy with reversed tip magnetization between the scans. Within the technique the sum of the scanned data with reversed tip magnetization depicts local atomic forces, while their difference maps the local magnetic forces. Here we propose the design and calculate the magnetic properties of tips suitable for this scanning probe technique. We find that for best performance the spin-polarized tips must exhibit low magnetic moment, lowmore » switching fields, and single-domain state at remanence. The switching field of such tips is calculated and optimum shape of the Permalloy elements for the tips is found. We show excellent correspondence between calculated and experimental results for Py elements.« less

Intermolecular artifacts in probe microscope images of C60 assemblies

NASA Astrophysics Data System (ADS)

Jarvis, Samuel Paul; Rashid, Mohammad Abdur; Sweetman, Adam; Leaf, Jeremy; Taylor, Simon; Moriarty, Philip; Dunn, Janette

2015-12-01

Claims that dynamic force microscopy has the capability to resolve intermolecular bonds in real space continue to be vigorously debated. To date, studies have been restricted to planar molecular assemblies with small separations between neighboring molecules. Here we report the observation of intermolecular artifacts over much larger distances in 2D assemblies of C60 molecules, with compelling evidence that in our case the tip apex is terminated by a C60 molecule (rather than the CO termination typically exploited in ultrahigh resolution force microscopy). The complete absence of directional interactions such as hydrogen or halogen bonding, the nonplanar structure of C60, and the fullerene termination of the tip apex in our case highlight that intermolecular artifacts are ubiquitous in dynamic force microscopy.

Mechanically adjustable single-molecule transistors and stencil mask nanofabrication of high-resolution scanning probes

NASA Astrophysics Data System (ADS)

Champagne, Alexandre

This dissertation presents the development of two original experimental techniques to probe nanoscale objects. The first one studies electronic transport in single organic molecule transistors in which the source-drain electrode spacing is mechanically adjustable. The second involves the fabrication of high-resolution scanning probe microscopy sensors using a stencil mask lithography technique. We describe the fabrication of transistors in which a single organic molecule can be incorporated. The source and drain leads of these transistors are freely suspended above a flexible substrate, and their spacing can be adjusted by bending the substrate. We detail the technology developed to carry out measurements on these samples. We study electronic transport in single C60 molecules at low temperature. We observe Coulomb blockaded transport and can resolve the discrete energy spectrum of the molecule. We are able to mechanically tune the spacing between the electrodes (over a range of 5 A) to modulate the lead-molecule coupling, and can electrostatically tune the energy levels on the molecule by up to 160 meV using a gate electrode. Initial progress in studying different transport regimes in other molecules is also discussed. We present a lithographic process that allows the deposition of metal nanostructures with a resolution down to 10 nm directly onto atomic force microscope (AFM) tips. We show that multiple layers of lithography can be deposited and aligned. We fabricate high-resolution magnetic force microscopy (MFM) probes using this method and discuss progress to fabricate other scanning probe microscopy (SPM) sensors.

Low-temperature post-deposition annealing investigation for 3D charge trap flash memory by Kelvin probe force microscopy

NASA Astrophysics Data System (ADS)

Huo, Zongliang; Jin, Lei; Han, Yulong; Li, Xinkai; Ye, Tianchun; Liu, Ming

2015-01-01

The influence of post-deposition annealing (PDA) temperature condition on charge distribution behavior of HfO2 thin films was systematically investigated by various-temperature Kelvin probe force microscopy technology. Contact potential difference profiles demonstrated that charge storage capability shrinks with decreasing annealing temperature from 1,000 to 500 °C and lower. Compared to 1,000 °C PDA, it was found that 500 °C PDA causes deeper effective trap energy level, suppresses lateral charge spreading, and improves the retention characteristics. It is concluded that low-temperature PDA can be adopted in 3D HfO2-based charge trap flash memory to improve the thermal treatment compatibility of the bottom peripheral logic and upper memory arrays.

Anomalous surface potential behavior observed in InN by photoassisted Kelvin probe force microscopy

NASA Astrophysics Data System (ADS)

Sun, Xiaoxiao; Wei, Jiandong; Wang, Xinqiang; Wang, Ping; Li, Shunfeng; Waag, Andreas; Li, Mo; Zhang, Jian; Ge, Weikun; Shen, Bo

2017-05-01

Lattice-polarity dependence of InN surface photovoltage has been identified by an anomalous surface potential behavior observed via photoassisted Kelvin probe force microscopy. Upon above bandgap light illumination in the ambient atmosphere, the surface photovoltage of the In-polar InN shows a pronounced decrease, while that of the N-polar one keeps almost constant. Those different behaviors between N-polar and In-polar surfaces are attributed to a polarity-related surface reactivity, which is found not to be influenced by Mg-doping. These findings provide a simple and non-destructive approach to determine the lattice polarity and allow us to suggest that the In-polar InN, especially that with buried p-type conduction, should be chosen for sensing application.

Band Excitation for Scanning Probe Microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jesse, Stephen

2017-01-02

The Band Excitation (BE) technique for scanning probe microscopy uses a precisely determined waveform that contains specific frequencies to excite the cantilever or sample in an atomic force microscope to extract more information, and more reliable information from a sample. There are a myriad of details and complexities associated with implementing the BE technique. There is therefore a need to have a user friendly interface that allows typical microscopists access to this methodology. This software enables users of atomic force microscopes to easily: build complex band-excitation waveforms, set-up the microscope scanning conditions, configure the input and output electronics for generatemore » the waveform as a voltage signal and capture the response of the system, perform analysis on the captured response, and display the results of the measurement.« less

Evaluating signal and noise spectral density of a qPlus sensor with an active feedback control

NASA Astrophysics Data System (ADS)

Lee, Manhee; An, Sangmin; Jhe, Wonho

2018-05-01

Q-control technique enables to actively change the quality factor of the probe oscillation in dynamic atomic force microscopy. The Q-control is realized by adding a self-feedback loop into the original actuation-detection system, in which a damping force with controllable damping coefficient in magnitude and sign is applied to the oscillating probe. While the applied force alters the total damping interaction and thus the overall `signal' of the probe motion, the added feedback system changes the `noise' of the motion as well. Here, we systematically investigate the signal, the noise, and the signal-to-noise ratio of the qPlus sensor under the active Q-control. We quantify the noise of the qPlus motion by measuring the noise spectral density, which is reproduced by a harmonic oscillator model including the thermal and the measurement noises. We show that the noise signal increases with the quality factor controlled, scaling as the square root of the quality factor. Because the overall signal is linearly proportional to the quality factor, the signal-to-noise ratio scales as the square root of the quality factor. The Q-controlled qPlus with a highly enhanced Q, up to 10,000 in air, leads to the minimum detectable force gradient of 0.001 N/m, which would enhance the capability of the qPlus sensor for atomic force microscopy and spectroscopy.

Indentation of Graphene-Covered Atomic Force Microscopy Probe Across a Lipid Bilayer Membrane: Effect of Tip Shape, Size, and Surface Hydrophobicity.

PubMed

Lv, Kang; Li, Yinfeng

2018-06-21

Understanding the interaction of graphene with cell membranes is crucial to the development of graphene-based biological applications and the management of graphene safety issues. To help reveal the key factors controlling the interaction between graphene and cell membranes, here we adopt the dissipative particle dynamics method to analyze the evolution of interaction force and free energy as the graphene-covered atomic force microscopy (AFM) probe indents across a lipid bilayer. The simulation results show that the graphene-covered AFM probe can cause severe deformation of the cell membrane which drives the lipid molecule to adsorb and diffuse at the surface of graphene. The breakthrough force and free energy are calculated to study the effects of the tip shape, size, and surface hydrophobicity on the piercing behaviors of graphene-covered AFM. In addition, the deformation of cell membrane can decrease the dependency of the breakthrough force on the tip shape. The analysis of surface functionalization suggests that the horizontal patterns on graphene can change the preferred orientation in the penetration process, but the vertical patterns on graphene may disrupt the cell membrane. What's more, the bending stiffness of graphene has little influence on the penetration process as graphene pierces into the cell membrane. These results provide useful guidelines for the molecular design of graphene materials with controllable cell penetrability.

Recent advancements in nanoelectrodes and nanopipettes used in combined scanning electrochemical microscopy techniques.

PubMed

Kranz, Christine

2014-01-21

In recent years, major developments in scanning electrochemical microscopy (SECM) have significantly broadened the application range of this electroanalytical technique from high-resolution electrochemical imaging via nanoscale probes to large scale mapping using arrays of microelectrodes. A major driving force in advancing the SECM methodology is based on developing more sophisticated probes beyond conventional micro-disc electrodes usually based on noble metals or carbon microwires. This critical review focuses on the design and development of advanced electrochemical probes particularly enabling combinations of SECM with other analytical measurement techniques to provide information beyond exclusively measuring electrochemical sample properties. Consequently, this critical review will focus on recent progress and new developments towards multifunctional imaging.

Method for imaging liquid and dielectric materials with scanning polarization force microscopy

DOEpatents

Hu, Jun; Ogletree, D. Frank; Salmeron, Miguel; Xiao, Xudong

1999-01-01

The invention images dielectric polarization forces on surfaces induced by a charged scanning force microscope (SFM) probe tip. On insulators, the major contribution to the surface polarizability at low frequencies is from surface ions. The mobility of these ions depends strongly on the humidity. Using the inventive SFM, liquid films, droplets, and other weakly adsorbed materials have been imaged.

Apparatus for imaging liquid and dielectric materials with scanning polarization force microscopy

DOEpatents

Hu, Jun; Ogletree, D. Frank; Salmeron, Miguel; Xiao, Xudong

1998-01-01

The invention images dielectric polarization forces on surfaces induced by a charged scanning force microscope (SFM) probe tip. On insulators, the major contribution to the surface polarizability at low frequencies is from surface ions. The mobility of these ions depends strongly on the humidity. Using the inventive SFM, liquid films, droplets, and other weakly adsorbed materials have been imaged.

Multifrequency scanning probe microscopy study of nanodiamond agglomerates

NASA Astrophysics Data System (ADS)

Aravind, Vasudeva; Lippold, Stephen; Li, Qian; Strelcov, Evgheny; Okatan, Baris; Legum, Benjamin; Kalinin, Sergei; Clarion University Team; Oak Ridge National Laboratory Team

Due to their rich surface chemistry and excellent mechanical properties and non-toxic nature, nanodiamond particles have found applications such as biomedicine, tribology and lubrication, targeted drug delivery systems, tissue scaffolds and surgical implants. Although single nanodiamond particles have diameters about 4-5nm, they tend to form agglomerates. While these agglomerates can be useful for some purposes, many applications of nanodiamonds require single particle, disaggregated nanodiamonds. This work is oriented towards studying forces and interactions that contribute to agglomeration in nanodiamonds. In this work, using multifrequency scanning probe microscopy techniques, we show that agglomerate sizes can vary between 50-100nm in raw nanodiamonds. Extremeties of particles and Interfaces between agglomerates show dissipative forces with scanning probe microscope tip, indicating agglomerates could act as points of increased adhesion, thus reducing lubricating efficiency when nanodiamonds are used as lubricant additives. This research was conducted at the Center for Nanophase Materials Sciences, which is a DOE Office of Science User Facility.

Determination of electrostatic force and its characteristics based on phase difference by amplitude modulation atomic force microscopy

NASA Astrophysics Data System (ADS)

Wang, Kesheng; Cheng, Jia; Yao, Shiji; Lu, Yijia; Ji, Linhong; Xu, Dengfeng

2016-12-01

Electrostatic force measurement at the micro/nano scale is of great significance in science and engineering. In this paper, a reasonable way of applying voltage is put forward by taking an electrostatic chuck in a real integrated circuit manufacturing process as a sample, applying voltage in the probe and the sample electrode, respectively, and comparing the measurement effect of the probe oscillation phase difference by amplitude modulation atomic force microscopy. Based on the phase difference obtained from the experiment, the quantitative dependence of the absolute magnitude of the electrostatic force on the tip-sample distance and applied voltage is established by means of theoretical analysis and numerical simulation. The results show that the varying characteristics of the electrostatic force with the distance and voltage at the micro/nano scale are similar to those at the macroscopic scale. Electrostatic force gradually decays with increasing distance. Electrostatic force is basically proportional to the square of applied voltage. Meanwhile, the applicable conditions of the above laws are discussed. In addition, a comparison of the results in this paper with the results of the energy dissipation method shows the two are consistent in general. The error decreases with increasing distance, and the effect of voltage on the error is small.

Facile Preparation of a Platinum Silicide Nanoparticle-Modified Tip Apex for Scanning Kelvin Probe Microscopy.

PubMed

Lin, Chun-Ting; Chen, Yu-Wei; Su, James; Wu, Chien-Ting; Hsiao, Chien-Nan; Shiao, Ming-Hua; Chang, Mao-Nan

2015-12-01

In this study, we propose an ultra-facile approach to prepare a platinum silicide nanoparticle-modified tip apex (PSM tip) used for scanning Kelvin probe microscopy (SKPM). We combined a localized fluoride-assisted galvanic replacement reaction (LFAGRR) and atmospheric microwave annealing (AMA) to deposit a single platinum silicide nanoparticle with a diameter of 32 nm on the apex of a bare silicon tip of atomic force microscopy (AFM). The total process was completed in an ambient environment in less than 3 min. The improved potential resolution in the SKPM measurement was verified. Moreover, the resolution of the topography is comparable to that of a bare silicon tip. In addition, the negative charges found on the PSM tips suggest the possibility of exploring the use of current PSM tips to sense electric fields more precisely. The ultra-fast and cost-effective preparation of the PSM tips provides a new direction for the preparation of functional tips for scanning probe microscopy.

Dynamic characterization of AFM probes by laser Doppler vibrometry and stroboscopic holographic methodologies

NASA Astrophysics Data System (ADS)

Kuppers, J. D.; Gouverneur, I. M.; Rodgers, M. T.; Wenger, J.; Furlong, C.

2006-08-01

In atomic probe microscopy, micro-probes of various sizes, geometries, and materials are used to define the interface between the samples under investigation and the measuring detectors and instrumentation. Therefore, measuring resolution in atomic probe microscopy is highly dependent on the transfer function characterizing the micro-probes used. In this paper, characterization of the dynamic transfer function of specific micro-cantilever probes used in an Atomic Force Microscope (AFM) operating in the tapping mode is presented. Characterization is based on the combined application of laser Doppler vibrometry (LDV) and real-time stroboscopic optoelectronic holographic microscopy (OEHM) methodologies. LDV is used for the rapid measurement of the frequency response of the probes due to an excitation function containing multiple frequency components. Data obtained from the measured frequency response is used to identify the principal harmonics. In order to identify mode shapes corresponding to the harmonics, full-field of view OEHM is applied. This is accomplished by measurements of motion at various points on the excitation curve surrounding the identified harmonics. It is shown that the combined application of LDV and OEHM enables the high-resolution characterization of mode shapes of vibration, damping characteristics, as well as transient response of the micro-cantilever probes. Such characterization is necessary in high-resolution AFM measurements.

Growth and adhesion properties of monosodium urate monohydrate (MSU) crystals

NASA Astrophysics Data System (ADS)

Perrin, Clare M.

The presence of monosodium urate monohydrate (MSU) crystals in the synovial fluid has long been associated with the joint disease gout. To elucidate the molecular level growth mechanism and adhesive properties of MSU crystals, atomic force microscopy (AFM), scanning electron microscopy, and dynamic light scattering (DLS) techniques were employed in the characterization of the (010) and (1-10) faces of MSU, as well as physiologically relevant solutions supersaturated with urate. Topographical AFM imaging of both MSU (010) and (1-10) revealed the presence of crystalline layers of urate arranged into v-shaped features of varying height. Growth rates were measured for both monolayers (elementary steps) and multiple layers (macrosteps) on both crystal faces under a wide range of urate supersaturation in physiologically relevant solutions. Step velocities for monolayers and multiple layers displayed a second order polynomial dependence on urate supersaturation on MSU (010) and (1-10), with step velocities on (1-10) generally half of those measured on MSU (010) in corresponding growth conditions. Perpendicular step velocities on MSU (010) were obtained and also showed a second order polynomial dependence of step velocity with respect to urate supersaturation, which implies a 2D-island nucleation growth mechanism for MSU (010). Extensive topographical imaging of MSU (010) showed island adsorption from urate growth solutions under all urate solution concentrations investigated, lending further support for the determined growth mechanism. Island sizes derived from DLS experiments on growth solutions were in agreement with those measured on MSU (010) topographical images. Chemical force microscopy (CFM) was utilized to characterize the adhesive properties of MSU (010) and (1-10). AFM probes functionalized with amino acid derivatives and bio-macromolecules found in the synovial fluid were brought into contact with both crystal faces and adhesion forces were tabulated into histograms for comparison. AFM probes functionalized with -COO-, -CH3, and -OH functionalities displayed similar adhesion force with both crystal surfaces of MSU, while adhesion force on (1-10) was three times greater than (010) for -NH2+ probes. For AFM probes functionalized with bovine serum albumin, adhesion force was three times greater on MSU (1-10) than (010), most likely due to the more ionic nature of (1-10).

GTG banding pattern on human metaphase chromosomes revealed by high resolution atomic-force microscopy.

PubMed

Thalhammer, S; Koehler, U; Stark, R W; Heckl, W M

2001-06-01

Surface topography of human metaphase chromosomes following GTG banding was examined using high resolution atomic force microscopy (AFM). Although using a completely different imaging mechanism, which is based on the mechanical interaction of a probe tip with the chromosome, the observed banding pattern is comparable to results from light microscopy and a karyotype of the AFM imaged metaphase spread can be generated. The AFM imaging process was performed on a normal 2n = 46, XX karyotype and on a 2n = 46, XY, t(2;15)(q23;q15) karyotype as an example of a translocation of chromosomal bands.

Back-focal-plane position detection with extended linear range for photonic force microscopy.

PubMed

Martínez, Ignacio A; Petrov, Dmitri

2012-09-01

In photonic force microscopes, the position detection with high temporal and spatial resolution is usually implemented by a quadrant position detector placed in the back focal plane of a condenser. An objective with high numerical aperture (NA) for the optical trap has also been used to focus a detection beam. In that case the displacement of the probe at a fixed position of the detector produces a unique and linear response only in a restricted region of the probe displacement, usually several hundred nanometers. There are specific experiments where the absolute position of the probe is a relevant measure together with the probe position relative the optical trap focus. In our scheme we introduce the detection beam into the condenser with low NA through a pinhole with tunable size. This combination permits us to create a wide detection spot and to achieve the linear range of several micrometers by the probe position detection without reducing the trapping force.

Spectroscopy and atomic force microscopy of biomass.

PubMed

Tetard, L; Passian, A; Farahi, R H; Kalluri, U C; Davison, B H; Thundat, T

2010-05-01

Scanning probe microscopy has emerged as a powerful approach to a broader understanding of the molecular architecture of cell walls, which may shed light on the challenge of efficient cellulosic ethanol production. We have obtained preliminary images of both Populus and switchgrass samples using atomic force microscopy (AFM). The results show distinctive features that are shared by switchgrass and Populus. These features may be attributable to the lignocellulosic cell wall composition, as the collected images exhibit the characteristic macromolecular globule structures attributable to the lignocellulosic systems. Using both AFM and a single case of mode synthesizing atomic force microscopy (MSAFM) to characterize Populus, we obtained images that clearly show the cell wall structure. The results are of importance in providing a better understanding of the characteristic features of both mature cells as well as developing plant cells. In addition, we present spectroscopic investigation of the same samples.

Method for imaging liquid and dielectric materials with scanning polarization force microscopy

DOEpatents

Hu, J.; Ogletree, D.F.; Salmeron, M.; Xiao, X.

1999-03-09

The invention images dielectric polarization forces on surfaces induced by a charged scanning force microscope (SFM) probe tip. On insulators, the major contribution to the surface polarizability at low frequencies is from surface ions. The mobility of these ions depends strongly on the humidity. Using the inventive SFM, liquid films, droplets, and other weakly adsorbed materials have been imaged. 9 figs.

Apparatus for imaging liquid and dielectric materials with scanning polarization force microscopy

DOEpatents

Hu, J.; Ogletree, D.F.; Salmeron, M.; Xiao, X.

1998-04-28

The invention images dielectric polarization forces on surfaces induced by a charged scanning force microscope (SFM) probe tip. On insulators, the major contribution to the surface polarizability at low frequencies is from surface ions. The mobility of these ions depends strongly on the humidity. Using the inventive SFM, liquid films, droplets, and other weakly adsorbed materials have been imaged. 9 figs.

Direct manipulation of metallic nanosheets by shear force microscopy.

PubMed

Bi, Z; Cai, W; Wang, Y; Shang, G

2018-05-15

Micro/nanomanipulation is a rapidly growing technology and holds promising applications in various fields, including photonic/electronic devices, chemical/biosensors etc. In this work, we present that shear force microscopy (ShFM) can be exploited to manipulate metallic nanosheets besides imaging. The manipulation is realized via controlling the shear force sensor probe position and shear force magnitude based on our homemade ShFM system under an optical microscopy for in situ observation. The main feature of the ShFM system is usage of a piezoelectric bimorph sensor, which has the ability of self-excitation and detection. Moreover, the shear force magnitude as a function of the spring constant of the sensor and setpoint is obtained, which indicates that operation modes can be switched between imaging and manipulation through designing the spring constant before experiment and changing the setpoint during manipulation process, respectively. We believe that this alternative manipulation technique could be used to assemble other nanostructures with different shapes, sizes and compositions for new properties and wider applications. © 2018 The Authors Journal of Microscopy © 2018 Royal Microscopical Society.

Electrochemical force microscopy

DOEpatents

Kalinin, Sergei V.; Jesse, Stephen; Collins, Liam F.; Rodriguez, Brian J.

2017-01-10

A system and method for electrochemical force microscopy are provided. The system and method are based on a multidimensional detection scheme that is sensitive to forces experienced by a biased electrode in a solution. The multidimensional approach allows separation of fast processes, such as double layer charging, and charge relaxation, and slow processes, such as diffusion and faradaic reactions, as well as capturing the bias dependence of the response. The time-resolved and bias measurements can also allow probing both linear (small bias range) and non-linear (large bias range) electrochemical regimes and potentially the de-convolution of charge dynamics and diffusion processes from steric effects and electrochemical reactivity.

Identifying Nanoscale Structure-Function Relationships Using Multimodal Atomic Force Microscopy, Dimensionality Reduction, and Regression Techniques.

PubMed

Kong, Jessica; Giridharagopal, Rajiv; Harrison, Jeffrey S; Ginger, David S

2018-05-31

Correlating nanoscale chemical specificity with operational physics is a long-standing goal of functional scanning probe microscopy (SPM). We employ a data analytic approach combining multiple microscopy modes, using compositional information in infrared vibrational excitation maps acquired via photoinduced force microscopy (PiFM) with electrical information from conductive atomic force microscopy. We study a model polymer blend comprising insulating poly(methyl methacrylate) (PMMA) and semiconducting poly(3-hexylthiophene) (P3HT). We show that PiFM spectra are different from FTIR spectra, but can still be used to identify local composition. We use principal component analysis to extract statistically significant principal components and principal component regression to predict local current and identify local polymer composition. In doing so, we observe evidence of semiconducting P3HT within PMMA aggregates. These methods are generalizable to correlated SPM data and provide a meaningful technique for extracting complex compositional information that are impossible to measure from any one technique.

Sensing Performance Analysis on Quartz Tuning Fork-Probe at the High Order Vibration Mode for Multi-Frequency Scanning Probe Microscopy

PubMed Central

Gao, Fengli; Li, Xide

2018-01-01

Multi-frequency scanning near-field optical microscopy, based on a quartz tuning fork-probe (QTF-p) sensor using the first two orders of in-plane bending symmetrical vibration modes, has recently been developed. This method can simultaneously achieve positional feedback (based on the 1st in-plane mode called the low mode) and detect near-field optically induced forces (based on the 2nd in-plane mode called the high mode). Particularly, the high mode sensing performance of the QTF-p is an important issue for characterizing the tip-sample interactions and achieving higher resolution microscopic imaging but the related researches are insufficient. Here, we investigate the vibration performance of QTF-p at high mode based on the experiment and finite element method. The frequency spectrum characteristics are obtained by our homemade laser Doppler vibrometer system. The effects of the properties of the connecting glue layer and the probe features on the dynamic response of the QTF-p sensor at the high mode are investigated for optimization design. Finally, compared with the low mode, an obvious improvement of quality factor, of almost 50%, is obtained at the high mode. Meanwhile, the QTF-p sensor has a high force sensing sensitivity and a large sensing range at the high mode, indicating a broad application prospect for force sensing. PMID:29364847

Microfabricated Electrical Connector for Atomic Force Microscopy Probes with Integrated Sensor/Actuator

NASA Astrophysics Data System (ADS)

Akiyama, Terunobu; Staufer, Urs; Rooij, Nico F. de

2002-06-01

A microfabricated, electrical connector is proposed for facilitating the mounting of atomic force microscopy (AFM) probes, which have an integrated sensor and/or actuator. Only a base chip, which acts as a socket, is permanently fixed onto a printed circuit board and electronically connected by standard wire bonding. The AFM chip, the “plug”, is flipped onto the base chip and pressed from the backside by a spring. Electrical contact with the eventual stress sensors, capacitive or piezoelectric sensor/actuators, is provided by contact bumps. These bumps of about 8 μm height are placed onto the base chip. They touch the pads on the AFM chip that were originally foreseen to be for wire bonding and thus provide the electrical contact. This connector schema was successfully used to register AFM images with piezoresistive cantilevers.

Combined use of atomic force microscopy, X-ray photoelectron spectroscopy, and secondary ion mass spectrometry for cell surface analysis.

PubMed

Dague, Etienne; Delcorte, Arnaud; Latgé, Jean-Paul; Dufrêne, Yves F

2008-04-01

Understanding the surface properties of microbial cells is a major challenge of current microbiological research and a key to efficiently exploit them in biotechnology. Here, we used three advanced surface analysis techniques with different sensitivity, probing depth, and lateral resolution, that is, in situ atomic force microscopy, X-ray photoelectron spectroscopy, and secondary ion mass spectrometry, to gain insight into the surface properties of the conidia of the human fungal pathogen Aspergillus fumigatus. We show that the native ultrastructure, surface protein and polysaccharide concentrations, and amino acid composition of three mutants affected in hydrophobin production are markedly different from those of the wild-type, thereby providing novel insight into the cell wall architecture of A. fumigatus. The results demonstrate the power of using multiple complementary techniques for probing microbial cell surfaces.

Resolution and contrast in Kelvin probe force microscopy

NASA Astrophysics Data System (ADS)

Jacobs, H. O.; Leuchtmann, P.; Homan, O. J.; Stemmer, A.

1998-08-01

The combination of atomic force microscopy and Kelvin probe technology is a powerful tool to obtain high-resolution maps of the surface potential distribution on conducting and nonconducting samples. However, resolution and contrast transfer of this method have not been fully understood, so far. To obtain a better quantitative understanding, we introduce a model which correlates the measured potential with the actual surface potential distribution, and we compare numerical simulations of the three-dimensional tip-specimen model with experimental data from test structures. The observed potential is a locally weighted average over all potentials present on the sample surface. The model allows us to calculate these weighting factors and, furthermore, leads to the conclusion that good resolution in potential maps is obtained by long and slender but slightly blunt tips on cantilevers of minimal width and surface area.

X-Ray Absorption Microspectroscopy with Electrostatic Force Microscopy and its Application to Chemical States Mapping

NASA Astrophysics Data System (ADS)

Ishii, M.; Rigopoulos, N.; Poolton, N. R. J.; Hamilton, B.

2007-02-01

A new technique named X-EFM that measures the x-ray absorption fine structure (XAFS) of nanometer objects was developed. In X-EFM, electrostatic force microscopy (EFM) is used as an x-ray absorption detector, and photoionization induced by x-ray absorption of surface electron trapping sites is detected by EFM. An EFM signal with respect to x-ray photon energy provides the XAFS spectra of the trapping sites. We adopted X-EFM to observe Si oxide thin films. An edge jump shift intrinsic to the X-EFM spectrum was found, and it was explained with a model where an electric field between the trapping site and probe deepens the energy level of the inner-shell. A scanning probe under x-rays with fixed photon energy provided the chemical state mapping on the surface.

Vector electric field measurement via position-modulated Kelvin probe force microscopy

NASA Astrophysics Data System (ADS)

Dwyer, Ryan P.; Smieska, Louisa M.; Tirmzi, Ali Moeed; Marohn, John A.

2017-10-01

High-quality spatially resolved measurements of electric fields are critical to understanding charge injection, charge transport, and charge trapping in semiconducting materials. Here, we report a variation of frequency-modulated Kelvin probe force microscopy that enables spatially resolved measurements of the electric field. We measure electric field components along multiple directions simultaneously by employing position modulation and lock-in detection in addition to numeric differentiation of the surface potential. We demonstrate the technique by recording linescans of the in-plane electric field vector in the vicinity of a patch of trapped charge in a 2,7-diphenyl[1]benzothieno[3,2-b][1]benzothiophene (DPh-BTBT) organic field-effect transistor. This technique is simple to implement and should be especially useful for studying electric fields in spatially inhomogeneous samples like organic transistors and photovoltaic blends.

Development of first ever scanning probe microscopy capabilities for plutonium

NASA Astrophysics Data System (ADS)

Beaux, Miles F.; Cordoba, Miguel Santiago; Zocco, Adam T.; Vodnik, Douglas R.; Ramos, Michael; Richmond, Scott; Moore, David P.; Venhaus, Thomas J.; Joyce, Stephen A.; Usov, Igor O.

2017-04-01

Scanning probe microscopy capabilities have been developed for plutonium and its derivative compounds. Specifically, a scanning tunneling microscope and an atomic force microscope housed in an ultra-high vacuum system and an inert atmosphere glove box, respectively, were prepared for the introduction of small non-dispersible δ-Pu coupons. Experimental details, procedures, and preliminary imaging of δ-Pu coupons are presented to demonstrate the functionality of these new capabilities. These first of a kind capabilities for plutonium represent a significant step forward in the ability to characterize and understand plutonium surfaces with high spatial resolution.

Development of first ever scanning probe microscopy capabilities for plutonium

DOE PAGES

Beaux, Miles F.; Cordoba, Miguel Santiago; Zocco, Adam T.; ...

2017-04-01

Scanning probe microscopy capabilities have been developed for plutonium and its derivative compounds. Specifically, a scanning tunneling microscope and an atomic force microscope housed in an ultra-high vacuum system and an inert atmosphere glove box, respectively, were prepared for the introduction of small non-dispersible δ-Pu coupons. Experimental details, procedures, and preliminary imaging of δ-Pu coupons are presented to demonstrate the functionality of these new capabilities. In conclusion, these first of a kind capabilities for plutonium represent a significant step forward in the ability to characterize and understand plutonium surfaces with high spatial resolution.

Design rules for biomolecular adhesion: lessons from force measurements.

PubMed

Leckband, Deborah

2010-01-01

Cell adhesion to matrix, other cells, or pathogens plays a pivotal role in many processes in biomolecular engineering. Early macroscopic methods of quantifying adhesion led to the development of quantitative models of cell adhesion and migration. The more recent use of sensitive probes to quantify the forces that alter or manipulate adhesion proteins has revealed much greater functional diversity than was apparent from population average measurements of cell adhesion. This review highlights theoretical and experimental methods that identified force-dependent molecular properties that are central to the biological activity of adhesion proteins. Experimental and theoretical methods emphasized in this review include the surface force apparatus, atomic force microscopy, and vesicle-based probes. Specific examples given illustrate how these tools have revealed unique properties of adhesion proteins and their structural origins.

High-voltage nano-oxidation in deionized water and atmospheric environments by atomic force microscopy.

PubMed

Huang, Jen-Ching; Chen, Chung-Ming

2012-01-01

This study used atomic force microscopy (AFM), metallic probes with a nanoscale tip, and high-voltage generators to investigate the feasibility of high-voltage nano-oxidation processing in deionized water (DI water) and atmospheric environments. Researchers used a combination of wire-cutting and electrochemical etching to transform a 20-μm-thick stainless steel sheet into a conductive metallic AFM probe with a tip radius of 60 nm, capable of withstanding high voltages. The combination of AFM, high-voltage generators, and nanoscale metallic probes enabled nano-oxidation processing at 200 V in DI water environments, producing oxides up to 66.6 nm in height and 467.03 nm in width. Oxides produced through high-voltage nano-oxidation in atmospheric environments were 117.29 nm in height and 551.28 nm in width, considerably exceeding the dimensions of those produced in DI water. An increase in the applied bias voltage led to an apparent logarithmic increase in the height of the oxide dots in the range of 200-400 V. The performance of the proposed high-voltage nano-oxidation technique was relatively high with seamless integration between the AFM machine and the metallic probe fabricated in this study. © Wiley Periodicals, Inc.

Direct measurements of intermolecular forces by chemical force microscopy

NASA Astrophysics Data System (ADS)

Vezenov, Dmitri Vitalievich

1999-12-01

Detailed description of intermolecular forces is key to understanding a wide range of phenomena from molecular recognition to materials failure. The unique features of atomic force microscopy (AFM) to make point contact force measurements with ultra high sensitivity and to generate spatial maps of surface topography and forces have been extended to include measurements between well-defined organic molecular groups. Chemical modification of AFM probes with self-assembled monolayers (SAMs) was used to make them sensitive to specific molecular interactions. This novel chemical force microscopy (CFM) technique was used to probe forces between different molecular groups in a range of environments (vacuum, organic liquids and aqueous solutions); measure surface energetics on a nanometer scale; determine pK values of the surface acid and base groups; measure forces to stretch and unbind a short synthetic DNA duplex and map the spatial distribution of specific functional groups and their ionization state. Studies of adhesion forces demonstrated the important contribution of hydrogen bonding to interactions between simple organic functionalities. The chemical identity of the tip and substrate surfaces as well as the medium had a dramatic effect on adhesion between model monolayers. A direct correlation between surface free energy and adhesion forces was established. The adhesion between epoxy polymer and model mixed SAMs varied with the amount of hydrogen bonding component in the monolayers. A consistent interpretation of CFM measurements in polar solvents was provided by contact mechanics models and intermolecular force components theory. Forces between tips and surfaces functionalized with SAMs terminating in acid or base groups depended on their ionization state. A novel method of force titration was introduced for highly local characterization of the pK's of surface functional groups. The pH-dependent changes in friction forces were exploited to map spatially the changes in ionization state on SAM surfaces. The phase contrast in tapping mode AFM between chemically distinct monolayer regions and corresponding adhesion forces were found to be directly correlated. Thus, both friction and intermittent contact CFM images could be interpreted in terms of the strength of intermolecular interactions. CFM was also used to probe biomolecular interactions. Separation forces between complementary oligonucleotide strands were significantly larger than the forces measured between noncomplementary strands and were consistent with the unbinding of a single DNA duplex. CFM data provided a direct measure of the forces required to elastically deform, structurally-transform and separate well-defined, synthetic duplexes into single strand oligonucleotides.

Conductive scanning probe microscopy of the semicontinuous gold film and its SERS enhancement toward two-step photo-induced charge transfer and effect of the supportive layer

NASA Astrophysics Data System (ADS)

Sinthiptharakoon, K.; Sapcharoenkun, C.; Nuntawong, N.; Duong, B.; Wutikhun, T.; Treetong, A.; Meemuk, B.; Kasamechonchung, P.; Klamchuen, A.

2018-05-01

The semicontinuous gold film, enabling various electronic applications including development of surface-enhanced Raman scattering (SERS) substrate, is investigated using conductive atomic force microscopy (CAFM) and Kelvin probe force microscopy (KPFM) to reveal and investigate local electronic characteristics potentially associated with SERS generation of the film material. Although the gold film fully covers the underlying silicon surface, CAFM results reveal that local conductivity of the film is not continuous with insulating nanoislands appearing throughout the surface due to incomplete film percolation. Our analysis also suggests the two-step photo-induced charge transfer (CT) play the dominant role in the enhancement of SERS intensity with strong contribution from free electrons of the silicon support. Silicon-to-gold charge transport is illustrated by KPFM results showing that Fermi level of the gold film is slightly inhomogeneous and far below the silicon conduction band. We propose that inhomogeneity of the film workfunction affecting chemical charge transfer between gold and Raman probe molecule is associated with the SERS intensity varying across the surface. These findings provide deeper understanding of charge transfer mechanism for SERS which can help in design and development of the semicontinuous gold film-based SERS substrate and other electronic applications.

Graphene engineering by neon ion beams

DOE PAGES

Iberi, Vighter; Ievlev, Anton V.; Vlassiouk, Ivan; ...

2016-02-18

Achieving the ultimate limits of materials and device performance necessitates the engineering of matter with atomic, molecular, and mesoscale fidelity. While common for organic and macromolecular chemistry, these capabilities are virtually absent for 2D materials. In contrast to the undesired effect of ion implantation from focused ion beam (FIB) lithography with gallium ions, and proximity effects in standard e-beam lithography techniques, the shorter mean free path and interaction volumes of helium and neon ions offer a new route for clean, resist free nanofabrication. Furthermore, with the advent of scanning helium ion microscopy, maskless He + and Ne + beam lithographymore » of graphene based nanoelectronics is coming to the forefront. Here, we will discuss the use of energetic Ne ions in engineering graphene devices and explore the mechanical, electromechanical and chemical properties of the ion-milled devices using scanning probe microscopy (SPM). By using SPM-based techniques such as band excitation (BE) force modulation microscopy, Kelvin probe force microscopy (KPFM) and Raman spectroscopy, we demonstrate that the mechanical, electrical and optical properties of the exact same devices can be quantitatively extracted. Additionally, the effect of defects inherent in ion beam direct-write lithography, on the overall performance of the fabricated devices is elucidated.« less

Atomic force microscopy of atomic-scale ledges and etch pits formed during dissolution of quartz

NASA Technical Reports Server (NTRS)

Gratz, A. J.; Manne, S.; Hansma, P. K.

1991-01-01

The processes involved in the dissolution and growth of crystals are closely related. Atomic force microscopy (AFM) of faceted pits (called negative crystals) formed during quartz dissolution reveals subtle details of these underlying physical mechanisms for silicates. In imaging these surfaces, the AFM detected ledges less than 1 nm high that were spaced 10 to 90 nm apart. A dislocation pit, invisible to optical and scanning electron microscopy measurements and serving as a ledge source, was also imaged. These observations confirm the applicability of ledge-motion models to dissolution and growth of silicates; coupled with measurements of dissolution rate on facets, these methods provide a powerful tool for probing mineral surface kinetics.

The nanoscale phase distinguishing of PCL-PB-PCL blended in epoxy resin by tapping mode atomic force microscopy

NASA Astrophysics Data System (ADS)

Li, Huiqin; Sun, Limin; Shen, Guangxia; Liang, Qi

2012-02-01

In this work, we investigated the bulk phase distinguishing of the poly(ɛ-caprolactone)-polybutadiene-poly(ɛ-caprolactone) (PCL-PB-PCL) triblock copolymer blended in epoxy resin by tapping mode atomic force microscopy (TM-AFM). We found that at a set-point amplitude ratio ( r sp) less than or equal to 0.85, a clear phase contrast could be obtained using a probe with a force constant of 40 N/m. When r sp was decreased to 0.1 or less, the measured size of the PB-rich domain relatively shrank; however, the height images of the PB-rich domain would take reverse (translating from the original light to dark) at r sp = 0.85. Force-probe measurements were carried out on the phase-separated regions by TM-AFM. According to the phase shift angle vs. r sp curve, it could be concluded that the different force exerting on the epoxy matrix or on the PB-rich domain might result in the height and phase image reversion. Furthermore, the indentation depth vs. r sp plot showed that with large tapping force (lower r sp), the indentation depth for the PB-rich domain was nearly identical for the epoxy resin matrix.

Measurements of stiff-material compliance on the nanoscale using ultrasonic force microscopy

NASA Astrophysics Data System (ADS)

Dinelli, F.; Biswas, S. K.; Briggs, G. A. D.; Kolosov, O. V.

2000-05-01

Ultrasonic force microscopy (UFM) was introduced to probe nanoscale mechanical properties of stiff materials. This was achieved by vibrating the sample far above the first resonance of the probing atomic force microscope cantilever where the cantilever becomes dynamically rigid. By operating UFM at different set force values, it is possible to directly measure the absolute values of the tip-surface contact stiffness. From this an evaluation of surface elastic properties can be carried out assuming a suitable solid-solid contact model. In this paper we present curves of stiffness as a function of the normal load in the range of 0-300 nN. The dependence of stiffness on the relative humidity has also been investigated. Materials with different elastic constants (such as sapphire lithium fluoride, and silicon) have been successfully differentiated. Continuum mechanics models cannot however explain the dependence of stiffness on the normal force and on the relative humidity. In this high-frequency regime, it is likely that viscous forces might play an important role modifying the tip-surface interaction. Plastic deformation might also occur due to the high strain rates applied when ultrasonically vibrating the sample. Another possible cause of these discrepancies might be the presence of water in between the two bodies in contact organizing in a solidlike way and partially sustaining the load.

Imaging latex–carbon nanotube composites by subsurface electrostatic force microscopy

DOE PAGES

Patel, Sajan; Petty, Clayton W.; Krafcik, Karen Lee; ...

2016-09-08

Electrostatic modes of atomic force microscopy have shown to be non-destructive and relatively simple methods for imaging conductors embedded in insulating polymers. Here we use electrostatic force microscopy to image the dispersion of carbon nanotubes in a latex-based conductive composite, which brings forth features not observed in previously studied systems employing linear polymer films. A fixed-potential model of the probe-nanotube electrostatics is presented which in principle gives access to the conductive nanoparticle's depth and radius, and the polymer film dielectric constant. Comparing this model to the data results in nanotube depths that appear to be slightly above the film–air interface.more » Furthermore, this result suggests that water-mediated charge build-up at the film–air interface may be the source of electrostatic phase contrast in ambient conditions.« less

Bias stress in PDI-CN2 and P3HT studied with Kelvin Probe Force Microscopy

NASA Astrophysics Data System (ADS)

Cao, Minxuan; Moscatello, Jason; Castaneda, Chloe; Xue, Binglan; Usluer, Ozlem; Briseno, Alejandro; Aidala, Katherine

We have developed a technique that uses scanning probe microscopy (SPM) to study the real-time injection and extraction of charge carriers in organic semiconductor devices. We investigate PDI-CN2 and P3HT in a back gate field effect transistor geometry with gold electrodes. By positioning the SPM tip at an individual location and using Kelvin probe microscopy to record the potential over time, we can record how the charge carriers respond to changing the gate voltage while the source and drain electrodes are grounded. We see relatively fast screening when carriers are injected into the film. The screening is slower when carriers must escape from traps to exit the film. By incrementally stepping the gate voltage, we can probe different trap depths. By repeating the measurement, we observe the development of longer lived trap states, shown by the longer time recorded to fully screen the gate voltage. This work is supported by NSF Grant DMR-0955348, and the Center for Heirarchical Manufacturing at the University of Massachusetts, Amherst (NSF CMMI-1025020).

Electrical Measurements and Nanomechanics Using Scanning Probe Microscopy

NASA Astrophysics Data System (ADS)

Chang, Yong

2002-10-01

In the early 1980s, G. Binnig et al. invented the Scanning Tunneling Microscopy (STM) [1], making it possible to obtain atomic resolution images of conducting surfaces. After that, many different types of Scanning Probe Microscopy (SPM) were invented and some of the most useful representatives are Atomic Force Microscopy (AFM) [2], Electrostatic Force Microscopy (EFM) [3] and Kelvin Probe Force Microscopy (KPFM) [4,5]. In 1985, G. Binnig et al. [2] invented the AFM, which now is used as a fundamental tool in many fields of research. Developed from AFM, Y. Martin et al. [3] invented EFM in 1987. The development of AC mode AFM allows the detection of weak long-range forces. EFM has also been used to study other systems and phenomena, such as thin liquid films on solid surfaces [6], electrically stressed gold nanowires [7], and spatial charge distribution in quantum wires [8]. In 1991, M. Nonnenmacher et al. [5] invented Kelvin Probe Force Microscopy. KPFM is used to study any property that affects the tip-surface Contact Potential Difference (CPD), such as voltage signals in integrated circuits (IC) [9], charged grain boundaries in polycrystalline silicon [10] and surface potential variations in multilayer semiconductor devices [11]. The aim of this poster is to discuss the application of SPM to electrical measurements. The theory of SPM was presented. The AFM was firstly introduced as it was developed before the other two. The design and theory were discussed. The force-distance curve was introduced. After this EFM was presented. EFM was developed from AC mode AFM. The technique was achieved by applying a DC voltage between the tip and the sample. The design, theory and features of it were surveyed. KPFM was also discussed. KPFM was developed from EFM. The central part of this technique is to measure the CPD. Experimental measurements of SPM were described after theory part. Research work using AFM was presented. The newest technique of AFM, UHV-AFM has been used in investigating the nano-mechanical properties of different materials. Normally common AFM has shortcomings as it has either strict limit resolution or difficulties in interpreting the data from the measurements. In order to solve these problems, Ultra High Vacuum (UHV) conditions were applied to acquire quantitative results. A typical UHV-AFM uses a cantilever whose spring constant is relatively high (>100 N/m) to obtain high-resolution image. Experimental measurements using KPFM was presented after AFM. Researchers are using KPFM to acquire the topography and measuring the CPD of semiconductor or metal surfaces. Similarly as in AFM, KPFM works best in UHV environment. A typical UHV-KPFM also uses a cantilever whose spring constant is relatively high. A UHV-KPFM may be able to achieve a high resolution in CPD images. In the past 20 years many different kinds of SPM were invented and used. AFM, EFM, and KPFM are representatives of them. Researchers are still developing new techniques. However, in recent years, they pay more attention in improving the measurement accuracy instead of trying to invent new SPM. These three SPM continue to be frequently used. The current capabilities of SPM do not satisfy us completely. We still cant measure the Electrical field directly. We actually measure the capacitance gradient. There are also some other questions. This is because the electrostatic force depends very strongly on the geometry of the probe at all length scales, so any model is subject to two big problems. First, the geometry is not known with complete accuracy; and second, the tip shape can change during an experiment due to wear. In the future, maybe the problems could be overcome by using a tip with a very well defined shape, such as a carbon nanotube, for which a realistic geometrical model could be more easily constructed, and the wear could be avoided or reduced.

DNA and RNA sequencing by nanoscale reading through programmable electrophoresis and nanoelectrode-gated tunneling and dielectric detection

DOEpatents

Lee, James W.; Thundat, Thomas G.

2005-06-14

An apparatus and method for performing nucleic acid (DNA and/or RNA) sequencing on a single molecule. The genetic sequence information is obtained by probing through a DNA or RNA molecule base by base at nanometer scale as though looking through a strip of movie film. This DNA sequencing nanotechnology has the theoretical capability of performing DNA sequencing at a maximal rate of about 1,000,000 bases per second. This enhanced performance is made possible by a series of innovations including: novel applications of a fine-tuned nanometer gap for passage of a single DNA or RNA molecule; thin layer microfluidics for sample loading and delivery; and programmable electric fields for precise control of DNA or RNA movement. Detection methods include nanoelectrode-gated tunneling current measurements, dielectric molecular characterization, and atomic force microscopy/electrostatic force microscopy (AFM/EFM) probing for nanoscale reading of the nucleic acid sequences.

Investigation of surface potentials in reduced graphene oxide flake by Kelvin probe force microscopy

NASA Astrophysics Data System (ADS)

Negishi, Ryota; Takashima, Kai; Kobayashi, Yoshihiro

2018-06-01

The surface potential (SP) of reduced graphene oxide (rGO) flakes prepared by thermal treatments of GO under several conditions was analyzed by Kelvin probe force microscopy. The low-crystalline rGO flakes in which a significant amount of oxygen functional groups and structural defects remain have a much lower SP than mechanically exfoliated graphene free from oxygen and defects. On the other hand, the highly crystalline rGO flake after a thermal treatment for the efficient removal of oxygen functional groups and healing of structural defects except for domain boundary shows SP equivalent to that of the mechanically exfoliated graphene. These results indicate that the work function of rGO is sensitively modulated by oxygen functional groups and structural defects remaining after the thermal reduction process, but is not affected significantly by the domain boundary remaining after the healing of structural defects through the thermal treatment at high temperature.

Visualizing the orientational dependence of an intermolecular potential

NASA Astrophysics Data System (ADS)

Sweetman, Adam; Rashid, Mohammad A.; Jarvis, Samuel P.; Dunn, Janette L.; Rahe, Philipp; Moriarty, Philip

2016-02-01

Scanning probe microscopy can now be used to map the properties of single molecules with intramolecular precision by functionalization of the apex of the scanning probe tip with a single atom or molecule. Here we report on the mapping of the three-dimensional potential between fullerene (C60) molecules in different relative orientations, with sub-Angstrom resolution, using dynamic force microscopy (DFM). We introduce a visualization method which is capable of directly imaging the variation in equilibrium binding energy of different molecular orientations. We model the interaction using both a simple approach based around analytical Lennard-Jones potentials, and with dispersion-force-corrected density functional theory (DFT), and show that the positional variation in the binding energy between the molecules is dominated by the onset of repulsive interactions. Our modelling suggests that variations in the dispersion interaction are masked by repulsive interactions even at displacements significantly larger than the equilibrium intermolecular separation.

Conductive-probe atomic force microscopy characterization of silicon nanowire

PubMed Central

2011-01-01

The electrical conduction properties of lateral and vertical silicon nanowires (SiNWs) were investigated using a conductive-probe atomic force microscopy (AFM). Horizontal SiNWs, which were synthesized by the in-plane solid-liquid-solid technique, are randomly deployed into an undoped hydrogenated amorphous silicon layer. Local current mapping shows that the wires have internal microstructures. The local current-voltage measurements on these horizontal wires reveal a power law behavior indicating several transport regimes based on space-charge limited conduction which can be assisted by traps in the high-bias regime (> 1 V). Vertical phosphorus-doped SiNWs were grown by chemical vapor deposition using a gold catalyst-driving vapor-liquid-solid process on higly n-type silicon substrates. The effect of phosphorus doping on the local contact resistance between the AFM tip and the SiNW was put in evidence, and the SiNWs resistivity was estimated. PMID:21711623

Calibrated work function mapping by Kelvin probe force microscopy

NASA Astrophysics Data System (ADS)

Fernández Garrillo, Pablo A.; Grévin, Benjamin; Chevalier, Nicolas; Borowik, Łukasz

2018-04-01

We propose and demonstrate the implementation of an alternative work function tip calibration procedure for Kelvin probe force microscopy under ultrahigh vacuum, using monocrystalline metallic materials with known crystallographic orientation as reference samples, instead of the often used highly oriented pyrolytic graphite calibration sample. The implementation of this protocol allows the acquisition of absolute and reproducible work function values, with an improved uncertainty with respect to unprepared highly oriented pyrolytic graphite-based protocols. The developed protocol allows the local investigation of absolute work function values over nanostructured samples and can be implemented in electronic structures and devices characterization as demonstrated over a nanostructured semiconductor sample presenting Al0.7Ga0.3As and GaAs layers with variable thickness. Additionally, using our protocol we find that the work function of annealed highly oriented pyrolytic graphite is equal to 4.6 ± 0.03 eV.

Probing local work function of electron emitting Si-nanofacets

NASA Astrophysics Data System (ADS)

Basu, Tanmoy; Som, Tapobrata

2017-10-01

Large area, Si-nanofacets are synthesized by obliquely incident low energy Ar+-ion-beam bombardment at room temperature (RT). The field emission properties of such nanofacets are studied based on current-voltage measurements and the Fowler-Nordheim equation. Low turn-on field with relatively high current density is obtained due to the shape and an overall rough morphology. We demonstrate a tunable field emission property from the silicon nanofacets by varying the ion exposure time. Atomic force microscopy (AFM) in conjunction with Kelvin probe force microscopy (KPFM) measurements provide the information on the aspect ratio and confirms the presence of native oxide layer near the apexes of the facets, respectively. The inhomogeneous oxidation leads to an increase in the local work function at the apexes of the facets, restricting the electron emission from the same. Due to its room temperature fabrication, the present method is of great significance to the low-cost vacuum field emission devices fabrication.

Diminish electrostatic in piezoresponse force microscopy through longer or ultra-stiff tips

NASA Astrophysics Data System (ADS)

Gomez, A.; Puig, T.; Obradors, X.

2018-05-01

Piezoresponse Force Microscopy is a powerful but delicate nanoscale technique that measures the electromechanical response resulting from the application of a highly localized electric field. Though mechanical response is normally due to piezoelectricity, other physical phenomena, especially electrostatic interaction, can contribute to the signal read. We address this problematic through the use of longer ultra-stiff probes providing state of the art sensitivity, with the lowest electrostatic interaction and avoiding working in high frequency regime. In order to find this solution we develop a theoretical description addressing the effects of electrostatic contributions in the total cantilever vibration and its quantification for different setups. The theory is subsequently tested in a Periodically Poled Lithium Niobate (PPLN) crystal, a sample with well-defined 0° and 180° domains, using different commercial available conductive tips. We employ the theoretical description to compare the electrostatic contribution effects into the total phase recorded. Through experimental data our description is corroborated for each of the tested commercially available probes. We propose that a larger probe length can be a solution to avoid electrostatic forces, so the cantilever-sample electrostatic interaction is reduced. Our proposed solution has great implications into avoiding artifacts while studying soft biological samples, multiferroic oxides, and thin film ferroelectric materials.

Picoampere Resistive Switching Characteristics Realized with Vertically Contacted Carbon Nanotube Atomic Force Microscope Probe

NASA Astrophysics Data System (ADS)

Nakano, Haruhisa; Takahashi, Makoto; Sato, Motonobu; Kotsugi, Masato; Ohkochi, Takuo; Muro, Takayuki; Nihei, Mizuhisa; Yokoyama, Naoki

2013-11-01

The resistive switching characteristics of a TiO2/Ti structure have been investigated using a conductive atomic force microscopy (AFM) system with 5-nm-diameter carbon nanotube (CNT) probes. The resistive switching showed bipolar resistive random access memory (ReRAM) behaviors with extremely low switching currents in the order of Picoamperes when voltages were applied. From transmission electron microscopy (TEM) observation, we confirmed that filament-like nanocrystals, having a diameter of about 10 nm, existed in TiO2 films at resistive switching areas after not only set operation but also reset operation. Moreover, photoemission electron microscopy (PEEM) analysis showed that the anatase-type TiO2 structure did not change after set and reset operations. From these results, we suggested that the Picoampere resistive switching occurred at the interface between the TiO2 dielectric and conductive nanocrystal without any structural changes in the TiO2 film and nanocrystal. The resistive switching mechanism we suggested is highly promising to realize extremely low-power-consumption ReRAMs with vertically contacted CNT electrodes.

A beginner's guide to atomic force microscopy probing for cell mechanics

PubMed Central

2016-01-01

Abstract Atomic Force microscopy (AFM) is becoming a prevalent tool in cell biology and biomedical studies, especially those focusing on the mechanical properties of cells and tissues. The newest generation of bio‐AFMs combine ease of use and seamless integration with live‐cell epifluorescence or more advanced optical microscopies. As a unique feature with respect to other bionanotools, AFM provides nanometer‐resolution maps for cell topography, stiffness, viscoelasticity, and adhesion, often overlaid with matching optical images of the probed cells. This review is intended for those about to embark in the use of bio‐AFMs, and aims to assist them in designing an experiment to measure the mechanical properties of adherent cells. In addition to describing the main steps in a typical cell mechanics protocol and explaining how data is analysed, this review will also discuss some of the relevant contact mechanics models available and how they have been used to characterize specific features of cellular and biological samples. Microsc. Res. Tech. 80:75–84, 2017. © 2016 Wiley Periodicals, Inc. PMID:27676584

Towards High-Resolution Tissue Imaging Using Nanospray Desorption Electrospray Ionization Mass Spectrometry Coupled to Shear Force Microscopy

NASA Astrophysics Data System (ADS)

Nguyen, Son N.; Sontag, Ryan L.; Carson, James P.; Corley, Richard A.; Ansong, Charles; Laskin, Julia

2018-02-01

Constant mode ambient mass spectrometry imaging (MSI) of tissue sections with high lateral resolution of better than 10 μm was performed by combining shear force microscopy with nanospray desorption electrospray ionization (nano-DESI). Shear force microscopy enabled precise control of the distance between the sample and nano-DESI probe during MSI experiments and provided information on sample topography. Proof-of-concept experiments were performed using lung and brain tissue sections representing spongy and dense tissues, respectively. Topography images obtained using shear force microscopy were comparable to the results obtained using contact profilometry over the same region of the tissue section. Variations in tissue height were found to be dependent on the tissue type and were in the range of 0-5 μm for lung tissue and 0-3 μm for brain tissue sections. Ion images of phospholipids obtained in this study are in good agreement with literature data. Normalization of nano-DESI MSI images to the signal of the internal standard added to the extraction solvent allowed us to construct high-resolution ion images free of matrix effects.

Probing lipid membrane electrostatics

NASA Astrophysics Data System (ADS)

Yang, Yi

The electrostatic properties of lipid bilayer membranes play a significant role in many biological processes. Atomic force microscopy (AFM) is highly sensitive to membrane surface potential in electrolyte solutions. With fully characterized probe tips, AFM can perform quantitative electrostatic analysis of lipid membranes. Electrostatic interactions between Silicon nitride probes and supported zwitterionic dioleoylphosphatidylcholine (DOPC) bilayer with a variable fraction of anionic dioleoylphosphatidylserine (DOPS) were measured by AFM. Classical Gouy-Chapman theory was used to model the membrane electrostatics. The nonlinear Poisson-Boltzmann equation was numerically solved with finite element method to provide the potential distribution around the AFM tips. Theoretical tip-sample electrostatic interactions were calculated with the surface integral of both Maxwell and osmotic stress tensors on tip surface. The measured forces were interpreted with theoretical forces and the resulting surface charge densities of the membrane surfaces were in quantitative agreement with the Gouy-Chapman-Stern model of membrane charge regulation. It was demonstrated that the AFM can quantitatively detect membrane surface potential at a separation of several screening lengths, and that the AFM probe only perturbs the membrane surface potential by <2%. One important application of this technique is to estimate the dipole density of lipid membrane. Electrostatic analysis of DOPC lipid bilayers with the AFM reveals a repulsive force between the negatively charged probe tips and the zwitterionic lipid bilayers. This unexpected interaction has been analyzed quantitatively to reveal that the repulsion is due to a weak external field created by the internai membrane dipole moment. The analysis yields a dipole moment of 1.5 Debye per lipid with a dipole potential of +275 mV for supported DOPC membranes. This new ability to quantitatively measure the membrane dipole density in a noninvasive manner will be useful in identifying the biological effects of the dipole potential. Finally, heterogeneous model membranes were studied with fluid electric force microscopy (FEFM). Electrostatic mapping was demonstrated with 50 nm resolution. The capabilities of quantitative electrostatic measurement and lateral charge density mapping make AFM a unique and powerful probe of membrane electrostatics.

Surface polymerization of (3,4-ethylenedioxythiophene) probed by in situ scanning tunneling microscopy on Au(111) in ionic liquids.

PubMed

Ahmad, Shahzada; Carstens, Timo; Berger, Rüdiger; Butt, Hans-Jürgen; Endres, Frank

2011-01-01

The electropolymerization of 3,4-ethylenedioxythiophene (EDOT) to poly(3,4-ethylenedioxythiophene) (PEDOT) was investigated in the air and water-stable ionic liquids 1-hexyl-3-methylimidazolium tris(pentafluoroethyl) trifluorophosphate [HMIm]FAP and 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl) amide [EMIm]TFSA. In situ scanning tunnelling microscopy (STM) results show that the electropolymerization of EDOT in the ionic liquid can be probed on the nanoscale. In contrast to present understanding, it was observed that the EDOT can be oxidised in ionic liquids well below its oxidation potential and the under potential growth of polymer was visualized by in situ STM. These results serve as the first study to confirm the under potential growth of conducting polymers in ionic liquids. Furthermore, ex situ microscopy measurements were performed. Quite a high current of 670 nA was observed on the nanoscale by conductive scanning force microscopy (CSFM).

Distinct Chemical Contrast in Adhesion Force Images of Hydrophobic-Hydrophilic Patterned Surfaces Using Multiwalled Carbon Nanotube Probe Tips

NASA Astrophysics Data System (ADS)

Azehara, Hiroaki; Kasanuma, Yuka; Ide, Koichiro; Hidaka, Kishio; Tokumoto, Hiroshi

2008-05-01

In this paper, we describe a fabrication procedure for large-diameter carbon nanotube probe tips (CNT tips) for atomic force microscopy, the tip-end chemistry of the CNT tips, and their advantage drawn from the study of adhesion force imaging in an ambient atmosphere on a patterned hydrophobic and hydrophilic self-assembled monolayer, which has been prepared by a microcontact printing method. Force titration measurements in phosphate buffer solutions reveal that the CNT tip has retained carboxyl groups at its end. In adhesion force imaging, a distinct chemical contrast is obtained for the patterned surfaces as compared to a case using a silicon nitride tip. The origin of the distinct contrast is discussed in terms of the tip-end chemistry featured by carboxyl groups and a possible weakening of capillary forces of water caused at around the tip-sample interface because of the intrinsically hydrophobic nature of CNTs.

Invited review article: high-speed flexure-guided nanopositioning: mechanical design and control issues.

PubMed

Yong, Y K; Moheimani, S O R; Kenton, B J; Leang, K K

2012-12-01

Recent interest in high-speed scanning probe microscopy for high-throughput applications including video-rate atomic force microscopy and probe-based nanofabrication has sparked attention on the development of high-bandwidth flexure-guided nanopositioning systems (nanopositioners). Such nanopositioners are designed to move samples with sub-nanometer resolution with positioning bandwidth in the kilohertz range. State-of-the-art designs incorporate uniquely designed flexure mechanisms driven by compact and stiff piezoelectric actuators. This paper surveys key advances in mechanical design and control of dynamic effects and nonlinearities, in the context of high-speed nanopositioning. Future challenges and research topics are also discussed.

Piezo-thermal Probe Array for High Throughput Applications

PubMed Central

Gaitas, Angelo; French, Paddy

2012-01-01

Microcantilevers are used in a number of applications including atomic-force microscopy (AFM). In this work, deflection-sensing elements along with heating elements are integrated onto micromachined cantilever arrays to increase sensitivity, and reduce complexity and cost. An array of probes with 5–10 nm gold ultrathin film sensors on silicon substrates for high throughput scanning probe microscopy is developed. The deflection sensitivity is 0.2 ppm/nm. Plots of the change in resistance of the sensing element with displacement are used to calibrate the probes and determine probe contact with the substrate. Topographical scans demonstrate high throughput and nanometer resolution. The heating elements are calibrated and the thermal coefficient of resistance (TCR) is 655 ppm/K. The melting temperature of a material is measured by locally heating the material with the heating element of the cantilever while monitoring the bending with the deflection sensing element. The melting point value measured with this method is in close agreement with the reported value in literature. PMID:23641125

Electron microscopy of electromagnetic waveforms.

PubMed

Ryabov, A; Baum, P

2016-07-22

Rapidly changing electromagnetic fields are the basis of almost any photonic or electronic device operation. We report how electron microscopy can measure collective carrier motion and fields with subcycle and subwavelength resolution. A collimated beam of femtosecond electron pulses passes through a metamaterial resonator that is previously excited with a single-cycle electromagnetic pulse. If the probing electrons are shorter in duration than half a field cycle, then time-frozen Lorentz forces distort the images quasi-classically and with subcycle time resolution. A pump-probe sequence reveals in a movie the sample's oscillating electromagnetic field vectors with time, phase, amplitude, and polarization information. This waveform electron microscopy can be used to visualize electrodynamic phenomena in devices as small and fast as available. Copyright © 2016, American Association for the Advancement of Science.

Time-resolved electric force microscopy of charge trapping in polycrystalline pentacene.

PubMed

Jaquith, Michael; Muller, Erik M; Marohn, John A

2007-07-12

Here we introduce time-resolved electric force microscopy measurements to directly and locally probe the kinetics of charge trap formation in a polycrystalline pentacene thin-film transistor. We find that the trapping rate depends strongly on the initial concentration of free holes and that trapped charge is highly localized. The observed dependence of trapping rate on the hole chemical potential suggests that the trapping process should not be viewed as a filling of midgap energy levels, but instead as a process in which the very creation of trapped states requires the presence of free holes.

Technology for fabrication of a micromagnet on a tip of a MFM/MRFM probe

DOEpatents

Pelekhov, Denis V.; Hammel, P. Chris; Nunes, Jr., Geoffrey; Midzor, Melissa M.; Roukes, Michael

2004-01-13

A method for coating the tip of a mechanical resonator for use in magnetic force microscopy and magnetic resonance force microscopy in which the tip is coated with a ferromagnetic material and the cantilever is not, and the product resulting from the method. A cantilever and incorporated tip are coated with a photoresist, except that surface tension keeps photoresist off the tip. The cantilever and tip are then coated with a magnetic material. Next, acetone is used to lift off the magnetic material from the cantilever but not from the tip.

Noncontact Viscoelastic Imaging of Living Cells Using a Long-Needle Atomic Force Microscope with Dual-Frequency Modulation

NASA Astrophysics Data System (ADS)

Guan, Dongshi; Charlaix, Elisabeth; Qi, Robert Z.; Tong, Penger

2017-10-01

Imaging of surface topography and elasticity of living cells can provide insight into the roles played by the cells' volumetric and mechanical properties and their response to external forces in regulating the essential cellular events and functions. Here, we report a unique technique of noncontact viscoelastic imaging of live cells using atomic force microscopy (AFM) with a long-needle glass probe. Because only the probe tip is placed in a liquid medium near the cell surface, the AFM cantilever in air functions well under dual-frequency modulation, retaining its high-quality resonant modes. The probe tip interacts with the cell surface through a minute hydrodynamic flow in the nanometer-thin gap region between them without physical contact. Quantitative measurements of the cell height, volume, and Young's modulus are conducted simultaneously. The experiment demonstrates that the long-needle AFM has a wide range of applications in the study of cell mechanics.

Measuring the mechanical properties of molecular conformers

NASA Astrophysics Data System (ADS)

Jarvis, S. P.; Taylor, S.; Baran, J. D.; Champness, N. R.; Larsson, J. A.; Moriarty, P.

2015-09-01

Scanning probe-actuated single molecule manipulation has proven to be an exceptionally powerful tool for the systematic atomic-scale interrogation of molecular adsorbates. To date, however, the extent to which molecular conformation affects the force required to push or pull a single molecule has not been explored. Here we probe the mechanochemical response of two tetra(4-bromophenyl)porphyrin conformers using non-contact atomic force microscopy where we find a large difference between the lateral forces required for manipulation. Remarkably, despite sharing very similar adsorption characteristics, variations in the potential energy surface are capable of prohibiting probe-induced positioning of one conformer, while simultaneously permitting manipulation of the alternative conformational form. Our results are interpreted in the context of dispersion-corrected density functional theory calculations which reveal significant differences in the diffusion barriers for each conformer. These results demonstrate that conformational variation significantly modifies the mechanical response of even simple porpyhrins, potentially affecting many other flexible molecules.

Detection of stiff nanoparticles within cellular structures by contact resonance atomic force microscopy subsurface nanomechanical imaging.

PubMed

Reggente, Melania; Passeri, Daniele; Angeloni, Livia; Scaramuzzo, Francesca Anna; Barteri, Mario; De Angelis, Francesca; Persiconi, Irene; De Stefano, Maria Egle; Rossi, Marco

2017-05-04

Detecting stiff nanoparticles buried in soft biological matrices by atomic force microscopy (AFM) based techniques represents a new frontier in the field of scanning probe microscopies, originally developed as surface characterization methods. Here we report the detection of stiff (magnetic) nanoparticles (NPs) internalized in cells by using contact resonance AFM (CR-AFM) employed as a potentially non-destructive subsurface characterization tool. Magnetite (Fe 3 O 4 ) NPs were internalized in microglial cells from cerebral cortices of mouse embryos of 18 days by phagocytosis. Nanomechanical imaging of cells was performed by detecting the contact resonance frequencies (CRFs) of an AFM cantilever held in contact with the sample. Agglomerates of NPs internalized in cells were visualized on the basis of the local increase in the contact stiffness with respect to the surrounding biological matrix. A second AFM-based technique for nanomechanical imaging, i.e., HarmoniX™, as well as magnetic force microscopy and light microscopy were used to confirm the CR-AFM results. Thus, CR-AFM was demonstrated as a promising technique for subsurface imaging of nanomaterials in biological samples.

A quantitative comparison of resolution, scanning speed and lifetime behavior of CVD grown Single Wall Carbon Nanotubes and silicon SPM probes using spectral methods

NASA Astrophysics Data System (ADS)

Krause, O.; Bouchiat, V.; Bonnot, A. M.

2007-03-01

Due to their extreme aspect ratios and exceptional mechanical properties Carbon Nanotubes terminated silicon probes have proven to be the ''ideal'' probe for Atomic Force Microscopy. But especially for the manufacturing and use of Single Walled Carbon Nanotubes there are serious problems, which have not been solved until today. Here, Single and Double Wall Carbon Nanotubes, batch processed and used as deposited by Chemical Vapor Deposition without any postprocessing, are compared to standard and high resolution silicon probes concerning resolution, scanning speed and lifetime behavior.

Surface characterization of InP trenches embedded in oxide using scanning probe microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mannarino, Manuel, E-mail: manuel.mannarino@imec.be, E-mail: manuelmannarino@gmail.com; Chintala, Ravi; Vandervorst, Wilfried

2015-12-14

Metrology for structural and electrical analyses at device level has been identified as one of the major challenges to be resolved for the sub-14 nm technology nodes. In these advanced nodes, new high mobility semiconductors, such as III–V compounds, are grown in narrow trenches on a Si substrate. Probing the nature of the defects, the defect density, and the role of processing steps on the surface of such structures are prime metrology requirements. In order to enable defect analysis on a (III–V) surface, a proper sample preparation for oxide removal is of primary importance. In this work, the effectiveness of differentmore » chemical cleanings and thermal annealing procedures is investigated on both blanket InP and oxide embedded InP trenches by means of scanning probe microscopy techniques. It is found that the most effective approach is a combination of an HCl-based chemical cleaning combined with a low-temperature thermal annealing leading to an oxide free surface with atomically flat areas. Scanning tunneling microscopy (STM) has been the preferred method for such investigations on blanket films due to its intrinsic sub-nm spatial resolution. However, its application on oxide embedded structures is non-trivial. To perform STM on the trenches of interest (generally <20 nm wide), we propose a combination of non-contact atomic force microscopy and STM using the same conductive atomic force microscopy tip Our results prove that with these procedures, it is possible to perform STM in narrow InP trenches showing stacking faults and surface reconstruction. Significant differences in terms of roughness and terrace formation are also observed between the blanket and the oxide embedded InP.« less

Organic nanofibers from squarylium dyes: local morphology, optical, and electrical properties

NASA Astrophysics Data System (ADS)

Balzer, Frank; Schiek, Manuela; Osadnik, Andreas; Lützen, Arne; Rubahn, Horst-Günter

2012-02-01

Environmentally stable, non-toxic squarylium dyes with strong absorption maxima in the red and near infrared spectral region are known for almost fifty years. Despite the fact that their optoelectronic properties distinguish them as promising materials for organics based photovoltaic cells, they have regained attention only very recently. For their application in heterojunction solar cells knowledge of their nanoscopic morphology as well as nanoscopic electrical properties is paramount. In this paper thin films from two different squarylium dyes, from squarylium (SQ) and from hydroxy-squarylium (SQOH) are investigated. The thin films are either solution casted or vacuum sublimed onto substrates such as muscovite mica, which are known to promote self-assembly into oriented, crystalline nanostructures such as nanofibers. Local characterization is performed via (polarized) optical microscopy, scanning electron microscopy (SEM), atomic force microscopy (AFM), and Kelvin probe force microscopy (KPFM).

Nano-material processing with laser radiation in the near field of a scanning probe tip

NASA Astrophysics Data System (ADS)

Jersch, J.; Demming, F.; Hildenhagen, J.; Dickmann, K.

1998-04-01

We report preliminary results of using a scanning probe microscope/laser combination to perform nanostructuring on insulator and metal surfaces in air. This technique enables processing of structures with a lateral resolution of approximately 10 nm. In this paper we present our last structuring results with both scanning tunnelling and scanning force microscopy. Some possible interaction mechanisms responsible for the structuring will be discussed.

Intermolecular and interfacial forces: Elucidating molecular mechanisms using chemical force microscopy

NASA Astrophysics Data System (ADS)

Ashby, Paul David

Investigation into the origin of forces dates to the early Greeks. Yet, only in recent decades have techniques for elucidating the molecular origin of forces been developed. Specifically, Chemical Force Microscopy uses the high precision and nanometer scale probe of Atomic Force Microscopy to measure molecular and interfacial interactions. This thesis presents the development of many novel Chemical Force Microscopy techniques for measuring equilibrium and time-dependant force profiles of molecular interactions, which led to a greater understanding of the origin of interfacial forces in solution. In chapter 2, Magnetic Feedback Chemical Force Microscopy stiffens the cantilever for measuring force profiles between self-assembled monolayer (SAM) surfaces. Hydroxyl and carboxyl terminated SAMs produce long-range interactions that extend one or three nanometers into the solvent, respectively. In chapter 3, an ultra low noise AFM is produced through multiple modifications to the optical deflection detection system and signal processing electronics. In chapter 4, Brownian Force Profile Reconstruction is developed for accurate measurement of steep attractive interactions. Molecular ordering is observed for OMCTS, 1-nonanol, and water near flat surfaces. The molecular ordering of the solvent produces structural or solvation forces, providing insight into the orientation and possible solidification of the confined solvent. Seven molecular layers of OMCTS are observed but the oil remains fluid to the last layer. 1-nonanol strongly orders near the surface and becomes quasi-crystalline with four layers. Water is oriented by the surface and symmetry requires two layers of water (3.7 A) to be removed simultaneously. In chapter 5, electronic control of the cantilever Q (Q-control) is used to obtain the highest imaging sensitivity. In chapter 6, Energy Dissipation Chemical Force Microscopy is developed to investigate the time dependence and dissipative characteristics of SAM interfacial interactions in solution. Long-range adhesive forces for hydroxyl and carboxyl terminated SAM surfaces arise from solvent, not ionic, interactions. Exclusion of the solvent and contact between the SAM surfaces leads to rearrangement of the SAM headgroups. The isolation of the chemical and physical interfacial properties from the topography by Energy Dissipation Chemical Force Microscopy produces a new quantitative high-sensitivity imaging mode.

Methodology for extraction of space charge density profiles at nanoscale from Kelvin probe force microscopy measurements.

PubMed

Villeneuve-Faure, C; Boudou, L; Makasheva, K; Teyssedre, G

2017-12-15

To understand the physical phenomena occurring at metal/dielectric interfaces, determination of the charge density profile at nanoscale is crucial. To deal with this issue, charges were injected applying a DC voltage on lateral Al-electrodes embedded in a SiN x thin dielectric layer. The surface potential induced by the injected charges was probed by Kelvin probe force microscopy (KPFM). It was found that the KPFM frequency mode is a better adapted method to probe accurately the charge profile. To extract the charge density profile from the surface potential two numerical approaches based on the solution to Poisson's equation for electrostatics were investigated: the second derivative model method, already reported in the literature, and a new 2D method based on the finite element method (FEM). Results highlight that the FEM is more robust to noise or artifacts in the case of a non-flat initial surface potential. Moreover, according to theoretical study the FEM appears to be a good candidate for determining charge density in dielectric films with thicknesses in the range from 10 nm to 10 μm. By applying this method, the charge density profile was determined at nanoscale, highlighting that the charge cloud remains close to the interface.

Vacuum scanning capillary photoemission microscopy.

PubMed

Aseyev, S A; Cherkun, A P; Mironov, B N; Petrunin, V V; Chekalin, S V

2017-08-01

We demonstrate the use of a conical capillary in a scanning probe microscopy for surface analysis. The probe can measure photoemission from a substrate by transmitting photoelectrons along the capillary as a function of probe position. The technique is demonstrated on a model substrate consisting of a gold reflecting layer on a compact disc which has been illuminated by an unfocused laser beam with a wavelength 400nm, from a femtosecond laser with a beam size of 4mm. A quartz capillary with a 2-µm aperture has been used in the experiments. The period of gold microstructure, shown to be 1.6µ, was measured by the conical probe operating in shear force mode. In shear force regime, the dielectric capillary has been used as a "classical" SPM tip, which provided images reflecting the surface topology. In a photoelectron regime photoelectrons passed through hollow tip and entered a detector. The spatial distribution of the recorded photoelectrons consisted of periodic mountain-valley strips, resembling the surface profile of the sample. Submicron spatial resolution has been achieved. This approach paves the way to study pulsed photodesorption of large organic molecular ions with high spatial and element resolution using the combination of a hollow-tip scanner with time-of-flight technique. Copyright © 2017 Elsevier B.V. All rights reserved.

Methodology for extraction of space charge density profiles at nanoscale from Kelvin probe force microscopy measurements

NASA Astrophysics Data System (ADS)

Villeneuve-Faure, C.; Boudou, L.; Makasheva, K.; Teyssedre, G.

2017-12-01

To understand the physical phenomena occurring at metal/dielectric interfaces, determination of the charge density profile at nanoscale is crucial. To deal with this issue, charges were injected applying a DC voltage on lateral Al-electrodes embedded in a SiN x thin dielectric layer. The surface potential induced by the injected charges was probed by Kelvin probe force microscopy (KPFM). It was found that the KPFM frequency mode is a better adapted method to probe accurately the charge profile. To extract the charge density profile from the surface potential two numerical approaches based on the solution to Poisson’s equation for electrostatics were investigated: the second derivative model method, already reported in the literature, and a new 2D method based on the finite element method (FEM). Results highlight that the FEM is more robust to noise or artifacts in the case of a non-flat initial surface potential. Moreover, according to theoretical study the FEM appears to be a good candidate for determining charge density in dielectric films with thicknesses in the range from 10 nm to 10 μm. By applying this method, the charge density profile was determined at nanoscale, highlighting that the charge cloud remains close to the interface.

Probing Cytoskeletal Structures by Coupling Optical Superresolution and AFM Techniques for a Correlative Approach

PubMed Central

Chacko, Jenu Varghese; Zanacchi, Francesca Cella; Diaspro, Alberto

2013-01-01

In this article, we describe and show the application of some of the most advanced fluorescence superresolution techniques, STED AFM and STORM AFM microscopy towards imaging of cytoskeletal structures, such as microtubule filaments. Mechanical and structural properties can play a relevant role in the investigation of cytoskeletal structures of interest, such as microtubules, that provide support to the cell structure. In fact, the mechanical properties, such as the local stiffness and the elasticity, can be investigated by AFM force spectroscopy with tens of nanometers resolution. Force curves can be analyzed in order to obtain the local elasticity (and the Young's modulus calculation by fitting the force curves from every pixel of interest), and the combination with STED/STORM microscopy integrates the measurement with high specificity and yields superresolution structural information. This hybrid modality of superresolution-AFM working is a clear example of correlative multimodal microscopy. PMID:24027190

Evaluation of the electrical contact area in contact-mode scanning probe microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Celano, Umberto, E-mail: celano@imec.be, E-mail: u.celano@gmail.com; Chintala, Ravi Chandra; Vandervorst, Wilfried

The tunneling current through an atomic force microscopy (AFM) tip is used to evaluate the effective electrical contact area, which exists between tip and sample in contact-AFM electrical measurements. A simple procedure for the evaluation of the effective electrical contact area is described using conductive atomic force microscopy (C-AFM) in combination with a thin dielectric. We characterize the electrical contact area for coated metal and doped-diamond tips operated at low force (<200 nN) in contact mode. In both cases, we observe that only a small fraction (<10 nm{sup 2}) of the physical contact (∼100 nm{sup 2}) is effectively contributing to the transportmore » phenomena. Assuming this reduced area is confined to the central area of the physical contact, these results explain the sub-10 nm electrical resolution observed in C-AFM measurements.« less

Silicon technology-based micro-systems for atomic force microscopy/photon scanning tunnelling microscopy.

PubMed

Gall-Borrut, P; Belier, B; Falgayrettes, P; Castagne, M; Bergaud, C; Temple-Boyer, P

2001-04-01

We developed silicon nitride cantilevers integrating a probe tip and a wave guide that is prolonged on the silicon holder with one or two guides. A micro-system is bonded to a photodetector. The resulting hybrid system enables us to obtain simultaneously topographic and optical near-field images. Examples of images obtained on a longitudinal cross-section of an optical fibre are shown.

Preface to Special Topic: Piezoresponse Force Microscopy

DOE PAGES

Balke, Nina; Bassiri-Gharb, Nazanin; Lichtensteiger, Céline

2015-08-19

Almost two decades beyond the inception of piezoresponse force microscopy (PFM) and the seminal papers by G€uthner and Dransfeld1 and Gruverman et al., the technique has become the prevailing approach for nanoscale functional characterization of polar materials and has been extended to the probing of other electromechanical effects through the advent of electrochemical strain microscopy (ESM). This focus issue celebrates some of the recent advances in the field and offers a wider outlook of polar materials and their overall characterization. In this paper, we cover topics that include discussions of the properties of traditional ferroelectrics, such as lead zirconate titanatemore » (PZT) and lithium niobate, relaxorferroelectrics, as well as more “exotic” ferroelectric oxides such as hafnia, ferroelectric biological matter, and multiferroic materials. Technique-oriented contributions include papers on the coupling of PFM with other characterization methods such as x-ray diffraction (XRD) and superconducting quantum interface device (SQUID), in addition to considerations on the open questions on the electromechanical response in biased scanning probe microscopy (SPM) techniques, including the effects of the laser spot placement on the readout cantilever displacement, the influence of the tip on the creation of the domain shapes, and the impact of ionic and electronic dynamics on the observed nanoscale hysteretic phenomena.« less

High indium content homogenous InAlN layers grown by plasma-assisted molecular beam epitaxy

NASA Astrophysics Data System (ADS)

Kyle, Erin C. H.; Kaun, Stephen W.; Wu, Feng; Bonef, Bastien; Speck, James S.

2016-11-01

InAlN grown by plasma-assisted molecular beam epitaxy often contains a honeycomb microstructure. The honeycomb microstructure consists of 5-10 nm diameter aluminum-rich regions which are surrounded by indium-rich regions. Layers without this microstructure were previously developed for nominally lattice-matched InAlN and have been developed here for higher indium content InAlN. In this study, InAlN was grown in a nitrogen-rich environment with high indium to aluminum flux ratios at low growth temperatures. Samples were characterized by high-resolution x-ray diffraction, atomic force microscopy, high-angle annular dark-field scanning transmission electron microscopy, and atom probe tomography. Atomic force microscopy showed InAlN layers grown at temperatures below 450 °C under nitrogen-rich conditions were free of droplets. InAlN films with indium contents up to 81% were grown at temperatures between 410 and 440 °C. High-angle annular dark-field scanning transmission electron microscopy and atom probe tomography showed no evidence of honeycomb microstructure for samples with indium contents of 34% and 62%. These layers are homogeneous and follow a random alloy distribution. A growth diagram for InAlN of all indium contents is reported.

Development of Tuning Fork Based Probes for Atomic Force Microscopy

NASA Astrophysics Data System (ADS)

Jalilian, Romaneh; Yazdanpanah, Mehdi M.; Torrez, Neil; Alizadeh, Amirali; Askari, Davood

2014-03-01

This article reports on the development of tuning fork-based AFM/STM probes in NaugaNeedles LLC for use in atomic force microscopy. These probes can be mounted on different carriers per customers' request. (e.g., RHK carrier, Omicron carrier, and tuning fork on a Sapphire disk). We are able to design and engineer tuning forks on any type of carrier used in the market. We can attach three types of tips on the edge of a tuning fork prong (i.e., growing Ag2Ga nanoneedles at any arbitrary angle, cantilever of AFM tip, and tungsten wire) with lengths from 100-500 μm. The nanoneedle is located vertical to the fork. Using a suitable insulation and metallic coating, we can make QPlus sensors that can detect tunneling current during the AFM scan. To make Qplus sensors, the entire quartz fork will be coated with an insulating material, before attaching the nanoneedle. Then, the top edge of one prong is coated with a thin layer of conductive metal and the nanoneedle is attached to the fork end of the metal coated prong. The metal coating provides electrical connection to the tip for tunneling current readout and to the electrodes and used to read the QPlus current. Since the amount of mass added to the fork is minimal, the resonance frequency spectrum does not change and still remains around 32.6 KHz and the Q factor is around 1,200 in ambient condition. These probes can enhance the performance of tuning fork based atomic microscopy.

Protein crystals as scanned probes for recognition atomic force microscopy.

PubMed

Wickremasinghe, Nissanka S; Hafner, Jason H

2005-12-01

Lysozyme crystal growth has been localized at the tip of a conventional silicon nitride cantilever through seeded nucleation. After cross-linking with glutaraldehyde, lysozyme protein crystal tips image gold nanoparticles and grating standards with a resolution comparable to that of conventional tips. Force spectra between the lysozyme crystal tips and surfaces covered with antilysozyme reveal an adhesion force that drops significantly upon blocking with free lysozyme, thus confirming that lysozyme crystal tips can detect molecular recognition interactions.

Scanning hall probe microscopy (SHPM) using quartz crystal AFM feedback.

PubMed

Dede, M; Urkmen, K; Girişen, O; Atabak, M; Oral, A; Farrer, I; Ritchie, D

2008-02-01

Scanning Hall Probe Microscopy (SHPM) is a quantitative and non-invasive technique for imaging localized surface magnetic field fluctuations such as ferromagnetic domains with high spatial and magnetic field resolution of approximately 50 nm and 7 mG/Hz(1/2) at room temperature. In the SHPM technique, scanning tunneling microscope (STM) or atomic force microscope (AFM) feedback is used to keep the Hall sensor in close proximity of the sample surface. However, STM tracking SHPM requires conductive samples; therefore the insulating substrates have to be coated with a thin layer of gold. This constraint can be eliminated with the AFM feedback using sophisticated Hall probes that are integrated with AFM cantilevers. However it is very difficult to micro fabricate these sensors. In this work, we have eliminated the difficulty in the cantilever-Hall probe integration process, just by gluing a Hall Probe chip to a quartz crystal tuning fork force sensor. The Hall sensor chip is simply glued at the end of a 32.768 kHz or 100 kHz Quartz crystal, which is used as force sensor. An LT-SHPM system is used to scan the samples. The sensor assembly is dithered at the resonance frequency using a digital Phase Locked Loop circuit and frequency shifts are used for AFM tracking. SHPM electronics is modified to detect AFM topography and the frequency shift, along with the magnetic field image. Magnetic domains and topography of an Iron Garnet thin film crystal, NdFeB demagnetised magnet and hard disk samples are presented at room temperature. The performance is found to be comparable with the SHPM using STM feedback.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Alexeev, A. V.; Maltseva, D. V.; Ivanov, V. A., E-mail: ivanov@polly.phys.msu.ru

We study force-extension curves of a single semiflexible chain consisting of several rigid rods connected by flexible spacers. The atomic force microscopy and laser optical or magnetic tweezers apparatus stretching these rod-coil macromolecules are discussed. In addition, the stretching by external isotropic force is analyzed. The main attention is focused on computer simulation and analytical results. We demonstrate that the force-extension curves for rod-coil chains composed of two or three rods of equal length differ not only quantitatively but also qualitatively in different probe methods. These curves have an anomalous shape for a chain of two rods. End-to-end distributions ofmore » rod-coil chains are calculated by Monte Carlo method and compared with analytical equations. The influence of the spacer’s length on the force-extension curves in different probe methods is analyzed. The results can be useful for interpreting experiments on the stretching of rod-coil block-copolymers.« less

Force-detected nuclear magnetic resonance: recent advances and future challenges.

PubMed

Poggio, M; Degen, C L

2010-08-27

We review recent efforts to detect small numbers of nuclear spins using magnetic resonance force microscopy. Magnetic resonance force microscopy (MRFM) is a scanning probe technique that relies on the mechanical measurement of the weak magnetic force between a microscopic magnet and the magnetic moments in a sample. Spurred by the recent progress in fabricating ultrasensitive force detectors, MRFM has rapidly improved its capability over the last decade. Today it boasts a spin sensitivity that surpasses conventional, inductive nuclear magnetic resonance detectors by about eight orders of magnitude. In this review we touch on the origins of this technique and focus on its recent application to nanoscale nuclear spin ensembles, in particular on the imaging of nanoscale objects with a three-dimensional (3D) spatial resolution better than 10 nm. We consider the experimental advances driving this work and highlight the underlying physical principles and limitations of the method. Finally, we discuss the challenges that must be met in order to advance the technique towards single nuclear spin sensitivity-and perhaps-to 3D microscopy of molecules with atomic resolution.

Localization and force analysis at the single virus particle level using atomic force microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Chih-Hao; Horng, Jim-Tong; Chang, Jeng-Shian

2012-01-06

Highlights: Black-Right-Pointing-Pointer Localization of single virus particle. Black-Right-Pointing-Pointer Force measurements. Black-Right-Pointing-Pointer Force mapping. -- Abstract: Atomic force microscopy (AFM) is a vital instrument in nanobiotechnology. In this study, we developed a method that enables AFM to simultaneously measure specific unbinding force and map the viral glycoprotein at the single virus particle level. The average diameter of virus particles from AFM images and the specificity between the viral surface antigen and antibody probe were integrated to design a three-stage method that sets the measuring area to a single virus particle before obtaining the force measurements, where the influenza virus was usedmore » as the object of measurements. Based on the purposed method and performed analysis, several findings can be derived from the results. The mean unbinding force of a single virus particle can be quantified, and no significant difference exists in this value among virus particles. Furthermore, the repeatability of the proposed method is demonstrated. The force mapping images reveal that the distributions of surface viral antigens recognized by antibody probe were dispersed on the whole surface of individual virus particles under the proposed method and experimental criteria; meanwhile, the binding probabilities are similar among particles. This approach can be easily applied to most AFM systems without specific components or configurations. These results help understand the force-based analysis at the single virus particle level, and therefore, can reinforce the capability of AFM to investigate a specific type of viral surface protein and its distributions.« less

High resolution subsurface imaging using resonance-enhanced detection in 2nd-harmonic KPFM.

PubMed

Cadena, Maria Jose; Reifenberger, Ronald G; Raman, Arvind

2018-06-28

Second harmonic Kelvin probe force microscopy is a robust mechanism for subsurface imaging at the nanoscale. Here we exploit resonance-enhanced detection as a way to boost the subsurface contrast with higher force sensitivity using lower bias voltages, in comparison to the traditional off-resonance case. In this mode, the second harmonic signal of the electrostatic force is acquired at one of the eigenmode frequencies of the microcantilever. As a result, high-resolution subsurface images are obtained in a variety of nanocomposites. To further understand the subsurface imaging detection upon electrostatic forces, we use a finite element model that approximates the geometry of the probe and sample. This allows the investigation of the contrast mechanism, the depth sensitivity and lateral resolution depending on tip-sample properties. © 2018 IOP Publishing Ltd.

Silver nanowires for highly reproducible cantilever based AFM-TERS microscopy: towards a universal TERS probe.

PubMed

Walke, Peter; Fujita, Yasuhiko; Peeters, Wannes; Toyouchi, Shuichi; Frederickx, Wout; De Feyter, Steven; Uji-I, Hiroshi

2018-04-26

Tip-enhanced Raman scattering (TERS) microscopy is a unique analytical tool to provide complementary chemical and topographic information of surfaces with nanometric resolution. However, difficulties in reliably producing the necessary metallized scanning probe tips has limited its widespread utilisation, particularly in the case of cantilever-based atomic force microscopy. Attempts to alleviate tip related issues using colloidal or bottom-up engineered tips have so far not reported consistent probes for both Raman and topographic imaging. Here we demonstrate the reproducible fabrication of cantilever-based high-performance TERS probes for both topographic and Raman measurements, based on an approach that utilises noble metal nanowires as the active TERS probe. The tips show 10 times higher TERS contrasts than the most typically used electrochemically-etched tips, and show a reproducibility for TERS greater than 90%, far greater than found with standard methods. We show that TERS can be performed in tapping as well as contact AFM mode, with optical resolutions around or below 15 nm, and with a maximum resolution achieved in tapping-mode of 6 nm. Our work illustrates that superior TERS probes can be produced in a fast and cost-effective manner using simple wet-chemistry methods, leading to reliable and reproducible high-resolution and high-sensitivity TERS, and thus renders the technique applicable for a broad community.

Controlled manipulation of oxygen vacancies using nanoscale flexoelectricity

DOE Office of Scientific and Technical Information (OSTI.GOV)

Das, Saikat; Wang, Bo; Cao, Ye

Oxygen vacancies, especially their distribution, are directly coupled to the electromagnetic properties of oxides and related emergent functionalities that have implications for device applications. Here using a homoepitaxial strontium titanate thin film, we demonstrate a controlled manipulation of the oxygen vacancy distribution using the mechanical force from a scanning probe microscope tip. By combining Kelvin probe force microscopy imaging and phase-field simulations, we show that oxygen vacancies can move under a stress-gradient-induced depolarisation field. When tailored, this nanoscale flexoelectric effect enables a controlled spatial modulation. In motion, the scanning probe tip thereby deterministically reconfigures the spatial distribution of vacancies. Finally,more » the ability to locally manipulate oxygen vacancies on-demand provides a tool for the exploration of mesoscale quantum phenomena and engineering multifunctional oxide devices.« less

Design and Optimization of Nanomaterials for Sensing Applications

NASA Astrophysics Data System (ADS)

Sanderson, Robert Noboru

Nanomaterials, materials with one or more of their dimensions on the nanoscale, have emerged as an important field in the development of next-generation sensing systems. Their high surface-to-volume ratio makes them useful for sensing, but also makes them sensitive to processing defects and inherent material defects. To develop and optimize these systems, it is thus necessary to characterize these defects to understand their origin and how to work around them. Scanning probe microscopy (SPM) techniques like atomic force microscopy (AFM) and scanning tunneling microscopy (STM) are important characterization methods which can measure nanoscale topography and electronic structure. These methods are appealing in nanomaterial systems because they are non-damaging and provide local, high-resolution data, and so are capable of detecting nanoscale features such as single defect sites. There are difficulties, however, in the interpretation of SPM data. For instance, AFM-based methods are prone to experimental artifacts due to long-range interactions, such as capacitive crosstalk in Kelvin probe force microscopy (KPFM), and artifacts due to the finite size of the probe tip, such as incorrect surface tracking at steep topographical features. Mechanical characterization (via force spectroscopy) of nanomaterials with significant nanoscale variations, such as tethered lipid bilayer membranes (tLBMs), is also difficult since variations in the bulk system's mechanical behavior must be distinguished from local fluctuations. Additionally, interpretation of STM data is non-trivial due to local variations in electron density in addition to topographical variations. In this thesis we overcome some limitations of SPM methods by supplementing them with additional surface analytical methods as well as computational methods, and we characterize several nanomaterial systems. Current-carrying vapor-liquid-solid Si nanowires (useful for interdigitated-electrode-based sensors) are characterized using finite-element-method (FEM)-supplemented KPFM to retrieve useful information about processing defects, contact resistance, and the primary charge carriers. Next, a tLBM system's stiffness and the stiffness' dependence on tethering molecule concentration is measured using statistical analysis of thousands of AFM force spectra, demonstrating a biosensor-compatible system with a controllable bulk rigidity. Finally, we utilize surface analytical techniques to inform the development of a novel three-dimensional graphene system for sensing applications.

Effect of molecular asymmetry on the charge transport physics of high mobility n-type molecular semiconductors investigated by scanning Kelvin probe microscopy.

PubMed

Hu, Yuanyuan; Berdunov, Nikolai; Di, Chong-an; Nandhakumar, Iris; Zhang, Fengjiao; Gao, Xike; Zhu, Daoben; Sirringhaus, Henning

2014-07-22

We have investigated the influence of the symmetry of the side chain substituents in high-mobility, solution processable n-type molecular semiconductors on the performance of organic field-effect transistors (OFETs). We compare two molecules with the same conjugated core, but either symmetric or asymmetric side chain substituents, and investigate the transport properties and thin film growth mode using scanning Kelvin probe microscopy (SKPM) and atomic force microscopy (AFM). We find that asymmetric side chains can induce a favorable two-dimensional growth mode with a bilayer structure, which enables ultrathin films with a single bilayer to exhibit excellent transport properties, while the symmetric molecules adopt an unfavorable three-dimensional growth mode in which transport in the first monolayer at the interface is severely hindered by high-resistance grain boundaries.

Characterizing Surfaces of the Wide Bandgap Semiconductor Ilmenite with Scanning Probe Microcopies

NASA Technical Reports Server (NTRS)

Wilkins, R.; Powell, Kirk St. A.

1997-01-01

Ilmenite (FeTiO3) is a wide bandgap semiconductor with an energy gap of about 2.5eV. Initial radiation studies indicate that ilmenite has properties suited for radiation tolerant applications, as well as a variety of other electronic applications. Two scanning probe microscopy methods have been used to characterize the surface of samples taken from Czochralski grown single crystals. The two methods, atomic force microscopy (AFM) and scanning tunneling microscopy (STM), are based on different physical principles and therefore provide different information about the samples. AFM provides a direct, three-dimensional image of the surface of the samples, while STM give a convolution of topographic and electronic properties of the surface. We will discuss the differences between the methods and present preliminary data of each method for ilmenite samples.

Materials and Manufacturing Technology Directorate Thermal Sciences and Materials Branch (Overview)

DTIC Science & Technology

2010-09-01

Molecular Mechanics for thermo-mechanical response Materials Characterization • CNT modified durable thermal interface ( DTI ) • MEMS-based RTD micro...stabilization. Surface Characterization by Atomic Force Microscopy: Probing Thermal, Electrical, and Mechanical Properties Heater Current Path Anchor Leg 50 µm

Nanometer-scale surface potential and resistance mapping of wide-bandgap Cu(In,Ga)Se2 thin films

NASA Astrophysics Data System (ADS)

Jiang, C.-S.; Contreras, M. A.; Mansfield, L. M.; Moutinho, H. R.; Egaas, B.; Ramanathan, K.; Al-Jassim, M. M.

2015-01-01

We report microscopic characterization studies of wide-bandgap Cu(In,Ga)Se2 photovoltaic thin films using the nano-electrical probes of scanning Kelvin probe force microscopy and scanning spreading resistance microscopy. With increasing bandgap, the potential imaging shows significant increases in both the large potential features due to extended defects or defect aggregations and the potential fluctuation due to unresolvable point defects with single or a few charges. The resistance imaging shows increases in both overall resistance and resistance nonuniformity due to defects in the subsurface region. These defects are expected to affect open-circuit voltage after the surfaces are turned to junction upon device completion.

High Performance Nuclear Magnetic Resonance Imaging Using Magnetic Resonance Force Microscopy

DTIC Science & Technology

2013-12-12

Micron- Size Ferromagnet . Physical Review Letters, 92(3) 037205 (2004) [22] A. Z. Genack and A. G. Redeld. Theory of nuclear spin diusion in a...perform spatially resolved scanned probe studies of spin dynamics in nanoscale ensembles of few electron spins of varying size . Our research culminated...perform spatially resolved scanned probe studies of spin dynamics in nanoscale ensembles of few electron spins of varying size . Our research culminated

DOE Office of Scientific and Technical Information (OSTI.GOV)

Göring, Gerald; Dietrich, Philipp-Immanuel; Blaicher, Matthias

3D direct laser writing based on two-photon polymerization is considered as a tool to fabricate tailored probes for atomic force microscopy. Tips with radii of 25 nm and arbitrary shape are attached to conventionally shaped micro-machined cantilevers. Long-term scanning measurements reveal low wear rates and demonstrate the reliability of such tips. Furthermore, we show that the resonance spectrum of the probe can be tuned for multi-frequency applications by adding rebar structures to the cantilever.

Systems and methods for laser assisted sample transfer to solution for chemical analysis

DOEpatents

Van Berkel, Gary J.; Kertesz, Vilmos; Ovchinnikova, Olga S.

2014-06-03

Systems and methods are described for laser ablation of an analyte from a specimen and capturing of the analyte in a dispensed solvent to form a testing solution. A solvent dispensing and extraction system can form a liquid microjunction with the specimen. The solvent dispensing and extraction system can include a surface sampling probe. The laser beam can be directed through the surface sampling probe. The surface sampling probe can also serve as an atomic force microscopy probe. The surface sampling probe can form a seal with the specimen. The testing solution including the analyte can then be analyzed using an analytical instrument or undergo further processing.

Systems and methods for laser assisted sample transfer to solution for chemical analysis

DOEpatents

Van Berkel, Gary J.; Kertesz, Vilmos; Ovchinnikova, Olga S.

2015-09-29

Systems and methods are described for laser ablation of an analyte from a specimen and capturing of the analyte in a dispensed solvent to form a testing solution. A solvent dispensing and extraction system can form a liquid microjunction with the specimen. The solvent dispensing and extraction system can include a surface sampling probe. The laser beam can be directed through the surface sampling probe. The surface sampling probe can also serve as an atomic force microscopy probe. The surface sampling probe can form a seal with the specimen. The testing solution including the analyte can then be analyzed using an analytical instrument or undergo further processing.

Systems and methods for laser assisted sample transfer to solution for chemical analysis

DOEpatents

Van Berkel, Gary J; Kertesz, Vilmos; Ovchinnikova, Olga S

2013-08-27

Systems and methods are described for laser ablation of an analyte from a specimen and capturing of the analyte in a dispensed solvent to form a testing solution. A solvent dispensing and extraction system can form a liquid microjunction with the specimen. The solvent dispensing and extraction system can include a surface sampling probe. The laser beam can be directed through the surface sampling probe. The surface sampling probe can also serve as an atomic force microscopy probe. The surface sampling probe can form a seal with the specimen. The testing solution including the analyte can then be analyzed using an analytical instrument or undergo further processing.

Atomic force microscopy of red-light photoreceptors using peakforce quantitative nanomechanical property mapping.

PubMed

Kroeger, Marie E; Sorenson, Blaire A; Thomas, J Santoro; Stojković, Emina A; Tsonchev, Stefan; Nicholson, Kenneth T

2014-10-24

Atomic force microscopy (AFM) uses a pyramidal tip attached to a cantilever to probe the force response of a surface. The deflections of the tip can be measured to ~10 pN by a laser and sectored detector, which can be converted to image topography. Amplitude modulation or "tapping mode" AFM involves the probe making intermittent contact with the surface while oscillating at its resonant frequency to produce an image. Used in conjunction with a fluid cell, tapping-mode AFM enables the imaging of biological macromolecules such as proteins in physiologically relevant conditions. Tapping-mode AFM requires manual tuning of the probe and frequent adjustments of a multitude of scanning parameters which can be challenging for inexperienced users. To obtain high-quality images, these adjustments are the most time consuming. PeakForce Quantitative Nanomechanical Property Mapping (PF-QNM) produces an image by measuring a force response curve for every point of contact with the sample. With ScanAsyst software, PF-QNM can be automated. This software adjusts the set-point, drive frequency, scan rate, gains, and other important scanning parameters automatically for a given sample. Not only does this process protect both fragile probes and samples, it significantly reduces the time required to obtain high resolution images. PF-QNM is compatible for AFM imaging in fluid; therefore, it has extensive application for imaging biologically relevant materials. The method presented in this paper describes the application of PF-QNM to obtain images of a bacterial red-light photoreceptor, RpBphP3 (P3), from photosynthetic R. palustris in its light-adapted state. Using this method, individual protein dimers of P3 and aggregates of dimers have been observed on a mica surface in the presence of an imaging buffer. With appropriate adjustments to surface and/or solution concentration, this method may be generally applied to other biologically relevant macromolecules and soft materials.

Simultaneous Scanning Ion Conductance Microscopy and Atomic Force Microscopy with Microchanneled Cantilevers

NASA Astrophysics Data System (ADS)

Ossola, Dario; Dorwling-Carter, Livie; Dermutz, Harald; Behr, Pascal; Vörös, János; Zambelli, Tomaso

2015-12-01

We combined scanning ion conductance microscopy (SICM) and atomic force microscopy (AFM) into a single tool using AFM cantilevers with an embedded microchannel flowing into the nanosized aperture at the apex of the hollow pyramid. An electrode was positioned in the AFM fluidic circuit connected to a second electrode in the bath. We could thus simultaneously measure the ionic current and the cantilever bending (in optical beam deflection mode). First, we quantitatively compared the SICM and AFM contact points on the approach curves. Second, we estimated where the probe in SICM mode touches the sample during scanning on a calibration grid and applied the finding to image a network of neurites on a Petri dish. Finally, we assessed the feasibility of a double controller using both the ionic current and the deflection as input signals of the piezofeedback. The experimental data were rationalized in the framework of finite elements simulations.

The study on the nanomachining property and cutting model of single-crystal sapphire by atomic force microscopy.

PubMed

Huang, Jen-Ching; Weng, Yung-Jin

2014-01-01

This study focused on the nanomachining property and cutting model of single-crystal sapphire during nanomachining. The coated diamond probe is used to as a tool, and the atomic force microscopy (AFM) is as an experimental platform for nanomachining. To understand the effect of normal force on single-crystal sapphire machining, this study tested nano-line machining and nano-rectangular pattern machining at different normal force. In nano-line machining test, the experimental results showed that the normal force increased, the groove depth from nano-line machining also increased. And the trend is logarithmic type. In nano-rectangular pattern machining test, it is found when the normal force increases, the groove depth also increased, but rather the accumulation of small chips. This paper combined the blew by air blower, the cleaning by ultrasonic cleaning machine and using contact mode probe to scan the surface topology after nanomaching, and proposed the "criterion of nanomachining cutting model," in order to determine the cutting model of single-crystal sapphire in the nanomachining is ductile regime cutting model or brittle regime cutting model. After analysis, the single-crystal sapphire substrate is processed in small normal force during nano-linear machining; its cutting modes are ductile regime cutting model. In the nano-rectangular pattern machining, due to the impact of machined zones overlap, the cutting mode is converted into a brittle regime cutting model. © 2014 Wiley Periodicals, Inc.

Determination of ferroelectric contributions to electromechanical response by frequency dependent piezoresponse force microscopy.

PubMed

Seol, Daehee; Park, Seongjae; Varenyk, Olexandr V; Lee, Shinbuhm; Lee, Ho Nyung; Morozovska, Anna N; Kim, Yunseok

2016-07-28

Hysteresis loop analysis via piezoresponse force microscopy (PFM) is typically performed to probe the existence of ferroelectricity at the nanoscale. However, such an approach is rather complex in accurately determining the pure contribution of ferroelectricity to the PFM. Here, we suggest a facile method to discriminate the ferroelectric effect from the electromechanical (EM) response through the use of frequency dependent ac amplitude sweep with combination of hysteresis loops in PFM. Our combined study through experimental and theoretical approaches verifies that this method can be used as a new tool to differentiate the ferroelectric effect from the other factors that contribute to the EM response.

Spatially resolved quantitative mapping of thermomechanical properties and phase transition temperatures using scanning probe microscopy

DOEpatents

Jesse, Stephen; Kalinin, Sergei V; Nikiforov, Maxim P

2013-07-09

An approach for the thermomechanical characterization of phase transitions in polymeric materials (polyethyleneterephthalate) by band excitation acoustic force microscopy is developed. This methodology allows the independent measurement of resonance frequency, Q factor, and oscillation amplitude of a tip-surface contact area as a function of tip temperature, from which the thermal evolution of tip-surface spring constant and mechanical dissipation can be extracted. A heating protocol maintained a constant tip-surface contact area and constant contact force, thereby allowing for reproducible measurements and quantitative extraction of material properties including temperature dependence of indentation-based elastic and loss moduli.

Determination of ferroelectric contributions to electromechanical response by frequency dependent piezoresponse force microscopy

PubMed Central

Seol, Daehee; Park, Seongjae; Varenyk, Olexandr V.; Lee, Shinbuhm; Lee, Ho Nyung; Morozovska, Anna N.; Kim, Yunseok

2016-01-01

Hysteresis loop analysis via piezoresponse force microscopy (PFM) is typically performed to probe the existence of ferroelectricity at the nanoscale. However, such an approach is rather complex in accurately determining the pure contribution of ferroelectricity to the PFM. Here, we suggest a facile method to discriminate the ferroelectric effect from the electromechanical (EM) response through the use of frequency dependent ac amplitude sweep with combination of hysteresis loops in PFM. Our combined study through experimental and theoretical approaches verifies that this method can be used as a new tool to differentiate the ferroelectric effect from the other factors that contribute to the EM response. PMID:27466086

Surface passivation of (100) GaSb using self-assembled monolayers of long-chain octadecanethiol

DOE Office of Scientific and Technical Information (OSTI.GOV)

Papis-Polakowska, E., E-mail: papis@ite.waw.pl; Kaniewski, J.; Jurenczyk, J.

2016-05-15

The passivation of (100) GaSb surface was investigated by means of the long-chain octadecanethiol (ODT) self-assembled monolayer (SAM). The properties of ODT SAM on (100) GaSb were characterized by the atomic force microscopy using Kelvin probe force microscopy mode and X-ray photoelectron spectroscopy. The chemical treatment of 10 mM ODT-C{sub 2}H{sub 5}OH has been applied to the passivation of a type-II superlattice InAs/GaSb photodetector. The electrical measurements indicate that the current density was reduced by one order of magnitude as compared to an unpassivated photodetector.

View of the bacterial strains of Escherichia coli M-17 and its interaction with the nanoparticles of zinc oxide by means of atomic force microscopy

NASA Astrophysics Data System (ADS)

Sagitova, A.; Yaminsky, I.; Meshkov, G.

2016-08-01

Visualization of the structure of biological objects plays a key role in medicine, biotechnology, nanotechnology and IT-technology. Atomic force microscopy (AFM) is a promising method of studying of objects’ morphology and structure. In this work, AFM was used to determine the size and shape of the bacterial strains of Escherichia coli M-17 and visualization its interaction with the nanoparticles of zinc oxide. The suspension of E.coli bacteria was applied to natural mica and studied by contact mode using the FemtoScan multifunctional scanning probe microscope.

Atomic force microscopy of starch systems.

PubMed

Zhu, Fan

2017-09-22

Atomic force microscopy (AFM) generates information on topography, adhesion, and elasticity of sample surface by touching with a tip. Under suitable experimental settings, AFM can image biopolymers of few nanometers. Starch is a major food and industrial component. AFM has been used to probe the morphology, properties, modifications, and interactions of starches from diverse botanical origins at both micro- and nano-structural levels. The structural information obtained by AFM supports the blocklet structure of the granules, and provides qualitative and quantitative basis for some physicochemical properties of diverse starch systems. It becomes evident that AFM can complement other microscopic techniques to provide novel structural insights for starch systems.

A versatile variable field module for Asylum Cypher scanning probe system

NASA Astrophysics Data System (ADS)

Liu, Hongxue; Comes, Ryan; Lu, Jiwei; Wolf, Stuart; Hodgson, Jim; Rutgers, Maarten

2013-03-01

Atomic force microscopy (AFM) has become one of the most widely used techniques for measuring and manipulating various characteristics of materials at the nanoscale. However, there are very limited option for the characterization of field dependence properties. In this work, we demonstrate a versatile variable field module (VFM) with magnetic field up to 1800 Oe for the Asylum Research Cypher system. The magnetic field is changed by adjusting the distance between a rare earth magnet and the AFM probe. A built-in Hall sensor makes it possible to perform in-situ measurements of the field. Rotating the magnet makes it possible to do angular field dependent measurements. The capability of the VFM system is demonstrated by degaussing a floppy disk media with increasing magnetic field. The written bits are erased at about 800 Oe. Angular dependence measurements clearly show the evolution of magnetic domain structures. A completely reversible magnetic force microscopy (MFM) phase contrast is observed when the magnetic field is rotated by 180°. Further demonstration of successful magnetic switching of CoFe2O4 pillars in CoFe2O4-BiFeO3 nanocomposites will be presented and field dependent MFM and piezoresponse force microscopy (PFM) will be discussed. The work at University of Virginia was supported by DARPA under contract no. HR-0011-10-1-0072.

Frequency shift, damping, and tunneling current coupling with quartz tuning forks in noncontact atomic force microscopy

NASA Astrophysics Data System (ADS)

Nony, Laurent; Bocquet, Franck; Para, Franck; Loppacher, Christian

2016-09-01

A combined experimental and theoretical approach to the coupling between frequency-shift (Δ f ) , damping, and tunneling current (It) in combined noncontact atomic force microscopy/scanning tunneling microscopy using quartz tuning forks (QTF)-based probes is reported. When brought into oscillating tunneling conditions, the tip located at the QTF prong's end radiates an electromagnetic field which couples to the QTF prong motion via its piezoelectric tensor and loads its electrodes by induction. Our approach explains how those It-related effects ultimately modify the Δ f and the damping measurements. This paradigm to the origin of the coupling between It and the nc-AFM regular signals relies on both the intrinsic piezoelectric nature of the quartz constituting the QTF and its electrodes design.

Electrical properties of films of zinc oxide nanoparticles and its hybrid with reduced graphene oxide

DOE Office of Scientific and Technical Information (OSTI.GOV)

Madhuri, K. Priya; Bramhaiah, K.; John, Neena S., E-mail: jsneena@cnsms.res.in

Free-standing films of ZnO nanoparticles (NPs) and reduced graphene oxide (rGO)-ZnO NPs hybrid are prepared at a liquid/liquid interface. The films are characterized by UV-visible spectroscopy, X-ray diffraction, scanning electron microscopy and atomic force microscopy. ZnO film consists of spherical aggregated NPs while the hybrid film contains folded sheets of rGO with embedded ZnO NPs. Electrical properties of the films and its photoresponse in presence of UV radiation are investigated using current sensing atomic force microscopy (CSAFM) at nanoscale and bulk measurements using two probe methods. Enhancement in photocurrent is observed in both cases and the current imaging reveals anmore » inhomogeneous contribution by different ZnO grains in the film.« less

Towards High-Resolution Tissue Imaging Using Nanospray Desorption Electrospray Ionization Mass Spectrometry Coupled to Shear Force Microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nguyen, Son N.; Sontag, Ryan L.; Carson, James P.

Constant mode ambient mass spectrometry imaging (MSI) of tissue sections with high lateral resolution of better than 10 µm was performed by combining shear force microscopy with nanospray desorption electrospray ionization (nano-DESI). Shear force microscopy enabled precise control of the distance between the sample and nano-DESI probe during MSI experiments and provided information on sample topography. Proof-of-concept experiments were performed using lung and brain tissue sections representing spongy and dense tissues, respectively. Topography images obtained using shear force microscopy were comparable to the results obtained using contact profilometry over the same region of the tissue section. Variations in tissue heightmore » were found to be dependent on the tissue type and were in the range of 0-5 µm for lung tissue and 0-3 µm for brain tissue sections. Ion images of phospholipids obtained in this study are in good agreement with literature data. Normalization of nano-DESI MSI images to the signal of the internal standard added to the extraction solvent allowed us to construct high-resolution ion images free of matrix effects.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Miranda, Adelaide; De Beule, Pieter A. A., E-mail: pieter.de-beule@inl.int; Martins, Marco

Combined microscopy techniques offer the life science research community a powerful tool to investigate complex biological systems and their interactions. Here, we present a new combined microscopy platform based on fluorescence optical sectioning microscopy through aperture correlation microscopy with a Differential Spinning Disk (DSD) and nanomechanical mapping with an Atomic Force Microscope (AFM). The illumination scheme of the DSD microscope unit, contrary to standard single or multi-point confocal microscopes, provides a time-independent illumination of the AFM cantilever. This enables a distortion-free simultaneous operation of fluorescence optical sectioning microscopy and atomic force microscopy with standard probes. In this context, we discussmore » sample heating due to AFM cantilever illumination with fluorescence excitation light. Integration of a DSD fluorescence optical sectioning unit with an AFM platform requires mitigation of mechanical noise transfer of the spinning disk. We identify and present two solutions to almost annul this noise in the AFM measurement process. The new combined microscopy platform is applied to the characterization of a DOPC/DOPS (4:1) lipid structures labelled with a lipophilic cationic indocarbocyanine dye deposited on a mica substrate.« less

Conductive paths through polycrystalline BaTiO{sub 3}: Scanning probe microscopy study

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ayvazian, Talin; Bersuker, Gennadi; Lingley, Zachary R.

2016-08-15

The microstructural features determining the leakage current through polycrystalline BaTiO{sub 3} films are investigated using Conductive Atomic Force Microscopy. Grain boundaries are found to be the dominant conductive paths compared to the conduction through the grains. Grain boundary currents are observed to reversibly rise with the increase of the applied DC voltages, indicating that the current is controlled by a field-activated charge transport process.

Atomic force microscopy study of the structure function relationships of the biofilm-forming bacterium Streptococcus mutans

NASA Astrophysics Data System (ADS)

Cross, Sarah E.; Kreth, Jens; Zhu, Lin; Qi, Fengxia; Pelling, Andrew E.; Shi, Wenyuan; Gimzewski, James K.

2006-02-01

Atomic force microscopy (AFM) has garnered much interest in recent years for its ability to probe the structure, function and cellular nanomechanics inherent to specific biological cells. In particular, we have used AFM to probe the important structure-function relationships of the bacterium Streptococcus mutans. S. mutans is the primary aetiological agent in human dental caries (tooth decay), and is of medical importance due to the virulence properties of these cells in biofilm initiation and formation, leading to increased tolerance to antibiotics. We have used AFM to characterize the unique surface structures of distinct mutants of S. mutans. These mutations are located in specific genes that encode surface proteins, thus using AFM we have resolved characteristic surface features for mutant strains compared to the wild type. Ultimately, our characterization of surface morphology has shown distinct differences in the local properties displayed by various S. mutans strains on the nanoscale, which is imperative for understanding the collective properties of these cells in biofilm formation.

Effect of dopant density on contact potential difference across n-type GaAs homojunctions using Kelvin Probe Force Microscopy

NASA Astrophysics Data System (ADS)

Boumenou, C. Kameni; Urgessa, Z. N.; Djiokap, S. R. Tankio; Botha, J. R.; Nel, J.

2018-04-01

In this study, cross-sectional surface potential imaging of n+/semi-insulating GaAs junctions is investigated by using amplitude mode kelvin probe force microscopy. The measurements have shown two different potential profiles, related to the difference in surface potential between the semi-insulating (SI) substrate and the epilayers. It is shown that the contact potential difference (CPD) between the tip and the sample is higher on the semi-insulating substrate side than on the n-type epilayer side. This change in CPD across the interface has been explained by means of energy band diagrams indicating the relative Fermi level positions. In addition, it has also been found that the CPD values across the interface are much smaller than the calculated values (on average about 25% of the theoretical values) and increase with the electron density. Therefore, the results presented in study are only in qualitative agreement with the theory.

Direct observation of the leakage current in epitaxial diamond Schottky barrier devices by conductive-probe atomic force microscopy and Raman imaging

NASA Astrophysics Data System (ADS)

Alvarez, J.; Boutchich, M.; Kleider, J. P.; Teraji, T.; Koide, Y.

2014-09-01

The origin of the high leakage current measured in several vertical-type diamond Schottky devices is conjointly investigated by conducting probe atomic force microscopy and confocal micro-Raman/photoluminescence imaging analysis. Local areas characterized by a strong decrease of the local resistance (5-6 orders of magnitude drop) with respect to their close surrounding have been identified in several different regions of the sample surface. The same local areas, also referenced as electrical hot-spots, reveal a slightly constrained diamond lattice and three dominant Raman bands in the low-wavenumber region (590, 914 and 1040 cm-1). These latter bands are usually assigned to the vibrational modes involving boron impurities and its possible complexes that can electrically act as traps for charge carriers. Local current-voltage measurements performed at the hot-spots point out a trap-filled-limited current as the main conduction mechanism favouring the leakage current in the Schottky devices.

Visualization of Live Cochlear Stereocilia at a Nanoscale Resolution Using Hopping Probe Ion Conductance Microscopy

PubMed Central

Vélez-Ortega, A. Catalina; Frolenkov, Gregory I.

2016-01-01

The mechanosensory apparatus that detects sound-induced vibrations in the cochlea is located on the apex of the auditory sensory hair cells and it is made up of actin-filled projections, called stereocilia. In young rodents, stereocilia bundles of auditory hair cells consist of 3 to 4 rows of stereocilia of decreasing height and varying thickness. Morphological studies of the auditory stereocilia bundles in live hair cells have been challenging because the diameter of each stereocilium is near or below the resolution limit of optical microscopy. In theory, scanning probe microscopy techniques, such as atomic force microscopy, could visualize the surface of a living cell at a nanoscale resolution. However, their implementations for hair cell imaging have been largely unsuccessful because the probe usually damages the bundle and disrupts the bundle cohesiveness during imaging. We overcome these limitations by using hopping probe ion conductance microscopy (HPICM), a non-contact scanning probe technique that is ideally suited for the imaging of live cells with a complex topography. Organ of Corti explants are placed in a physiological solution and then a glass nanopipette –which is connected to a 3D-positioning piezoelectric system and to a patch clamp amplifier– is used to scan the surface of the live hair cells at nanometer resolution without ever touching the cell surface. Here we provide a detailed protocol for the imaging of mouse or rat stereocilia bundles in live auditory hair cells using HPICM. We provide information about the fabrication of the nanopipettes, the calibration of the HPICM setup, the parameters we have optimized for the imaging of live stereocilia bundles and, lastly, a few basic image post-processing manipulations. PMID:27259929

Visualization of Live Cochlear Stereocilia at a Nanoscale Resolution Using Hopping Probe Ion Conductance Microscopy.

PubMed

Vélez-Ortega, A Catalina; Frolenkov, Gregory I

2016-01-01

The mechanosensory apparatus that detects sound-induced vibrations in the cochlea is located on the apex of the auditory sensory hair cells and it is made up of actin-filled projections, called stereocilia. In young rodents, stereocilia bundles of auditory hair cells consist of 3-4 rows of stereocilia of decreasing height and varying thickness. Morphological studies of the auditory stereocilia bundles in live hair cells have been challenging because the diameter of each stereocilium is near or below the resolution limit of optical microscopy. In theory, scanning probe microscopy techniques, such as atomic force microscopy, could visualize the surface of a living cell at a nanoscale resolution. However, their implementations for hair cell imaging have been largely unsuccessful because the probe usually damages the bundle and disrupts the bundle cohesiveness during imaging. We overcome these limitations by using hopping probe ion conductance microscopy (HPICM), a non-contact scanning probe technique that is ideally suited for the imaging of live cells with a complex topography. Organ of Corti explants are placed in a physiological solution and then a glass nanopipette-which is connected to a 3D-positioning piezoelectric system and to a patch clamp amplifier-is used to scan the surface of the live hair cells at nanometer resolution without ever touching the cell surface.Here, we provide a detailed protocol for the imaging of mouse or rat stereocilia bundles in live auditory hair cells using HPICM. We provide information about the fabrication of the nanopipettes, the calibration of the HPICM setup, the parameters we have optimized for the imaging of live stereocilia bundles and, lastly, a few basic image post-processing manipulations.

Proximity effect on hydrodynamic interaction between a sphere and a plane measured by force feedback microscopy at different frequencies

NASA Astrophysics Data System (ADS)

Carpentier, Simon; Rodrigues, Mario S.; Charlaix, Elisabeth; Chevrier, Joël

2015-07-01

In this article, we measure the viscous damping G″, and the associated stiffness G', of a liquid flow in sphere-plane geometry over a large frequency range. In this regime, the lubrication approximation is expected to dominate. We first measure the static force applied to the tip. This is made possible thanks to a force feedback method. Adding a sub-nanometer oscillation of the tip, we obtain the dynamic part of the interaction with solely the knowledge of the lever properties in the experimental context using a linear transformation of the amplitude and phase change. Using a Force Feedback Microscope (FFM), we are then able to measure simultaneously the static force, the stiffness, and the dissipative part of the interaction in a broad frequency range using a single AFM probe. Similar measurements have been performed by the Surface Force Apparatus (SFA) with a probe radius hundred times bigger. In this context, the FFM can be called nano-SFA.

Electric contributions to magnetic force microscopy response from graphene and MoS{sub 2} nanosheets

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Lu Hua, E-mail: luhua.li@deakin.edu.au; Chen, Ying

Magnetic force microscopy (MFM) signals have recently been detected from whole pieces of mechanically exfoliated graphene and molybdenum disulfide (MoS{sub 2}) nanosheets, and magnetism of the two nanomaterials was claimed based on these observations. However, non-magnetic interactions or artefacts are commonly associated with MFM signals, which make the interpretation of MFM signals not straightforward. A systematic investigation has been done to examine possible sources of the MFM signals from graphene and MoS{sub 2} nanosheets and whether the MFM signals can be correlated with magnetism. It is found that the MFM signals have significant non-magnetic contributions due to capacitive and electrostaticmore » interactions between the nanosheets and conductive cantilever tip, as demonstrated by electric force microscopy and scanning Kevin probe microscopy analyses. In addition, the MFM signals of graphene and MoS{sub 2} nanosheets are not responsive to reversed magnetic field of the magnetic cantilever tip. Therefore, the observed MFM response is mainly from electric artefacts and not compelling enough to correlate with magnetism of graphene and MoS{sub 2} nanosheets.« less

Nanoscale simultaneous chemical and mechanical imaging via peak force infrared microscopy

PubMed Central

Wang, Le; Wang, Haomin; Wagner, Martin; Yan, Yong; Jakob, Devon S.; Xu, Xiaoji G.

2017-01-01

Nondestructive chemical and mechanical measurements of materials with ~10-nm spatial resolution together with topography provide rich information on the compositions and organizations of heterogeneous materials and nanoscale objects. However, multimodal nanoscale correlations are difficult to achieve because of the limitation on spatial resolution of optical microscopy and constraints from instrumental complexities. We report a novel noninvasive spectroscopic scanning probe microscopy method—peak force infrared (PFIR) microscopy—that allows chemical imaging, collection of broadband infrared spectra, and mechanical mapping at a spatial resolution of 10 nm. In our technique, chemical absorption information is directly encoded in the withdraw curve of the peak force tapping cycle after illumination with synchronized infrared laser pulses in a simple apparatus. Nanoscale phase separation in block copolymers and inhomogeneity in CH3NH3PbBr3 perovskite crystals are studied with correlative infrared/mechanical nanoimaging. Furthermore, we show that the PFIR method is sensitive to the presence of surface phonon polaritons in boron nitride nanotubes. PFIR microscopy will provide a powerful analytical tool for explorations at the nanoscale across wide disciplines. PMID:28691096

Sensing of silver nanoparticles on/in endothelial cells using atomic force spectroscopy.

PubMed

Kolodziejczyk, Agnieszka; Jakubowska, Aleksandra; Kucinska, Magdalena; Wasiak, Tomasz; Komorowski, Piotr; Makowski, Krzysztof; Walkowiak, Bogdan

2018-05-10

Endothelial cells, due to their location, are interesting objects for atomic force spectroscopy study. They constitute a barrier between blood and vessel tissues located deeper, and therefore they are the first line of contact with various substances present in blood, eg, drugs or nanoparticles. This work intends to verify whether the mechanical response of immortalized human umbilical vein endothelial cells (EA.hy926), when exposed to silver nanoparticles, as measured using force spectroscopy, could be effectively used as a bio-indicator of the physiological state of the cells. Silver nanoparticles were characterized with transmission electron microscopy and dynamic light scattering techniques. Tetrazolium salt reduction test was used to determine cell viability after treatment with silver nanoparticles. An elasticity of native cells was examined in the Hanks' buffer whereas fixed cells were softly fixed with formaldehyde. Additional aspect of the work is the comparative force spectroscopy utilizing AFM probes of ball-shape and conical geometries, in order to understand what changes in cell elasticity, caused by SNPs, were detectable with each probe. As a supplement to elasticity studies, cell morphology observation by atomic force microscopy and detection of silver nanoparticles inside cells using transmission electron microscopy were also performed. Cells exposed to silver nanoparticles at the highest selected concentrations (3.6 μg/mL, 16 μg/mL) are less elastic. It may be associated with the reorganization of the cellular cytoskeleton and the "strengthening" of the cell cortex caused by presence of silver nanoparticles. This observation does not depend on cell fixation. Agglomerates of silver nanoparticles were observed on the cell membrane as well as inside the cells. Copyright © 2018 John Wiley & Sons, Ltd.

Bipolar charge storage characteristics in copper and cobalt co-doped zinc oxide (ZnO) thin film.

PubMed

Kumar, Amit; Herng, Tun Seng; Zeng, Kaiyang; Ding, Jun

2012-10-24

The bipolar charge phenomenon in Cu and Co co-doped zinc oxide (ZnO) film samples has been studied using scanning probe microscopy (SPM) techniques. Those ZnO samples are made using a pulsed laser deposition (PLD) technique. It is found that the addition of Cu and Co dopants suppresses the electron density in ZnO and causes a significant change in the work function (Fermi level) value of the ZnO film; this results in the ohmic nature of the contact between the electrode (probe tip) and codoped sample, whereas this contact exhibits a Schottky nature in the undoped and single-element-doped samples. These results are verified by Kelvin probe force microscopy (KPFM) and ultraviolet photoelectron spectroscopy (UPS) measurements. It is also found that the co-doping (Cu and Co) can stabilize the bipolar charge, whereas Cu doping only stabilizes the positive charge in ZnO thin films.

Systematic validation and atomic force microscopy of non-covalent short oligonucleotide barcode microarrays.

PubMed

Cook, Michael A; Chan, Chi-Kin; Jorgensen, Paul; Ketela, Troy; So, Daniel; Tyers, Mike; Ho, Chi-Yip

2008-02-06

Molecular barcode arrays provide a powerful means to analyze cellular phenotypes in parallel through detection of short (20-60 base) unique sequence tags, or "barcodes", associated with each strain or clone in a collection. However, costs of current methods for microarray construction, whether by in situ oligonucleotide synthesis or ex situ coupling of modified oligonucleotides to the slide surface are often prohibitive to large-scale analyses. Here we demonstrate that unmodified 20mer oligonucleotide probes printed on conventional surfaces show comparable hybridization signals to covalently linked 5'-amino-modified probes. As a test case, we undertook systematic cell size analysis of the budding yeast Saccharomyces cerevisiae genome-wide deletion collection by size separation of the deletion pool followed by determination of strain abundance in size fractions by barcode arrays. We demonstrate that the properties of a 13K unique feature spotted 20 mer oligonucleotide barcode microarray compare favorably with an analogous covalently-linked oligonucleotide array. Further, cell size profiles obtained with the size selection/barcode array approach recapitulate previous cell size measurements of individual deletion strains. Finally, through atomic force microscopy (AFM), we characterize the mechanism of hybridization to unmodified barcode probes on the slide surface. These studies push the lower limit of probe size in genome-scale unmodified oligonucleotide microarray construction and demonstrate a versatile, cost-effective and reliable method for molecular barcode analysis.

Quantitative assessment of intermolecular interactions by atomic force microscopy imaging using copper oxide tips

NASA Astrophysics Data System (ADS)

Mönig, Harry; Amirjalayer, Saeed; Timmer, Alexander; Hu, Zhixin; Liu, Lacheng; Díaz Arado, Oscar; Cnudde, Marvin; Strassert, Cristian Alejandro; Ji, Wei; Rohlfing, Michael; Fuchs, Harald

2018-05-01

Atomic force microscopy is an impressive tool with which to directly resolve the bonding structure of organic compounds1-5. The methodology usually involves chemical passivation of the probe-tip termination by attaching single molecules or atoms such as CO or Xe (refs 1,6-9). However, these probe particles are only weakly connected to the metallic apex, which results in considerable dynamic deflection. This probe particle deflection leads to pronounced image distortions, systematic overestimation of bond lengths, and in some cases even spurious bond-like contrast features, thus inhibiting reliable data interpretation8-12. Recently, an alternative approach to tip passivation has been used in which slightly indenting a tip into oxidized copper substrates and subsequent contrast analysis allows for the verification of an oxygen-terminated Cu tip13-15. Here we show that, due to the covalently bound configuration of the terminal oxygen atom, this copper oxide tip (CuOx tip) has a high structural stability, allowing not only a quantitative determination of individual bond lengths and access to bond order effects, but also reliable intermolecular bond characterization. In particular, by removing the previous limitations of flexible probe particles, we are able to provide conclusive experimental evidence for an unusual intermolecular N-Au-N three-centre bond. Furthermore, we demonstrate that CuOx tips allow the characterization of the strength and configuration of individual hydrogen bonds within a molecular assembly.

Force Spectrum Microscopy Using Mitochondrial Fluctuations of Control and ATP-Depleted Cells.

PubMed

Xu, Wenlong; Alizadeh, Elaheh; Prasad, Ashok

2018-06-19

A single-cell assay of active and passive intracellular mechanical properties of mammalian cells could give significant insight into cellular processes. Force spectrum microscopy (FSM) is one such technique, which combines the spontaneous motion of probe particles and the mechanical properties of the cytoskeleton measured by active microrheology using optical tweezers to determine the force spectrum of the cytoskeleton. A simpler and noninvasive method to perform FSM would be very useful, enabling its widespread adoption. Here, we develop an alternative method of FSM using measurement of the fluctuating motion of mitochondria. Mitochondria of the C3H-10T1/2 cell line were labeled and tracked using confocal microscopy. Mitochondrial probes were selected based on morphological characteristics, and their mean-square displacement, creep compliance, and distributions of directional change were measured. We found that the creep compliance of mitochondria resembles that of particles in viscoelastic media. However, comparisons of creep compliance between controls and cells treated with pharmacological agents showed that perturbations to the actomysoin network had surprisingly small effects on mitochondrial fluctuations, whereas microtubule disruption and ATP depletion led to a significantly decreased creep compliance. We used properties of the distribution of directional change to identify a regime of thermally dominated fluctuations in ATP-depleted cells, allowing us to estimate the viscoelastic parameters for a range of timescales. We then determined the force spectrum by combining these viscoelastic properties with measurements of spontaneous fluctuations tracked in control cells. Comparisons with previous measurements made using FSM revealed an excellent match. Copyright © 2018 Biophysical Society. Published by Elsevier Inc. All rights reserved.

Making the Nanoworld Accessible: Nanoscience Education Using Scanning Probe Methods

NASA Astrophysics Data System (ADS)

Knorr, Daniel; Killgore, Jason; Gray, Tomoko; Ginger, David; Wei, Joseph; Chen, Yeechi; Sarikaya, Mehmet; Fong, Hanson; Griffith, Tom; Overney, Rene

2008-03-01

A partnership between researchers and educators at the University of Washington, North Seattle Community College and two companies, Nanosurf, AG and nanoScience Instruments has been forged to develop a nationally replicable model of a sustainable and up-to-date undergraduate teaching laboratory of scanning probe microscopy (SPM) methods applied to nanoscience and nanotechnology. Within this partnership a new paradigm of operating and maintaining a SPM laboratory has been developed that provides a truly hands-on experience in a classroom laboratory setting with a small student to instrument ratio involving a variety of SPM techniques and topics. To date, we have run a first successful undergraduate laboratory workshop, where students were able to have extensive hands-on experience on five SPM modes of operation including: electrostatic force microscopy involving photovoltaic polymeric materials, tunneling microscopy and the determination of the workfunction, and nanolithography using the dip-pen method. http://depts.washington.edu/nanolab/NUE/UNIQUE/NUE/UNIQUE.htm

Electro-optical interfacial effects on a graphene/π-conjugated organic semiconductor hybrid system

PubMed Central

Araujo, Karolline A S; Cury, Luiz A; Matos, Matheus J S; Fernandes, Thales F D; Cançado, Luiz G

2018-01-01

The influence of graphene and retinoic acid (RA) – a π-conjugated organic semiconductor – interface on their hybrid system is investigated. The physical properties of the interface are assessed via scanning probe microscopy, optical spectroscopy (photoluminescence and Raman) and ab initio calculations. The graphene/RA interaction induces the formation of a well-organized π-conjugated self-assembled monolayer (SAM) at the interface. Such structural organization leads to the high optical emission efficiency of the RA SAM, even at room temperature. Additionally, photo-assisted electrical force microscopy, photo-assisted scanning Kelvin probe microscopy and Raman spectroscopy indicate a RA-induced graphene doping and photo-charge generation. Finally, the optical excitation of the RA monolayer generates surface potential changes on the hybrid system. In summary, interface-induced organized structures atop 2D materials may have an important impact on both design and operation of π-conjugated nanomaterial-based hybrid systems. PMID:29600157

Full data acquisition in Kelvin Probe Force Microscopy: Mapping dynamic electric phenomena in real space.

PubMed

Collins, Liam; Belianinov, Alex; Somnath, Suhas; Balke, Nina; Kalinin, Sergei V; Jesse, Stephen

2016-08-12

Kelvin probe force microscopy (KPFM) has provided deep insights into the local electronic, ionic and electrochemical functionalities in a broad range of materials and devices. In classical KPFM, which utilizes heterodyne detection and closed loop bias feedback, the cantilever response is down-sampled to a single measurement of the contact potential difference (CPD) per pixel. This level of detail, however, is insufficient for materials and devices involving bias and time dependent electrochemical events; or at solid-liquid interfaces, where non-linear or lossy dielectrics are present. Here, we demonstrate direct recovery of the bias dependence of the electrostatic force at high temporal resolution using General acquisition Mode (G-Mode) KPFM. G-Mode KPFM utilizes high speed detection, compression, and storage of the raw cantilever deflection signal in its entirety at high sampling rates. We show how G-Mode KPFM can be used to capture nanoscale CPD and capacitance information with a temporal resolution much faster than the cantilever bandwidth, determined by the modulation frequency of the AC voltage. In this way, G-Mode KPFM offers a new paradigm to study dynamic electric phenomena in electroactive interfaces as well as a promising route to extend KPFM to the solid-liquid interface.

Epitaxial growth of pentacene on alkali halide surfaces studied by Kelvin probe force microscopy.

PubMed

Neff, Julia L; Milde, Peter; León, Carmen Pérez; Kundrat, Matthew D; Eng, Lukas M; Jacob, Christoph R; Hoffmann-Vogel, Regina

2014-04-22

In the field of molecular electronics, thin films of molecules adsorbed on insulating surfaces are used as the functional building blocks of electronic devices. Control of the structural and electronic properties of the thin films is required for reliably operating devices. Here, noncontact atomic force and Kelvin probe force microscopies have been used to investigate the growth and electrostatic landscape of pentacene on KBr(001) and KCl(001) surfaces. We have found that, together with molecular islands of upright standing pentacene, a new phase of tilted molecules appears near step edges on KBr. Local contact potential differences (LCPD) have been studied with both Kelvin experiments and density functional theory calculations. Our images reveal that differently oriented molecules display different LCPD and that their value is independent of the number of molecular layers. These results point to the formation of an interface dipole, which may be explained by a partial charge transfer from the pentacene to the surface. Moreover, the monitoring of the evolution of the pentacene islands shows that they are strongly affected by dewetting: Multilayers build up at the expense of monolayers, and in the Kelvin images, previously unknown line defects appear, which reveal the epitaxial growth of pentacene crystals.

SPM investigation of local aging effects in glassy polymers

NASA Astrophysics Data System (ADS)

Crider, Philip

2005-03-01

We investigate the cooperative and heterogeneous nature of glassy dynamics by nanometer-scale probing in a glassy polymer, Polyvinyl-Actetate (PVAc), with a Scanning Force Microscope (SFM). Using ultra-high-vacuum (UHV) Scanning Capacitive Force Microscopy techniques, nanometer-scale capacitive responses are probed. Dielectric relaxation near the glass transition is investigated, and scanning capabilities are utilized to analyze spatial response on a nanometer scale. The results of these studies may yield insight into the understanding of temperature-dependent cooperative length scales, local aging properties, and energy landscape properties of evolving dipole clusters on a mesoscopic scale. Results are used to test the validity and relevance of current models of glassy dynamics.

Development of in-situ high-voltage and high-temperature stressing capability on atomic force microscopy platform

DOE PAGES

Xiao, Chuanxiao; Jiang, Chun-Sheng; Johnston, Steve; ...

2017-10-18

Reliability has become an increasingly important issue as photovoltaic technologies mature. However, researching reliability at the nanometer scale is in its infancy; in particular, in-situ studies have not been reported to date. Here, to investigate potential-induced degradation (PID) of solar cell modules, we have developed an in-situ stressing capability with applied high voltage (HV) and high temperature (HT) on an atomic force microscopy (AFM) platform. We designed a sample holder to simultaneously accommodate 1000-V HV and 200 degrees C HT stressing. Three technical challenges have been overcome along with the development: thermal drift at HT, HV interference with measurement, andmore » arc discharge caused by HV. We demonstrated no observable measurement artifact under the stress conditions. Based on our in-situ stressing AFM, Kelvin probe force microscopy potential imaging revealed the evolution of electrical potential across the junction along with the PID stressing time, which provides vital information to further study the PID mechanism.« less

Magnetic force microscopy with frequency-modulated capacitive tip-sample distance control

NASA Astrophysics Data System (ADS)

Zhao, X.; Schwenk, J.; Mandru, A. O.; Penedo, M.; Baćani, M.; Marioni, M. A.; Hug, H. J.

2018-01-01

In a step towards routinely achieving 10 nm spatial resolution with magnetic force microscopy, we have developed a robust method for active tip-sample distance control based on frequency modulation of the cantilever oscillation. It allows us to keep a well-defined tip-sample distance of the order of 10 nm within better than +/- 0.4 nm precision throughout the measurement even in the presence of energy dissipative processes, and is adequate for single-passage non-contact operation in vacuum. The cantilever is excited mechanically in a phase-locked loop to oscillate at constant amplitude on its first flexural resonance mode. This frequency is modulated by an electrostatic force gradient generated by tip-sample bias oscillating from a few hundred Hz up to a few kHz. The sum of the side bands’ amplitudes is a proxy for the tip-sample distance and can be used for tip-sample distance control. This method can also be extended to other scanning probe microscopy techniques.

Development of in-situ high-voltage and high-temperature stressing capability on atomic force microscopy platform

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xiao, Chuanxiao; Jiang, Chun-Sheng; Johnston, Steve

Reliability has become an increasingly important issue as photovoltaic technologies mature. However, researching reliability at the nanometer scale is in its infancy; in particular, in-situ studies have not been reported to date. Here, to investigate potential-induced degradation (PID) of solar cell modules, we have developed an in-situ stressing capability with applied high voltage (HV) and high temperature (HT) on an atomic force microscopy (AFM) platform. We designed a sample holder to simultaneously accommodate 1000-V HV and 200 degrees C HT stressing. Three technical challenges have been overcome along with the development: thermal drift at HT, HV interference with measurement, andmore » arc discharge caused by HV. We demonstrated no observable measurement artifact under the stress conditions. Based on our in-situ stressing AFM, Kelvin probe force microscopy potential imaging revealed the evolution of electrical potential across the junction along with the PID stressing time, which provides vital information to further study the PID mechanism.« less

Segmentation of vessels cluttered with cells using a physics based model.

PubMed

Schmugge, Stephen J; Keller, Steve; Nguyen, Nhat; Souvenir, Richard; Huynh, Toan; Clemens, Mark; Shin, Min C

2008-01-01

Segmentation of vessels in biomedical images is important as it can provide insight into analysis of vascular morphology, topology and is required for kinetic analysis of flow velocity and vessel permeability. Intravital microscopy is a powerful tool as it enables in vivo imaging of both vasculature and circulating cells. However, the analysis of vasculature in those images is difficult due to the presence of cells and their image gradient. In this paper, we provide a novel method of segmenting vessels with a high level of cell related clutter. A set of virtual point pairs ("vessel probes") are moved reacting to forces including Vessel Vector Flow (VVF) and Vessel Boundary Vector Flow (VBVF) forces. Incorporating the cell detection, the VVF force attracts the probes toward the vessel, while the VBVF force attracts the virtual points of the probes to localize the vessel boundary without being distracted by the image features of the cells. The vessel probes are moved according to Newtonian Physics reacting to the net of forces applied on them. We demonstrate the results on a set of five real in vivo images of liver vasculature cluttered by white blood cells. When compared against the ground truth prepared by the technician, the Root Mean Squared Error (RMSE) of segmentation with VVF and VBVF was 55% lower than the method without VVF and VBVF.

Integrin-specific mechanoresponses to compression and extension probed by cylindrical flat-ended AFM tips in lung cells.

PubMed

Acerbi, Irene; Luque, Tomás; Giménez, Alícia; Puig, Marta; Reguart, Noemi; Farré, Ramon; Navajas, Daniel; Alcaraz, Jordi

2012-01-01

Cells from lung and other tissues are subjected to forces of opposing directions that are largely transmitted through integrin-mediated adhesions. How cells respond to force bidirectionality remains ill defined. To address this question, we nanofabricated flat-ended cylindrical Atomic Force Microscopy (AFM) tips with ~1 µm(2) cross-section area. Tips were uncoated or coated with either integrin-specific (RGD) or non-specific (RGE/BSA) molecules, brought into contact with lung epithelial cells or fibroblasts for 30 s to form focal adhesion precursors, and used to probe cell resistance to deformation in compression and extension. We found that cell resistance to compression was globally higher than to extension regardless of the tip coating. In contrast, both tip-cell adhesion strength and resistance to compression and extension were the highest when probed at integrin-specific adhesions. These integrin-specific mechanoresponses required an intact actin cytoskeleton, and were dependent on tyrosine phosphatases and Ca(2+) signaling. Cell asymmetric mechanoresponse to compression and extension remained after 5 minutes of tip-cell adhesion, revealing that asymmetric resistance to force directionality is an intrinsic property of lung cells, as in most soft tissues. Our findings provide new insights on how lung cells probe the mechanochemical properties of the microenvironment, an important process for migration, repair and tissue homeostasis.

Optical and electrical properties of Cu-based all oxide semi-transparent photodetector

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kim, Hong-Sik; Patel, Malkeshkumar; Yadav, Pankaj

2016-09-05

Zero-bias operating Cu oxide-based photodetector was achieved by using large-scale available sputtering method. Cu oxide (Cu{sub 2}O or CuO) was used as p-type transparent layer to form a heterojunction by contacting n-type ZnO layer. All metal-oxide materials were employed to realize transparent device at room temperature and showed a high transparency (>75% at 600 nm) with excellent photoresponses. The structural, morphological, optical, and electrical properties of Cu oxides of CuO and Cu{sub 2}O are evaluated in depth by UV-visible spectrometer, X-ray diffraction, scanning electron microscopy, atomic force microscopy, Kelvin probe force microscopy, and Hall measurements. We may suggest a route ofmore » high-functional Cu oxide-based photoelectric devices for the applications in flexible and transparent electronics.« less

Single- and multi-frequency detection of surface displacements via scanning probe microscopy.

PubMed

Romanyuk, Konstantin; Luchkin, Sergey Yu; Ivanov, Maxim; Kalinin, Arseny; Kholkin, Andrei L

2015-02-01

Piezoresponse force microscopy (PFM) provides a novel opportunity to detect picometer-level displacements induced by an electric field applied through a conducting tip of an atomic force microscope (AFM). Recently, it was discovered that superb vertical sensitivity provided by PFM is high enough to monitor electric-field-induced ionic displacements in solids, the technique being referred to as electrochemical strain microscopy (ESM). ESM has been implemented only in multi-frequency detection modes such as dual AC resonance tracking (DART) and band excitation, where the response is recorded within a finite frequency range, typically around the first contact resonance. In this paper, we analyze and compare signal-to-noise ratios of the conventional single-frequency method with multi-frequency regimes of measuring surface displacements. Single-frequency detection ESM is demonstrated using a commercial AFM.

Universal aspects of adhesion and atomic force microscopy

NASA Technical Reports Server (NTRS)

Banerjea, Amitava; Smith, John R.; Ferrante, John

1990-01-01

Adhesive energies are computed for flat and atomically sharp tips as a function of the normal distance to the substrate. The dependence of binding energies on tip shape is investigated. The magnitudes of the binding energies for the atomic force microscope are found to depend sensitively on tip material, tip shape and the sample site being probed. The form of the energy-distance curve, however, is universal and independent of these variables, including tip shape.

Determination of ferroelectric contributions to electromechanical response by frequency dependent piezoresponse force microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Seol, Daehee; Park, Seongjae; Varenyk, Olexandr V.

Hysteresis loop analysis via piezoresponse force microscopy (PFM) is typically performed to probe the existence of ferroelectricity at the nanoscale. But, such an approach is rather complex in accurately determining the pure contribution of ferroelectricity to the PFM. We suggest a facile method to discriminate the ferroelectric effect from the electromechanical (EM) response through the use of frequency dependent ac amplitude sweep with combination of hysteresis loops in PFM. This combined study through experimental and theoretical approaches verifies that this method can be used as a new tool to differentiate the ferroelectric effect from the other factors that contribute tomore » the EM response.« less

Direct quantitative measurement of the C═O⋅⋅⋅H–C bond by atomic force microscopy

PubMed Central

Kawai, Shigeki; Nishiuchi, Tomohiko; Kodama, Takuya; Spijker, Peter; Pawlak, Rémy; Meier, Tobias; Tracey, John; Kubo, Takashi; Meyer, Ernst; Foster, Adam S.

2017-01-01

The hydrogen atom—the smallest and most abundant atom—is of utmost importance in physics and chemistry. Although many analysis methods have been applied to its study, direct observation of hydrogen atoms in a single molecule remains largely unexplored. We use atomic force microscopy (AFM) to resolve the outermost hydrogen atoms of propellane molecules via very weak C═O⋅⋅⋅H–C hydrogen bonding just before the onset of Pauli repulsion. The direct measurement of the interaction with a hydrogen atom paves the way for the identification of three-dimensional molecules such as DNAs and polymers, building the capabilities of AFM toward quantitative probing of local chemical reactivity. PMID:28508080

Current Transport Properties of Monolayer Graphene/n-Si Schottky Diodes

NASA Astrophysics Data System (ADS)

Pathak, C. S.; Garg, Manjari; Singh, J. P.; Singh, R.

2018-05-01

The present work reports on the fabrication and the detailed macroscopic and nanoscale electrical characteristics of monolayer graphene/n-Si Schottky diodes. The temperature dependent electrical transport properties of monolayer graphene/n-Si Schottky diodes were investigated. Nanoscale electrical characterizations were carried out using Kelvin probe force microscopy and conducting atomic force microscopy. Most the values of ideality factor and barrier height are found to be in the range of 2.0–4.4 and 0.50–0.70 eV for monolayer graphene/n-Si nanoscale Schottky contacts. The tunneling of electrons is found to be responsible for the high value of ideality factor for nanoscale Schottky contacts.

Nanoscale amorphization of GeTe nanowire with conductive atomic force microscope.

PubMed

Kim, JunHo

2014-10-01

We fabricated GeTe nanowires by using Au catalysis mediated vapor-liquid-solid method. The fabricated nanowires were confirmed by X-ray diffraction, scanning electron microscopy and transmission electron microscopy. For a nanowire with - 150 nm diameter, we performed amorphization experiment with conductive atomic force microscope. We examined the structural change of the nanowire with several bias voltages from 0 V to 10 V. Above bias voltage of 6-7 V, some points of the nanowire showed transition to amorphous phase. The consumed energy for the amorphization was estimated to be 4-5 nJ, which was close to the other result of nanowire tested with a four probe device.

Determination of ferroelectric contributions to electromechanical response by frequency dependent piezoresponse force microscopy

DOE PAGES

Seol, Daehee; Park, Seongjae; Varenyk, Olexandr V.; ...

2016-07-28

Hysteresis loop analysis via piezoresponse force microscopy (PFM) is typically performed to probe the existence of ferroelectricity at the nanoscale. But, such an approach is rather complex in accurately determining the pure contribution of ferroelectricity to the PFM. We suggest a facile method to discriminate the ferroelectric effect from the electromechanical (EM) response through the use of frequency dependent ac amplitude sweep with combination of hysteresis loops in PFM. This combined study through experimental and theoretical approaches verifies that this method can be used as a new tool to differentiate the ferroelectric effect from the other factors that contribute tomore » the EM response.« less

Sub-microsecond-resolution probe microscopy

DOEpatents

Ginger, David; Giridharagopal, Rajiv; Moore, David; Rayermann, Glennis; Reid, Obadiah

2014-04-01

Methods and apparatus are provided herein for time-resolved analysis of the effect of a perturbation (e.g., a light or voltage pulse) on a sample. By operating in the time domain, the provided method enables sub-microsecond time-resolved measurement of transient, or time-varying, forces acting on a cantilever.

Direct probing of electron and hole trapping into nano-floating-gate in organic field-effect transistor nonvolatile memories

NASA Astrophysics Data System (ADS)

Cui, Ze-Qun; Wang, Shun; Chen, Jian-Mei; Gao, Xu; Dong, Bin; Chi, Li-Feng; Wang, Sui-Dong

2015-03-01

Electron and hole trapping into the nano-floating-gate of a pentacene-based organic field-effect transistor nonvolatile memory is directly probed by Kelvin probe force microscopy. The probing is straightforward and non-destructive. The measured surface potential change can quantitatively profile the charge trapping, and the surface characterization results are in good accord with the corresponding device behavior. Both electrons and holes can be trapped into the nano-floating-gate, with a preference of electron trapping than hole trapping. The trapped charge quantity has an approximately linear relation with the programming/erasing gate bias, indicating that the charge trapping in the device is a field-controlled process.

Instant live-cell super-resolution imaging of cellular structures by nanoinjection of fluorescent probes.

PubMed

Hennig, Simon; van de Linde, Sebastian; Lummer, Martina; Simonis, Matthias; Huser, Thomas; Sauer, Markus

2015-02-11

Labeling internal structures within living cells with standard fluorescent probes is a challenging problem. Here, we introduce a novel intracellular staining method that enables us to carefully control the labeling process and provides instant access to the inner structures of living cells. Using a hollow glass capillary with a diameter of <100 nm, we deliver functionalized fluorescent probes directly into the cells by (di)electrophoretic forces. The label density can be adjusted and traced directly during the staining process by fluorescence microscopy. We demonstrate the potential of this technique by delivering and imaging a range of commercially available cell-permeable and nonpermeable fluorescent probes to cells.

Surface polymerization of (3,4-ethylenedioxythiophene) probed by in situ scanning tunneling microscopy on Au(111) in ionic liquids

NASA Astrophysics Data System (ADS)

Ahmad, Shahzada; Carstens, Timo; Berger, Rüdiger; Butt, Hans-Jürgen; Endres, Frank

2011-01-01

The electropolymerization of 3,4-ethylenedioxythiophene (EDOT) to poly(3,4-ethylenedioxythiophene) (PEDOT) was investigated in the air and water-stable ionic liquids 1-hexyl-3-methylimidazolium tris(pentafluoroethyl) trifluorophosphate [HMIm]FAP and 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl) amide [EMIm]TFSA. In situscanning tunnelling microscopy (STM) results show that the electropolymerization of EDOT in the ionic liquid can be probed on the nanoscale. In contrast to present understanding, it was observed that the EDOT can be oxidised in ionic liquids well below its oxidation potential and the under potential growth of polymer was visualized by in situSTM. These results serve as the first study to confirm the under potential growth of conducting polymers in ionic liquids. Furthermore, ex situmicroscopy measurements were performed. Quite a high current of 670 nA was observed on the nanoscale by conductive scanning force microscopy (CSFM).The electropolymerization of 3,4-ethylenedioxythiophene (EDOT) to poly(3,4-ethylenedioxythiophene) (PEDOT) was investigated in the air and water-stable ionic liquids 1-hexyl-3-methylimidazolium tris(pentafluoroethyl) trifluorophosphate [HMIm]FAP and 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl) amide [EMIm]TFSA. In situscanning tunnelling microscopy (STM) results show that the electropolymerization of EDOT in the ionic liquid can be probed on the nanoscale. In contrast to present understanding, it was observed that the EDOT can be oxidised in ionic liquids well below its oxidation potential and the under potential growth of polymer was visualized by in situSTM. These results serve as the first study to confirm the under potential growth of conducting polymers in ionic liquids. Furthermore, ex situmicroscopy measurements were performed. Quite a high current of 670 nA was observed on the nanoscale by conductive scanning force microscopy (CSFM). Electronic supplementary information (ESI) available: In situ image of PEDOT in [HMIm]FAP and in situ studies of PEDOT grown in [EMIm]TFSA and redox behavior of PEDOT. See DOI: 10.1039/c0nr00579g

Probing atomic-scale friction on reconstructed surfaces of single-crystal semiconductors

NASA Astrophysics Data System (ADS)

Goryl, M.; Budzioch, J.; Krok, F.; Wojtaszek, M.; Kolmer, M.; Walczak, L.; Konior, J.; Gnecco, E.; Szymonski, M.

2012-02-01

Friction force microscopy (FFM) investigations have been performed on reconstructed (001) surfaces of InSb and Ge in an ultrahigh vacuum. On the c(8×2) reconstruction of InSb(001) atomic resolution is achieved under superlubric conditions, and the features observed in the lateral force images are precisely reproduced by numerical simulations, taking into account possible decorations of the probing tip. On the simultaneously acquired (1×3) reconstruction a significant disorder of the surface atoms is observed. If the loading force increases, friction becomes much larger on this reconstruction compared to the c(8×2) one. In FFM images acquired on the Ge(001)(2×1) characteristic substructures are resolved within the unit cells. In such a case, a strong dependence of the friction pattern on the scan direction is observed.

A test method for determining adhesion forces and Hamaker constants of cementitious materials using atomic force microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lomboy, Gilson; Sundararajan, Sriram, E-mail: srirams@iastate.edu; Wang Kejin

2011-11-15

A method for determining Hamaker constant of cementitious materials is presented. The method involved sample preparation, measurement of adhesion force between the tested material and a silicon nitride probe using atomic force microscopy in dry air and in water, and calculating the Hamaker constant using appropriate contact mechanics models. The work of adhesion and Hamaker constant were computed from the pull-off forces using the Johnson-Kendall-Roberts and Derjagin-Muller-Toropov models. Reference materials with known Hamaker constants (mica, silica, calcite) and commercially available cementitious materials (Portland cement (PC), ground granulated blast furnace slag (GGBFS)) were studied. The Hamaker constants of the reference materialsmore » obtained are consistent with those published by previous researchers. The results indicate that PC has a higher Hamaker constant than GGBFS. The Hamaker constant of PC in water is close to the previously predicted value C{sub 3}S, which is attributed to short hydration time ({<=} 45 min) used in this study.« less

Probing the compressibility of tumor cell nuclei by combined atomic force-confocal microscopy

NASA Astrophysics Data System (ADS)

Krause, Marina; te Riet, Joost; Wolf, Katarina

2013-12-01

The cell nucleus is the largest and stiffest organelle rendering it the limiting compartment during migration of invasive tumor cells through dense connective tissue. We here describe a combined atomic force microscopy (AFM)-confocal microscopy approach for measurement of bulk nuclear stiffness together with simultaneous visualization of the cantilever-nucleus contact and the fate of the cell. Using cantilevers functionalized with either tips or beads and spring constants ranging from 0.06-10 N m-1, force-deformation curves were generated from nuclear positions of adherent HT1080 fibrosarcoma cell populations at unchallenged integrity, and a nuclear stiffness range of 0.2 to 2.5 kPa was identified depending on cantilever type and the use of extended fitting models. Chromatin-decondensating agent trichostatin A (TSA) induced nuclear softening of up to 50%, demonstrating the feasibility of our approach. Finally, using a stiff bead-functionalized cantilever pushing at maximal system-intrinsic force, the nucleus was deformed to 20% of its original height which after TSA treatment reduced further to 5% remaining height confirming chromatin organization as an important determinant of nuclear stiffness. Thus, combined AFM-confocal microscopy is a feasible approach to study nuclear compressibility to complement concepts of limiting nuclear deformation in cancer cell invasion and other biological processes.

Towards a unified description of the charge transport mechanisms in conductive atomic force microscopy studies of semiconducting polymers.

PubMed

Moerman, D; Sebaihi, N; Kaviyil, S E; Leclère, P; Lazzaroni, R; Douhéret, O

2014-09-21

In this work, conductive atomic force microscopy (C-AFM) is used to study the local electrical properties in thin films of self-organized fibrillate poly(3-hexylthiophene) (P3HT), as a reference polymer semiconductor. Depending on the geometrical confinement in the transport channel, the C-AFM current is shown to be governed either by the charge transport in the film or by the carrier injection at the tip-sample contact, leading to either bulk or local electrical characterization of the semiconducting polymer, respectively. Local I-V profiles allow discrimination of the different dominating electrical mechanisms, i.e., resistive in the transport regime and space charge limited current (SCLC) in the local regime. A modified Mott-Gurney law is analytically derived for the contact regime, taking into account the point-probe geometry of the contact and the radial injection of carriers. Within the SCLC regime, the probed depth is shown to remain below 12 nm with a lateral electrical resolution below 5 nm. This confirms that high resolution is reached in those C-AFM measurements, which therefore allows for the analysis of single organic semiconducting nanostructures. The carrier density and mobility in the volume probed under the tip under steady-state conditions are also determined in the SCLC regime.

Direct Probing of Polarization Charge at Nanoscale Level

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kwon, Owoong; Seol, Daehee; Lee, Dongkyu

Ferroelectric materials possess spontaneous polarization that can be used for multiple applications. Owing to a long-term development of reducing the sizes of devices, the preparation of ferroelectric materials and devices is entering the nanometer-scale regime. In order to evaluate the ferroelectricity, there is a need to investigate the polarization charge at the nanoscale. Nonetheless, it is generally accepted that the detection of polarization charges using a conventional conductive atomic force microscopy (CAFM) without a top electrode is not feasible because the nanometer-scale radius of an atomic force microscopy (AFM) tip yields a very low signal-to-noise ratio. But, the detection ismore » unrelated to the radius of an AFM tip and, in fact, a matter of the switched area. In this work, the direct probing of the polarization charge at the nanoscale is demonstrated using the positive-up-negative-down method based on the conventional CAFM approach without additional corrections or circuits to reduce the parasitic capacitance. The polarization charge densities of 73.7 and 119.0 µC cm -2 are successfully probed in ferroelectric nanocapacitors and thin films, respectively. The results we obtained show the feasibility of the evaluation of polarization charge at the nanoscale and provide a new guideline for evaluating the ferroelectricity at the nanoscale.« less

Probing physical properties at the nanoscale using atomic force microscopy

NASA Astrophysics Data System (ADS)

Ditzler, Lindsay Rachel

Techniques that measure physical properties at the nanoscale with high sensitivity are significantly limited considering the number of new nanomaterials being developed. The development of atomic force microscopy (AFM) has lead to significant advancements in the ability to characterize physical properties of materials in all areas of science: chemistry, physics, engineering, and biology have made great scientific strides do to the versatility of the AFM. AFM is used for quantification of many physical properties such as morphology, electrical, mechanical, magnetic, electrochemical, binding interactions, and protein folding. This work examines the electrical and mechanical properties of materials applicable to the field of nano-electronics. As electronic devices are miniaturized the demand for materials with unique electrical properties, which can be developed and exploited, has increased. For example, discussed in this work, a derivative of tetrathiafulvalene, which exhibits a unique loss of conductivity upon compression of the self-assembled monolayer could be developed into a molecular switch. This work also compares tunable organic (tetraphenylethylene tetracarboxylic acid and bis(pyridine)s assemblies) and metal-organic (Silver-stilbizole coordination compounds) crystals which show high electrical conductivity. The electrical properties of these materials vary depending on their composition allowing for the development of compositionally tunable functional materials. Additional work was done to investigate the effects of molecular environment on redox active 11-ferroceneyl-1 undecanethiol (Fc) molecules. The redox process of mixed monolayers of Fc and decanethiol was measured using conductive probe atomic force microscopy and force spectroscopy. As the concentration of Fc increased large, variations in the force were observed. Using these variations the number of oxidized molecules in the monolayer was determined. AFM is additionally capable of investigating interactions at the nanoscale, such as ligand-receptor interactions. This work examines the interactions between the enzyme dihydrofolate reductase (DHFR), a widely investigated enzyme targeted for cancer and antimicrobial pharmaceutical, and methotrexate (MTX), a strong competitive inhibitor of DHFR. The DHFR was immobilized on a gold substrate, bound through a single surface cysteine, and maintained catalytic activity. AFM probe was functionalized with MTX and the interaction strength was measured using AFM. This work highlights the versatility of AFM, specifically force spectroscopy for the quantification of electrical, mechanical, and ligand-receptor interactions at the nanoscale.

Investigating the Mechanical Properties of Plasma von Willebrand Factor Using Atomic Force Microscopy

NASA Astrophysics Data System (ADS)

Wijeratne, Sitara; Botello, Eric; Yeh, Hui-Chun; Zhou, Zhou; Bergeron, Angela; Frey, Eric; Moake, Joel; Dong, Jing-Fei; Kiang, Ching-Hwa

2011-10-01

Single-molecule manipulation allows us to study the real-time kinetics of complex cellular processes. The mechanochemistry of different forms of von Willebrand factor (VWF) and their receptor-ligand binding kinetics can be probed by atomic force microscopy (AFM). Since plasma VWF can be activated upon shear, the structural and functional properties of VWF that are critical in mediating thrombus formation become important. Here we characterized the mechanical resistance to domain unfolding of VWF to determine its conformational states. We found the shear-induced conformational changes, hence the mechanical property, can be detected by the change in unfolding forces. The relaxation rate of such effect is much longer than expected. Our results offer an insight in establishing strategies for regulating VWF adhesion activity, increasing our understanding of surface-induced thrombosis as mediated by VWF.

Single molecule imaging of RNA polymerase II using atomic force microscopy

NASA Astrophysics Data System (ADS)

Rhodin, Thor; Fu, Jianhua; Umemura, Kazuo; Gad, Mohammed; Jarvis, Suzi; Ishikawa, Mitsuru

2003-03-01

An atomic force microscopy (AFM) study of the shape, orientation and surface topology of RNA polymerase II supported on silanized freshly cleaved mica was made. The overall aim is to define the molecular topology of RNA polymerase II in appropriate fluids to help clarify the relationship of conformational features to biofunctionality. A Nanoscope III atomic force microscope was used in the tapping mode with oxide-sharpened (8-10 nm) Si 3N 4 probes in aqueous zinc chloride buffer. The main structural features observed by AFM were compared to those derived from electron-density plots based on X-ray crystallographic studies. The conformational features included a bilobal silhouette with an inverted umbrella-shaped crater connected to a reaction site. These studies provide a starting point for constructing a 3D-AFM profiling analysis of proteins such as RNA polymerase complexes.

Sharp-Tip Silver Nanowires Mounted on Cantilevers for High-Aspect-Ratio High-Resolution Imaging.

PubMed

Ma, Xuezhi; Zhu, Yangzhi; Kim, Sanggon; Liu, Qiushi; Byrley, Peter; Wei, Yang; Zhang, Jin; Jiang, Kaili; Fan, Shoushan; Yan, Ruoxue; Liu, Ming

2016-11-09

Despite many efforts to fabricate high-aspect-ratio atomic force microscopy (HAR-AFM) probes for high-fidelity, high-resolution topographical imaging of three-dimensional (3D) nanostructured surfaces, current HAR probes still suffer from unsatisfactory performance, low wear-resistivity, and extravagant prices. The primary objective of this work is to demonstrate a novel design of a high-resolution (HR) HAR AFM probe, which is fabricated through a reliable, cost-efficient benchtop process to precisely implant a single ultrasharp metallic nanowire on a standard AFM cantilever probe. The force-displacement curve indicated that the HAR-HR probe is robust against buckling and bending up to 150 nN. The probes were tested on polymer trenches, showing a much better image fidelity when compared with standard silicon tips. The lateral resolution, when scanning a rough metal thin film and single-walled carbon nanotubes (SW-CNTs), was found to be better than 8 nm. Finally, stable imaging quality in tapping mode was demonstrated for at least 15 continuous scans indicating high resistance to wear. These results demonstrate a reliable benchtop fabrication technique toward metallic HAR-HR AFM probes with performance parallel or exceeding that of commercial HAR probes, yet at a fraction of their cost.

Effects of methotrexate on the viscoelastic properties of single cells probed by atomic force microscopy.

PubMed

Li, Mi; Liu, Lianqing; Xiao, Xiubin; Xi, Ning; Wang, Yuechao

2016-10-01

Methotrexate is a commonly used anti-cancer chemotherapy drug. Cellular mechanical properties are fundamental parameters that reflect the physiological state of a cell. However, so far the role of cellular mechanical properties in the actions of methotrexate is still unclear. In recent years, probing the behaviors of single cells with the use of atomic force microscopy (AFM) has contributed much to the field of cell biomechanics. In this work, with the use of AFM, the effects of methotrexate on the viscoelastic properties of four types of cells were quantitatively investigated. The inhibitory and cytotoxic effects of methotrexate on the proliferation of cells were observed by optical and fluorescence microscopy. AFM indenting was used to measure the changes of cellular viscoelastic properties (Young's modulus and relaxation time) by using both conical tip and spherical tip, quantitatively showing that the stimulation of methotrexate resulted in a significant decrease of both cellular Young's modulus and relaxation times. The morphological changes of cells induced by methotrexate were visualized by AFM imaging. The study improves our understanding of methotrexate action and offers a novel way to quantify drug actions at the single-cell level by measuring cellular viscoelastic properties, which may have potential impacts on developing label-free methods for drug evaluation.

Atomic Force Microscope for Imaging and Spectroscopy

NASA Technical Reports Server (NTRS)

Pike, W. T.; Hecht, M. H.; Anderson, M. S.; Akiyama, T.; Gautsch, S.; deRooij, N. F.; Staufer, U.; Niedermann, Ph.; Howald, L.; Mueller, D.

2000-01-01

We have developed, built, and tested an atomic force microscope (AFM) for extraterrestrial applications incorporating a micromachined tip array to allow for probe replacement. It is part of a microscopy station originally intended for NASA's 2001 Mars lander to identify the size, distribution, and shape of Martian dust and soil particles. As well as imaging topographically down to nanometer resolution, this instrument can be used to reveal chemical information and perform infrared and Raman spectroscopy at unprecedented resolution.

Reconstruction of Energy Surfaces from Friction Force Microscopy Measurements with the Jarzynski Equality

NASA Astrophysics Data System (ADS)

Berkovich, Ronen; Klafter, Joseph; Urbakh, Michael

Free energy is one of the most fundamental thermodynamic functions, determining relative phase stability and serving as a generating function for other thermodynamic quantities. The calculation of free energies is a challenging enterprise. In equilibrium statistical mechanics, the free energy is related to the canonical partition function. The partition function itself involves integrations over all degrees of freedom in the system and, in most cases, cannot be easily calculated directly. In 1997, Jarzynski proved a remarkable equality that allows computing the equilibrium free-energy difference between two states from the probability distribution of the nonequilibrium work done on the system to switch between the two states. The Jarzynski equality provides a powerful free-energy difference estimator from a set of irreversible experiments. This method is closely related to free-energy perturbation approach, which is also a computational technique for estimating free-energy differences. The ability to map potential profiles and topologies is of major significance to areas as diverse as biological recognition and nanoscale friction. This capability has been demonstrated for frictional studies where a force between the tip of the scanning force microscope and the surface is probed. The surface free-energy corrugation produces a detectable friction forces. Thus, friction force microscopy (FFM) should be able to discriminate between energetically different areas on the probed surface. Here, we apply the Jarzynski equality for the analysis of FFM measurements and thus obtain a variation of the free energy along a surface.

Combined frequency modulated atomic force microscopy and scanning tunneling microscopy detection for multi-tip scanning probe microscopy applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Morawski, Ireneusz; Institute of Experimental Physics, University of Wrocław, pl. M. Borna 9, 50-204 Wrocław; Spiegelberg, Richard

A method which allows scanning tunneling microscopy (STM) tip biasing independent of the sample bias during frequency modulated atomic force microscopy (AFM) operation is presented. The AFM sensor is supplied by an electronic circuit combining both a frequency shift signal and a tunneling current signal by means of an inductive coupling. This solution enables a control of the tip potential independent of the sample potential. Individual tip biasing is specifically important in order to implement multi-tip STM/AFM applications. An extensional quartz sensor (needle sensor) with a conductive tip is applied to record simultaneously topography and conductivity of the sample. Themore » high resonance frequency of the needle sensor (1 MHz) allows scanning of a large area of the surface being investigated in a reasonably short time. A recipe for the amplitude calibration which is based only on the frequency shift signal and does not require the tip being in contact is presented. Additionally, we show spectral measurements of the mechanical vibration noise of the scanning system used in the investigations.« less

Systematic Validation and Atomic Force Microscopy of Non-Covalent Short Oligonucleotide Barcode Microarrays

PubMed Central

Cook, Michael A.; Chan, Chi-Kin; Jorgensen, Paul; Ketela, Troy; So, Daniel; Tyers, Mike; Ho, Chi-Yip

2008-01-01

Background Molecular barcode arrays provide a powerful means to analyze cellular phenotypes in parallel through detection of short (20–60 base) unique sequence tags, or “barcodes”, associated with each strain or clone in a collection. However, costs of current methods for microarray construction, whether by in situ oligonucleotide synthesis or ex situ coupling of modified oligonucleotides to the slide surface are often prohibitive to large-scale analyses. Methodology/Principal Findings Here we demonstrate that unmodified 20mer oligonucleotide probes printed on conventional surfaces show comparable hybridization signals to covalently linked 5′-amino-modified probes. As a test case, we undertook systematic cell size analysis of the budding yeast Saccharomyces cerevisiae genome-wide deletion collection by size separation of the deletion pool followed by determination of strain abundance in size fractions by barcode arrays. We demonstrate that the properties of a 13K unique feature spotted 20 mer oligonucleotide barcode microarray compare favorably with an analogous covalently-linked oligonucleotide array. Further, cell size profiles obtained with the size selection/barcode array approach recapitulate previous cell size measurements of individual deletion strains. Finally, through atomic force microscopy (AFM), we characterize the mechanism of hybridization to unmodified barcode probes on the slide surface. Conclusions/Significance These studies push the lower limit of probe size in genome-scale unmodified oligonucleotide microarray construction and demonstrate a versatile, cost-effective and reliable method for molecular barcode analysis. PMID:18253494

Charge ordering, ferroelectric, and magnetic domains in LuFe{sub 2}O{sub 4} observed by scanning probe microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yang, I. K.; Jeong, Y. H., E-mail: yhj@postech.ac.kr; Kim, Jeehoon

2015-04-13

LuFe{sub 2}O{sub 4} is a multiferroic system which exhibits charge order, ferroelectricity, and ferrimagnetism simultaneously below ∼230 K. The ferroelectric/charge order domains of LuFe{sub 2}O{sub 4} are imaged with both piezoresponse force microscopy (PFM) and electrostatic force microscopy (EFM), while the magnetic domains are characterized by magnetic force microscopy (MFM). Comparison of PFM and EFM results suggests that the proposed ferroelectricity in LuFe{sub 2}O{sub 4} is not of usual displacive type but of electronic origin. Simultaneous characterization of ferroelectric/charge order and magnetic domains by EFM and MFM, respectively, on the same surface of LuFe{sub 2}O{sub 4} reveals that both domains havemore » irregular patterns of similar shape, but the length scales are quite different. The domain size is approximately 100 nm for the ferroelectric domains, while the magnetic domain size is much larger and gets as large as 1 μm. We also demonstrate that the origin of the formation of irregular domains in LuFe{sub 2}O{sub 4} is not extrinsic but intrinsic.« less

Deposition And Characterization of (Ti,Zr)N Thin Films Grown Through PAPVD By The Pulsed Arc Technique

DOE Office of Scientific and Technical Information (OSTI.GOV)

Marulanda, D. M.; Trujillo, O.; Devia, A.

The Plasma Assisted Physic Vapor Deposition (PAPVD) by the pulsed arc technique has been used for deposition of Titanium Zirconium Nitride (Ti,Zr)N coatings, using a segmented target of TiZr. The deposition was performed in a vacuum chamber with two faced electrodes (target and substrate) using nitrogen as working gas, and a power-controlled source used to produce the arc discharges. Films were deposited on stainless steel 304, and they were characterized using the X-Ray Photoelectron Spectroscopy (XPS), X-Ray Diffraction (XRD), Energy Dispersion Spectroscopy (EDS) and Scanning Probe Microscopy (SPM) techniques. The XRD patterns show different planes in which the film grows.more » Through SPM, using Atomic Force Microscopy (AFM) and Lateral Force Microscopy (LFM) modes, a nanotribologic study of the thin film was made, determining hardness and friction coefficient.« less

In situ mechanical characterization of the cell nucleus by atomic force microscopy.

PubMed

Liu, Haijiao; Wen, Jun; Xiao, Yun; Liu, Jun; Hopyan, Sevan; Radisic, Milica; Simmons, Craig A; Sun, Yu

2014-04-22

The study of nuclear mechanical properties can provide insights into nuclear dynamics and its role in cellular mechanotransduction. While several methods have been developed to characterize nuclear mechanical properties, direct intracellular probing of the nucleus in situ is challenging. Here, a modified AFM (atomic force microscopy) needle penetration technique is demonstrated to mechanically characterize cell nuclei in situ. Cytoplasmic and nuclear stiffness were determined based on two different segments on the AFM indentation curves and were correlated with simultaneous confocal Z-stack microscopy reconstructions. On the basis of direct intracellular measurement, we show that the isolated nuclei from fibroblast-like cells exhibited significantly lower Young's moduli than intact nuclei in situ. We also show that there is in situ nucleus softening in the highly metastatic bladder cancer cell line T24 when compared to its less metastatic counterpart RT4. This technique has potential to become a reliable quantitative measurement tool for intracellular mechanics studies.

Decoupling indirect topographic cross-talk in band excitation piezoresponse force microscopy imaging and spectroscopy

DOE PAGES

Mazet, Lucie; Jesse, Stephen; Niu, Gang; ...

2016-06-20

Here, all scanning probe microscopies are subjected to topographic cross-talk, meaning the topography-related contrast in functional images. Here, we investigate the signatures of indirect topographic cross-talk in piezoresponse force microscopy (PFM) imaging and spectroscopy and its decoupling using band excitation (BE) method in ferroelectric BaTiO 3 deposited on the Si substrates with free standing nanopillars of diameter 50 nm. Comparison between the single-frequency PFM and BE-PFM results shows that the measured signal can be significantly distorted by topography-induced shifts in the contact resonance frequency and cantilever transfer function. However, with proper correction, such shifts do not affect PFM imaging andmore » hysteresis loop measurements. This suggests the necessity of an advanced approach, such as BE-PFM, for detection of intrinsic sample piezoresponse on the topographically non-uniform surfaces.« less

Development of a DNA Sensor Based on Nanoporous Pt-Rich Electrodes

NASA Astrophysics Data System (ADS)

Van Hao, Pham; Thanh, Pham Duc; Xuan, Chu Thi; Hai, Nguyen Hoang; Tuan, Mai Anh

2017-06-01

Nanoporous Pt-rich electrodes with 72 at.% Pt composition were fabricated by sputtering a Pt-Ag alloy, followed by an electrochemical dealloying process to selectively etch away Ag atoms. The surface properties of nanoporous membranes were investigated by energy-dispersive x-ray spectroscopy (EDS), scanning electron microscopy (SEM), atomic force microscopy (AFM), a documentation system, and a gel image system (Gel Doc Imager). A single strand of probe deoxyribonucleic acid (DNA) was immobilized onto the electrode surface by physical adsorption. The DNA probe and target hybridization were measured using a lock-in amplifier and an electrochemical impedance spectroscope (EIS). The nanoporous Pt-rich electrode-based DNA sensor offers a fast response time of 3.7 s, with a limit of detection (LOD) of 4.35 × 10-10 M of DNA target.

Ultrasonically synthesized organic liquid-filled chitosan microcapsules: part 2: characterization using AFM (atomic force microscopy) and combined AFM-confocal laser scanning fluorescence microscopy.

PubMed

Mettu, Srinivas; Ye, Qianyu; Zhou, Meifang; Dagastine, Raymond; Ashokkumar, Muthupandian

2018-04-25

Atomic Force Microscopy (AFM) is used to measure the stiffness and Young's modulus of individual microcapsules that have a chitosan cross-linked shell encapsulating tetradecane. The oil filled microcapsules were prepared using a one pot synthesis via ultrasonic emulsification of tetradecane and crosslinking of the chitosan shell in aqueous solutions of acetic acid. The concentration of acetic acid in aqueous solutions of chitosan was varied from 0.2% to 25% v/v. The effect of acetic acid concentration and size of the individual microcapsules on the strength was probed. The deformations and forces required to rupture the microcapsules were also measured. Three dimensional deformations of microcapsules under large applied loads were obtained by the combination of Laser Scanning Confocal Microscopy (LSCM) with Atomic Force Microscopy (AFM). The stiffness, and hence the modulus, of the microcapsules was found to decrease with an increase in size with the average stiffness ranging from 82 to 111 mN m-1 and average Young's modulus ranging from 0.4 to 6.5 MPa. The forces required to rupture the microcapsules varied from 150 to 250 nN with deformations of the microcapsules up to 62 to 110% relative to their radius, respectively. Three dimensional images obtained using laser scanning confocal microscopy showed that the microcapsules retained their structure and shape after being subjected to large deformations and subsequent removal of the loads. Based on the above observations, the oil filled chitosan crosslinked microcapsules are an ideal choice for use in the food and pharmaceutical industries as they would be able to withstand the process conditions encountered.

Scanning Kelvin Probe Microscopy | Materials Science | NREL

Science.gov Websites

the measurement is performed under thermoequilibrium state; and it is the electrical potential when and electrical signals. The electrostatic force is zero when the CPD is completely compensated by a dc the measurement capabilities of the technique when a device sample is in the dark. Right: This

Sparse imaging for fast electron microscopy

NASA Astrophysics Data System (ADS)

Anderson, Hyrum S.; Ilic-Helms, Jovana; Rohrer, Brandon; Wheeler, Jason; Larson, Kurt

2013-02-01

Scanning electron microscopes (SEMs) are used in neuroscience and materials science to image centimeters of sample area at nanometer scales. Since imaging rates are in large part SNR-limited, large collections can lead to weeks of around-the-clock imaging time. To increase data collection speed, we propose and demonstrate on an operational SEM a fast method to sparsely sample and reconstruct smooth images. To accurately localize the electron probe position at fast scan rates, we model the dynamics of the scan coils, and use the model to rapidly and accurately visit a randomly selected subset of pixel locations. Images are reconstructed from the undersampled data by compressed sensing inversion using image smoothness as a prior. We report image fidelity as a function of acquisition speed by comparing traditional raster to sparse imaging modes. Our approach is equally applicable to other domains of nanometer microscopy in which the time to position a probe is a limiting factor (e.g., atomic force microscopy), or in which excessive electron doses might otherwise alter the sample being observed (e.g., scanning transmission electron microscopy).

Direct assessment of p-n junctions in single GaN nanowires by Kelvin probe force microscopy.

PubMed

Minj, Albert; Cros, Ana; Auzelle, Thomas; Pernot, Julien; Daudin, Bruno

2016-09-23

Making use of Kelvin probe force microscopy, in dark and under ultraviolet illumination, we study the characteristics of p-n junctions formed along the axis of self-organized GaN nanowires (NWs). We map the contact potential difference of the single NW p-n junctions to locate the space charge region and directly measure the depletion width and the junction voltage. Simulations indicate a shrinkage of the built-in potential for NWs with small diameter due to surface band bending, in qualitative agreement with the measurements. The photovoltage of the NW/substrate contact is studied by analyzing the response of NW segments with p- and n-type doping under illumination. Our results show that the shifts of the Fermi levels, and not the changes in surface band bending, are the most important effects under above band-gap illumination. The quantitative electrical information obtained here is important for the use of NW p-n junctions as photovoltaic or rectifying devices at the nanoscale, and is especially relevant since the technique does not require the formation of ohmic contacts to the NW junction.

Exploring Anomalous Polarization Dynamics in Organometallic Halide Perovskites

DOE PAGES

Ahmadi, Mahshid; Collins, Liam; Puretzky, Alexander; ...

2018-01-22

Organometallic halide perovskites (OMHPs) have attracted broad attention as prospective materials for optoelectronic applications. Among the many anomalous properties of these materials, of special interest are the ferroelectric properties including both classical and relaxor-like components, as a potential origin of slow dynamics, field enhancement, and anomalous mobilities. Here, ferroelectric properties of the three representative OMHPs are explored, including FAPb xSn 1–xI 3 (x = 0, x = 0.85) and FA 0.85MA 0.15PbI 3 using band excitation piezoresponse force microscopy and contact mode Kelvin probe force microscopy, providing insight into long- and short-range dipole and charge dynamics in these materials andmore » probing ferroelectric density of states. Furthermore, second-harmonic generation in thin films of OMHPs is observed, providing a direct information on the noncentrosymmetric polarization in such materials. Overall, the data provide strong evidence for the presence of ferroelectric domains in these systems; however, the domain dynamics is suppressed by fast ion dynamics. These materials hence present the limit of ferroelectric materials with spontaneous polarization dynamically screened by ionic and electronic carriers.« less

Graphene Visualizes the Ion Distribution on Air-Cleaved Mica.

PubMed

Bampoulis, Pantelis; Sotthewes, Kai; Siekman, Martin H; Zandvliet, Harold J W; Poelsema, Bene

2017-03-06

The distribution of potassium (K + ) ions on air-cleaved mica is important in many interfacial phenomena such as crystal growth, self-assembly and charge transfer on mica. However, due to experimental limitations to nondestructively probe single ions and ionic domains, their exact lateral organization is yet unknown. We show, by the use of graphene as an ultra-thin protective coating and scanning probe microscopies, that single potassium ions form ordered structures that are covered by an ice layer. The K + ions prefer to minimize the number of nearest neighbour K + ions by forming row-like structures as well as small domains. This trend is a result of repulsive ionic forces between adjacent ions, weakened due to screening by the surrounding water molecules. Using high resolution conductive atomic force microscopy maps, the local conductance of the graphene is measured, revealing a direct correlation between the K + distribution and the structure of the ice layer. Our results shed light on the local distribution of ions on the air-cleaved mica, solving a long-standing enigma. They also provide a detailed understanding of charge transfer from the ionic domains towards graphene.

Diffusing colloidal probes of protein-carbohydrate interactions.

PubMed

Eichmann, Shannon L; Meric, Gulsum; Swavola, Julia C; Bevan, Michael A

2013-02-19

We present diffusing colloidal probe measurements of weak, multivalent, specific protein-polysaccharide interactions mediated by a competing monosaccharide. Specifically, we used integrated evanescent wave and video microscopy methods to monitor the three-dimensional Brownian excursions of conconavilin A (ConA) decorated colloids interacting with dextran-functionalized surfaces in the presence of glucose. Particle trajectories were interpreted as binding lifetime histograms, binding isotherms, and potentials of mean force. Binding lifetimes and isotherms showed clear trends of decreasing ConA-dextran-specific binding with increasing glucose concentration, consistent with expectations. Net potentials were accurately captured by superposition of a short-range, glucose-independent ConA-dextran repulsion and a longer-range, glucose-dependent dextran bridging attraction modeled as a harmonic potential. For glucose concentrations greater than 100 mM, the net ConA-dextran potential was found to have only a nonspecific repulsion, similar to that of bovine serum albumin (BSA) decorated colloids over dextran determined in control experiments. Our results demonstrate the first use of optical microscopy methods to quantify the connections between potentials of mean force and the binding behavior of ConA-decorated colloids on dextran-functionalized surfaces.

Investigation of the surface potential of TiO2 (110) by frequency-modulation Kelvin probe force microscopy

NASA Astrophysics Data System (ADS)

Kou, Lili; Li, Yan Jun; Kamijyo, Takeshi; Naitoh, Yoshitaka; Sugawara, Yasuhiro

2016-12-01

We investigate the surface potential distribution on a TiO2 (110)-1 × 1 surface by Kelvin probe force microscopy (KPFM) and atom-dependent bias-distance spectroscopic mapping. The experimental results demonstrate that the local contact potential difference increases on twofold-coordinated oxygen sites, and decreases on OH defects and fivefold-coordinated Ti sites. We propose a qualitative model to explain the origin of the surface potential of TiO2 (110). We qualitatively calculate the surface potential induced by chemical potential and permanent surface dipole. The calculated results agree with our experimental ones. Therefore, we suggest that the surface potential of TiO2 (110) is dominated not only by the permanent surface dipole between the tip apex atom and surface, but also by the dipoles induced by the chemical interaction between the tip and sample. The KPFM technique demonstrate the possibility of investigation of the charge transfer phenomenon on TiO2 surface under gas conditions. It is useful for the elucidation of the mechanism of the catalytic reactions.

Investigation of the surface potential of TiO2 (110) by frequency-modulation Kelvin probe force microscopy.

PubMed

Kou, Lili; Li, Yan Jun; Kamijyo, Takeshi; Naitoh, Yoshitaka; Sugawara, Yasuhiro

2016-12-16

We investigate the surface potential distribution on a TiO 2 (110)-1 × 1 surface by Kelvin probe force microscopy (KPFM) and atom-dependent bias-distance spectroscopic mapping. The experimental results demonstrate that the local contact potential difference increases on twofold-coordinated oxygen sites, and decreases on OH defects and fivefold-coordinated Ti sites. We propose a qualitative model to explain the origin of the surface potential of TiO 2 (110). We qualitatively calculate the surface potential induced by chemical potential and permanent surface dipole. The calculated results agree with our experimental ones. Therefore, we suggest that the surface potential of TiO 2 (110) is dominated not only by the permanent surface dipole between the tip apex atom and surface, but also by the dipoles induced by the chemical interaction between the tip and sample. The KPFM technique demonstrate the possibility of investigation of the charge transfer phenomenon on TiO 2 surface under gas conditions. It is useful for the elucidation of the mechanism of the catalytic reactions.

Direct assessment of p-n junctions in single GaN nanowires by Kelvin probe force microscopy

NASA Astrophysics Data System (ADS)

Minj, Albert; Cros, Ana; Auzelle, Thomas; Pernot, Julien; Daudin, Bruno

2016-09-01

Making use of Kelvin probe force microscopy, in dark and under ultraviolet illumination, we study the characteristics of p-n junctions formed along the axis of self-organized GaN nanowires (NWs). We map the contact potential difference of the single NW p-n junctions to locate the space charge region and directly measure the depletion width and the junction voltage. Simulations indicate a shrinkage of the built-in potential for NWs with small diameter due to surface band bending, in qualitative agreement with the measurements. The photovoltage of the NW/substrate contact is studied by analyzing the response of NW segments with p- and n-type doping under illumination. Our results show that the shifts of the Fermi levels, and not the changes in surface band bending, are the most important effects under above band-gap illumination. The quantitative electrical information obtained here is important for the use of NW p-n junctions as photovoltaic or rectifying devices at the nanoscale, and is especially relevant since the technique does not require the formation of ohmic contacts to the NW junction.

Exploring Anomalous Polarization Dynamics in Organometallic Halide Perovskites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ahmadi, Mahshid; Collins, Liam; Puretzky, Alexander

Organometallic halide perovskites (OMHPs) have attracted broad attention as prospective materials for optoelectronic applications. Among the many anomalous properties of these materials, of special interest are the ferroelectric properties including both classical and relaxor-like components, as a potential origin of slow dynamics, field enhancement, and anomalous mobilities. Here, ferroelectric properties of the three representative OMHPs are explored, including FAPb xSn 1–xI 3 (x = 0, x = 0.85) and FA 0.85MA 0.15PbI 3 using band excitation piezoresponse force microscopy and contact mode Kelvin probe force microscopy, providing insight into long- and short-range dipole and charge dynamics in these materials andmore » probing ferroelectric density of states. Furthermore, second-harmonic generation in thin films of OMHPs is observed, providing a direct information on the noncentrosymmetric polarization in such materials. Overall, the data provide strong evidence for the presence of ferroelectric domains in these systems; however, the domain dynamics is suppressed by fast ion dynamics. These materials hence present the limit of ferroelectric materials with spontaneous polarization dynamically screened by ionic and electronic carriers.« less

EDITORIAL: Nanoscale metrology Nanoscale metrology

NASA Astrophysics Data System (ADS)

Klapetek, P.; Koenders, L.

2011-09-01

This special issue of Measurement Science and Technology presents selected contributions from the NanoScale 2010 seminar held in Brno, Czech Republic. It was the 5th Seminar on Nanoscale Calibration Standards and Methods and the 9th Seminar on Quantitative Microscopy (the first being held in 1995). The seminar was jointly organized with the Czech Metrology Institute (CMI) and the Nanometrology Group of the Technical Committee-Length of EURAMET. There were two workshops that were integrated into NanoScale 2010: first a workshop presenting the results obtained in NANOTRACE, a European Metrology Research Project (EMRP) on displacement-measuring optical interferometers, and second a workshop about the European metrology landscape in nanometrology related to thin films, scanning probe microscopy and critical dimension. The aim of this workshop was to bring together developers, applicants and metrologists working in this field of nanometrology and to discuss future needs. For more information see www.co-nanomet.eu. The articles in this special issue of Measurement Science and Technology cover some novel scientific results. This issue can serve also as a representative selection of topics that are currently being investigated in the field of European and world-wide nanometrology. Besides traditional topics of dimensional metrology, like development of novel interferometers or laser stabilization techniques, some novel interesting trends in the field of nanometrology are observed. As metrology generally reflects the needs of scientific and industrial research, many research topics addressed refer to current trends in nanotechnology, too, focusing on traceability and improved measurement accuracy in this field. While historically the most studied standards in nanometrology were related to simple geometric structures like step heights or 1D or 2D gratings, now we are facing tasks to measure 3D structures and many unforeseen questions arising from interesting physical properties of nanoparticles, nanotubes, quantum dots and similar fascinating objects. Currently there is a high level of interest in characterization of nanoparticles since they are increasingly encountered in science, technology, life sciences and even everyday life. Quantitative characterization of nanoparticles has been the subject of many discussions and some recent work over the last couple of years, and both scanning probe microscopy and scanning or transmission electron microscopy characterization of nanoparticles are presented here. There is also a continuous need for improvement of scanning probe microscopy that is a basic tool for nanometrology. Increasing thermal stability, scanning speed and tip stability, improving traceability and reducing uncertainty are all areas being addressed. As scanning probe microscopy is essentially based on force measurements in the nano- and piconewton range, we take notice of large developments, both theoretical and experimental, in the field of traceable measurements of nanoscale forces. This will greatly increase the understanding and quantification of many basic phenomena in scanning probe microscopy. Finally, we observe that high resolution techniques for acquiring more than just morphology are slowly shifting from purely qualitative tools to well defined quantitative methods. Lack of simple and reliable chemical identification in scanning probe microscopy is compensated by many other local probing methods seen in commercial microscopes, like scanning thermal microscopy or the Kelvin probe technique. All these methods still require underpinning with theoretical and experimental work before they can become traceable analytical methods; however, the increased interest in the metrology community gives rise to optimism in this field. The production of this issue involved considerable effort from many contributors. We would like to thank all the authors for their contributions, the referees for their time spent reviewing the contributions and their valuable comments, and the whole Editorial Board of Measurement Science and Technology for their support.

Three-dimensional nanoscale imaging by plasmonic Brownian microscopy

NASA Astrophysics Data System (ADS)

Labno, Anna; Gladden, Christopher; Kim, Jeongmin; Lu, Dylan; Yin, Xiaobo; Wang, Yuan; Liu, Zhaowei; Zhang, Xiang

2017-12-01

Three-dimensional (3D) imaging at the nanoscale is a key to understanding of nanomaterials and complex systems. While scanning probe microscopy (SPM) has been the workhorse of nanoscale metrology, its slow scanning speed by a single probe tip can limit the application of SPM to wide-field imaging of 3D complex nanostructures. Both electron microscopy and optical tomography allow 3D imaging, but are limited to the use in vacuum environment due to electron scattering and to optical resolution in micron scales, respectively. Here we demonstrate plasmonic Brownian microscopy (PBM) as a way to improve the imaging speed of SPM. Unlike photonic force microscopy where a single trapped particle is used for a serial scanning, PBM utilizes a massive number of plasmonic nanoparticles (NPs) under Brownian diffusion in solution to scan in parallel around the unlabeled sample object. The motion of NPs under an evanescent field is three-dimensionally localized to reconstruct the super-resolution topology of 3D dielectric objects. Our method allows high throughput imaging of complex 3D structures over a large field of view, even with internal structures such as cavities that cannot be accessed by conventional mechanical tips in SPM.

Moving towards the magnetoelectric graphene transistor

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cao, Shi; Xiao, Zhiyong; Kwan, Chun -Pui

Here, the interfacial charge transfer between mechanically exfoliated few-layer graphene and Cr 2O 3 (0001) surfaces has been investigated. Electrostatic force microscopy and Kelvin probe force microscopy studies point to hole doping of few-layer graphene, with up to a 150 meV shift in the Fermi level, an aspect that is confirmed by Raman spectroscopy. Density functional theory calculations furthermore confirm the p-type nature of the graphene/chromia interface and suggest that the chromia is able to induce a significant carrier spin polarization in the graphene layer. A large magnetoelectrically controlled magneto-resistance can therefore be anticipated in transistor structures based on thismore » system, a finding important for developing graphene-based spintronic applications.« less

KPFM/AFM imaging on TiO2(110) surface in O2 gas

NASA Astrophysics Data System (ADS)

Arima, Eiji; Wen, Huan Fei; Naitoh, Yoshitaka; Li, Yan Jun; Sugawara, Yasuhiro

2018-03-01

We have carried out high-speed imaging of the topography and local contact potential difference (LCPD) on rutile TiO2(110) in O2 gas by atomic force microscopy (AFM) and Kelvin probe force microscopy (KPFM). We succeeded in KPFM/AFM imaging with atomic resolution at 1 frame min-1 and observed the adsorbate on a hydroxylated TiO2(110) surface. The observed adsorbate is considered to be oxygen adatoms (Oa), hydroperoxyls (HO2), or terminal hydroxyls (OHt). After adsorption, changes in the topography and the LCPD of the adsorbate were observed. This phenomenon is thought to be caused by the charge transfer of the adsorbate. This technique has the potential to observe catalytic behavior with atomic resolution.

Moving towards the magnetoelectric graphene transistor

DOE PAGES

Cao, Shi; Xiao, Zhiyong; Kwan, Chun -Pui; ...

2017-10-30

Here, the interfacial charge transfer between mechanically exfoliated few-layer graphene and Cr 2O 3 (0001) surfaces has been investigated. Electrostatic force microscopy and Kelvin probe force microscopy studies point to hole doping of few-layer graphene, with up to a 150 meV shift in the Fermi level, an aspect that is confirmed by Raman spectroscopy. Density functional theory calculations furthermore confirm the p-type nature of the graphene/chromia interface and suggest that the chromia is able to induce a significant carrier spin polarization in the graphene layer. A large magnetoelectrically controlled magneto-resistance can therefore be anticipated in transistor structures based on thismore » system, a finding important for developing graphene-based spintronic applications.« less

Combined low-temperature scanning tunneling/atomic force microscope for atomic resolution imaging and site-specific force spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Schwarz, Udo; Albers, Boris J.; Liebmann, Marcus

2008-02-27

The authors present the design and first results of a low-temperature, ultrahigh vacuum scanning probe microscope enabling atomic resolution imaging in both scanning tunneling microscopy (STM) and noncontact atomic force microscopy (NC-AFM) modes. A tuning-fork-based sensor provides flexibility in selecting probe tip materials, which can be either metallic or nonmetallic. When choosing a conducting tip and sample, simultaneous STM/NC-AFM data acquisition is possible. Noticeable characteristics that distinguish this setup from similar systems providing simultaneous STM/NC-AFM capabilities are its combination of relative compactness (on-top bath cryostat needs no pit), in situ exchange of tip and sample at low temperatures, short turnaroundmore » times, modest helium consumption, and unrestricted access from dedicated flanges. The latter permits not only the optical surveillance of the tip during approach but also the direct deposition of molecules or atoms on either tip or sample while they remain cold. Atomic corrugations as low as 1 pm could successfully be resolved. In addition, lateral drifts rates of below 15 pm/h allow long-term data acquisition series and the recording of site-specific spectroscopy maps. Results obtained on Cu(111) and graphite illustrate the microscope's performance.« less

Research on the Sensing Performance of the Tuning Fork-Probe as a Micro Interaction Sensor

PubMed Central

Gao, Fengli; Li, Xide

2015-01-01

The shear force position system has been widely used in scanning near-field optical microscopy (SNOM) and recently extended into the force sensing area. The dynamic properties of a tuning fork (TF), the core component of this system, directly determine the sensing performance of the shear positioning system. Here, we combine experimental results and finite element method (FEM) analysis to investigate the dynamic behavior of the TF probe assembled structure (TF-probe). Results from experiments under varying atmospheric pressures illustrate that the oscillation amplitude of the TF-probe is linearly related to the quality factor, suggesting that decreasing the pressure will dramatically increase the quality factor. The results from FEM analysis reveal the influences of various parameters on the resonant performance of the TF-probe. We compared numerical results of the frequency spectrum with the experimental data collected by our recently developed laser Doppler vibrometer system. Then, we investigated the parameters affecting spatial resolution of the SNOM and the dynamic response of the TF-probe under longitudinal and transverse interactions. It is found that the interactions in transverse direction is much more sensitive than that in the longitudinal direction. Finally, the TF-probe was used to measure the friction coefficient of a silica–silica interface. PMID:26404310

Resonant difference-frequency atomic force ultrasonic microscope

NASA Technical Reports Server (NTRS)

Cantrell, John H. (Inventor); Cantrell, Sean A. (Inventor)

2010-01-01

A scanning probe microscope and methodology called resonant difference-frequency atomic force ultrasonic microscopy (RDF-AFUM), employs an ultrasonic wave launched from the bottom of a sample while the cantilever of an atomic force microscope, driven at a frequency differing from the ultrasonic frequency by one of the contact resonance frequencies of the cantilever, engages the sample top surface. The nonlinear mixing of the oscillating cantilever and the ultrasonic wave in the region defined by the cantilever tip-sample surface interaction force generates difference-frequency oscillations at the cantilever contact resonance. The resonance-enhanced difference-frequency signals are used to create images of nanoscale near-surface and subsurface features.

Precise Orientation of a Single C60 Molecule on the Tip of a Scanning Probe Microscope

NASA Astrophysics Data System (ADS)

Chiutu, C.; Sweetman, A. M.; Lakin, A. J.; Stannard, A.; Jarvis, S.; Kantorovich, L.; Dunn, J. L.; Moriarty, P.

2012-06-01

We show that the precise orientation of a C60 molecule which terminates the tip of a scanning probe microscope can be determined with atomic precision from submolecular contrast images of the fullerene cage. A comparison of experimental scanning tunneling microscopy data with images simulated using computationally inexpensive Hückel theory provides a robust method of identifying molecular rotation and tilt at the end of the probe microscope tip. Noncontact atomic force microscopy resolves the atoms of the C60 cage closest to the surface for a range of molecular orientations at tip-sample separations where the molecule-substrate interaction potential is weakly attractive. Measurements of the C60C60 pair potential acquired using a fullerene-terminated tip are in excellent agreement with theoretical predictions based on a pairwise summation of the van der Waals interactions between C atoms in each cage, i.e., the Girifalco potential [L. Girifalco, J. Phys. Chem. 95, 5370 (1991)JPCHAX0022-365410.1021/j100167a002].

Self-sensing cantilevers with integrated conductive coaxial tips for high-resolution electrical scanning probe metrology

DOE Office of Scientific and Technical Information (OSTI.GOV)

Haemmerli, Alexandre J.; Pruitt, Beth L., E-mail: pruitt@stanford.edu; Harjee, Nahid

The lateral resolution of many electrical scanning probe techniques is limited by the spatial extent of the electrostatic potential profiles produced by their probes. Conventional unshielded conductive atomic force microscopy probes produce broad potential profiles. Shielded probes could offer higher resolution and easier data interpretation in the study of nanostructures. Electrical scanning probe techniques require a method of locating structures of interest, often by mapping surface topography. As the samples studied with these techniques are often photosensitive, the typical laser measurement of cantilever deflection can excite the sample, causing undesirable changes electrical properties. In this work, we present the design,more » fabrication, and characterization of probes that integrate coaxial tips for spatially sharp potential profiles with piezoresistors for self-contained, electrical displacement sensing. With the apex 100 nm above the sample surface, the electrostatic potential profile produced by our coaxial tips is more than 2 times narrower than that of unshielded tips with no long tails. In a scan bandwidth of 1 Hz–10 kHz, our probes have a displacement resolution of 2.9 Å at 293 K and 79 Å at 2 K, where the low-temperature performance is limited by amplifier noise. We show scanning gate microscopy images of a quantum point contact obtained with our probes, highlighting the improvement to lateral resolution resulting from the coaxial tip.« less

Mechanical manipulation of magnetic nanoparticles by magnetic force microscopy

NASA Astrophysics Data System (ADS)

Liu, Jinyun; Zhang, Wenxiao; Li, Yiquan; Zhu, Hanxing; Qiu, Renxi; Song, Zhengxun; Wang, Zuobin; Li, Dayou

2017-12-01

A method has been developed in this work for the mechanical manipulation of magnetic nanoparticles (MNPs). A helical curve was designed as the capture path to pick up and remove the target nanoparticle on a mica surface by a magnetic probe based on the magnetic force microscope (MFM). There were magnetic, tangential and pushing forces acting on the target particle during the approaching process when the tip followed the helical curve as the capture path. The magnetic force was significant when the tip was closer to the particle. The target particle can be attached on the surface of the magnetic probe tip and then be picked up after the tip retracted from the mica surface. Theoretical analysis and experimental results were presented for the pick-up and removal of MNPs. With this method, the precision and flexibility of manipulation of MNPs were improved significantly compared to the pushing or sliding of the target object away from the corresponding original location following a planned path.

Atomic force microscopy of biological samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Doktycz, Mitchel John

2010-01-01

The ability to evaluate structural-functional relationships in real time has allowed scanning probe microscopy (SPM) to assume a prominent role in post genomic biological research. In this mini-review, we highlight the development of imaging and ancillary techniques that have allowed SPM to permeate many key areas of contemporary research. We begin by examining the invention of the scanning tunneling microscope (STM) by Binnig and Rohrer in 1982 and discuss how it served to team biologists with physicists to integrate high-resolution microscopy into biological science. We point to the problems of imaging nonconductive biological samples with the STM and relate howmore » this led to the evolution of the atomic force microscope (AFM) developed by Binnig, Quate, and Gerber, in 1986. Commercialization in the late 1980s established SPM as a powerful research tool in the biological research community. Contact mode AFM imaging was soon complemented by the development of non-contact imaging modes. These non-contact modes eventually became the primary focus for further new applications including the development of fast scanning methods. The extreme sensitivity of the AFM cantilever was recognized and has been developed into applications for measuring forces required for indenting biological surfaces and breaking bonds between biomolecules. Further functional augmentation to the cantilever tip allowed development of new and emerging techniques including scanning ion-conductance microscopy (SICM), scanning electrochemical microscope (SECM), Kelvin force microscopy (KFM) and scanning near field ultrasonic holography (SNFUH).« less

Quadratic electromechanical strain in silicon investigated by scanning probe microscopy

NASA Astrophysics Data System (ADS)

Yu, Junxi; Esfahani, Ehsan Nasr; Zhu, Qingfeng; Shan, Dongliang; Jia, Tingting; Xie, Shuhong; Li, Jiangyu

2018-04-01

Piezoresponse force microscopy (PFM) is a powerful tool widely used to characterize piezoelectricity and ferroelectricity at the nanoscale. However, it is necessary to distinguish microscopic mechanisms between piezoelectricity and non-piezoelectric contributions measured by PFM. In this work, we systematically investigate the first and second harmonic apparent piezoresponses of a silicon wafer in both vertical and lateral modes, and we show that it exhibits an apparent electromechanical response that is quadratic to the applied electric field, possibly arising from ionic electrochemical dipoles induced by the charged probe. As a result, the electromechanical response measured is dominated by the second harmonic response in the vertical mode, and its polarity can be switched by the DC voltage with the evolving coercive field and maximum amplitude, in sharp contrast to typical ferroelectric materials we used as control. The ionic activity in silicon is also confirmed by the scanning thermo-ionic microscopy measurement, and the work points toward a set of methods to distinguish true piezoelectricity from the apparent ones.

Nanoscale chemical imaging by photoinduced force microscopy

PubMed Central

Nowak, Derek; Morrison, William; Wickramasinghe, H. Kumar; Jahng, Junghoon; Potma, Eric; Wan, Lei; Ruiz, Ricardo; Albrecht, Thomas R.; Schmidt, Kristin; Frommer, Jane; Sanders, Daniel P.; Park, Sung

2016-01-01

Correlating spatial chemical information with the morphology of closely packed nanostructures remains a challenge for the scientific community. For example, supramolecular self-assembly, which provides a powerful and low-cost way to create nanoscale patterns and engineered nanostructures, is not easily interrogated in real space via existing nondestructive techniques based on optics or electrons. A novel scanning probe technique called infrared photoinduced force microscopy (IR PiFM) directly measures the photoinduced polarizability of the sample in the near field by detecting the time-integrated force between the tip and the sample. By imaging at multiple IR wavelengths corresponding to absorption peaks of different chemical species, PiFM has demonstrated the ability to spatially map nm-scale patterns of the individual chemical components of two different types of self-assembled block copolymer films. With chemical-specific nanometer-scale imaging, PiFM provides a powerful new analytical method for deepening our understanding of nanomaterials. PMID:27051870

Probing the Mechanical Properties of Plasma von Willebrand Factor Using Atomic Force Microscopy

NASA Astrophysics Data System (ADS)

Wijeratne, Sitara; Botello, Eric; Frey, Eric; Kiang, Ching-Hwa; Dong, Jing-Fei; Yeh, Hui-Chun

2010-03-01

Single-molecule manipulation allows us to study the real time kinetics of many complex cellular processes. The mechanochemistry of different forms of von Willebrand factor (VWF) and their receptor-ligand binding kinetics can be unraveled by atomic force microscopy (AFM). Since plasma VWF can be activated upon shear, the structural and functional properties of VWF are critical in mediating thrombus formation become important. Here we characterized the mechanical resistance to domain unfolding of VWF to determine the conformational states of VWF. We found the shear induced conformational, hence mechanical property changes can be detected by the change in unfolding forces. The relaxation rate of such effect is much longed than expected. This supports the model of lateral association VWF under shear stress. Our results offer an insight in establishing strategies for regulating VWF adhesion activity, increasing our understanding of surface-induced thrombosis as mediated by VWF.

Accurate formula for dissipative interaction in frequency modulation atomic force microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Suzuki, Kazuhiro; Matsushige, Kazumi; Yamada, Hirofumi

2014-12-08

Much interest has recently focused on the viscosity of nano-confined liquids. Frequency modulation atomic force microscopy (FM-AFM) is a powerful technique that can detect variations in the conservative and dissipative forces between a nanometer-scale tip and a sample surface. We now present an accurate formula to convert the dissipation power of the cantilever measured during the experiment to damping of the tip-sample system. We demonstrated the conversion of the dissipation power versus tip-sample separation curve measured using a colloidal probe cantilever on a mica surface in water to the damping curve, which showed a good agreement with the theoretical curve.more » Moreover, we obtained the damping curve from the dissipation power curve measured on the hydration layers on the mica surface using a nanometer-scale tip, demonstrating that the formula allows us to quantitatively measure the viscosity of a nano-confined liquid using FM-AFM.« less

Evaluating the potential energy landscape over single molecules at room temperature with lateral force microscopy

NASA Astrophysics Data System (ADS)

Weymouth, Alfred J.; Riegel, Elisabeth; Matencio, Sonia; Giessibl, Franz J.

2018-04-01

One of the challenges of AFM, in contrast to STM, is that the measured signal includes both long-range and short-range components. The most accurate method for removing long-range components is to measure both on and off an adsorbate and to subtract the difference. This on-off method is challenging at room temperature due to thermal drift. By moving to a non-contact scheme in which the lateral component of the force interaction is probed, the measurement is dominated by short-range interactions. We use frequency-modulation lateral force microscopy to measure individual PTCDA molecules adsorbed on Ag/Si(111)-( √{3 }×√{3 } ). By fitting the data to a model potential, we can extract the depth and width of the potential. When the tip is closer to the sample, a repulsive feature can be observed in the data.

Fast time-resolved electrostatic force microscopy: Achieving sub-cycle time resolution

DOE Office of Scientific and Technical Information (OSTI.GOV)

Karatay, Durmus U.; Harrison, Jeffrey S.; Glaz, Micah S.

The ability to measure microsecond- and nanosecond-scale local dynamics below the diffraction limit with widely available atomic force microscopy hardware would enable new scientific studies in fields ranging from biology to semiconductor physics. However, commercially available scanning-probe instruments typically offer the ability to measure dynamics only on time scales of milliseconds to seconds. Here, we describe in detail the implementation of fast time-resolved electrostatic force microscopy using an oscillating cantilever as a means to measure fast local dynamics following a perturbation to a sample. We show how the phase of the oscillating cantilever relative to the perturbation event is criticalmore » to achieving reliable sub-cycle time resolution. We explore how noise affects the achievable time resolution and present empirical guidelines for reducing noise and optimizing experimental parameters. Specifically, we show that reducing the noise on the cantilever by using photothermal excitation instead of piezoacoustic excitation further improves time resolution. We demonstrate the discrimination of signal rise times with time constants as fast as 10 ns, and simultaneous data acquisition and analysis for dramatically improved image acquisition times.« less

Quantitative measurement of solvation shells using frequency modulated atomic force microscopy

NASA Astrophysics Data System (ADS)

Uchihashi, T.; Higgins, M.; Nakayama, Y.; Sader, J. E.; Jarvis, S. P.

2005-03-01

The nanoscale specificity of interaction measurements and additional imaging capability of the atomic force microscope make it an ideal technique for measuring solvation shells in a variety of liquids next to a range of materials. Unfortunately, the widespread use of atomic force microscopy for the measurement of solvation shells has been limited by uncertainties over the dimensions, composition and durability of the tip during the measurements, and problems associated with quantitative force calibration of the most sensitive dynamic measurement techniques. We address both these issues by the combined use of carbon nanotube high aspect ratio probes and quantifying the highly sensitive frequency modulation (FM) detection technique using a recently developed analytical method. Due to the excellent reproducibility of the measurement technique, additional information regarding solvation shell size as a function of proximity to the surface has been obtained for two very different liquids. Further, it has been possible to identify differences between chemical and geometrical effects in the chosen systems.

[Atomic force microscopy: a tool to analyze the viral cycle].

PubMed

Bernaud, Julien; Castelnovo, Martin; Muriaux, Delphine; Faivre-Moskalenko, Cendrine

2015-05-01

Each step of the HIV-1 life cycle frequently involves a change in the morphology and/or mechanical properties of the viral particle or core. The atomic force microscope (AFM) constitutes a powerful tool for characterizing these physical changes at the scale of a single virus. Indeed, AFM enables the visualization of viral capsids in a controlled physiological environment and to probe their mechanical properties by nano-indentation. Finally, AFM force spectroscopy allows to characterize the affinities between viral envelope proteins and cell receptors at the single molecule level. © 2015 médecine/sciences – Inserm.

Nanoscale Subsurface Imaging via Resonant Difference-Frequency Atomic Force Ultrasonic Microscopy

NASA Technical Reports Server (NTRS)

Cantrell, Sean A.; Cantrell, John H.; Lilehei, Peter T.

2007-01-01

A novel scanning probe microscope methodology has been developed that employs an ultrasonic wave launched from the bottom of a sample while the cantilever of an atomic force microscope, driven at a frequency differing from the ultrasonic frequency by the fundamental resonance frequency of the cantilever, engages the sample top surface. The nonlinear mixing of the oscillating cantilever and the ultrasonic wave in the region defined by the cantilever tip-sample surface interaction force generates difference-frequency oscillations at the cantilever fundamental resonance. The resonance-enhanced difference-frequency signals are used to create images of embedded nanoscale features.

Application of focused ion beam for the fabrication of AFM probes

NASA Astrophysics Data System (ADS)

Kolomiytsev, A. S.; Lisitsyn, S. A.; Smirnov, V. A.; Fedotov, A. A.; Varzarev, Yu N.

2017-10-01

The results of an experimental study of the probe tips fabrication for critical-dimension atomic force microscopy (CD-AFM) using the focused ion beam (FIB) induced deposition are presented. Methods of the FIB-induced deposition of tungsten and carbon onto the tip of an AFM probe are studied. Based on the results obtained in the study, probes for the CD-AFM technique with a tip height about 1 μm and radius of 20 nm were created. The formation of CD-AFM probes by FIB-induced deposition allows creating a high efficiency tool for nanotechnology and nanodiagnostics. The use of modified cantilevers allows minimizing the artefacts of AFM images and increasing the accuracy of the relief measurement. The obtained results can be used for fabrication of AFM probes for express monitoring of the technological process in the manufacturing of the elements for micro- and nanoelectronics.

Note: Compact and light displacement sensor for a precision measurement system in large motion

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lee, Sang Heon, E-mail: shlee@andong.ac.kr

We developed a compact and light displacement sensor applicable to systems that require wide range motions of its sensing device. The proposed sensor utilized the optical pickup unit of the optical disk drive, which has been used applied to atomic force microscopy (AFM) because of its compactness and lightness as well as its high performance. We modified the structure of optical pickup unit and made the compact sensor driver attachable to a probe head of AFM to make large rotation. The feasibilities of the developed sensor for a general probe-moving measurement device and for probe-rotating AFM were verified. Moreover, amore » simple and precise measurement of alignment between centers of rotator and probe tip in probe-rotation AFM was experimentally demonstrated using the developed sensor.« less

Nanofabrication of insulated scanning probes for electromechanical imaging in liquid solutions

PubMed Central

Noh, Joo Hyon; Nikiforov, Maxim; Kalinin, Sergei V.; Vertegel, Alexey A.; Rack, Philip D.

2011-01-01

In this paper, the fabrication and electrical and electromechanical characterization of insulated scanning probes have been demonstrated in liquid solutions. The silicon cantilevers were sequentially coated with chromium and silicon dioxide, and the silicon dioxide was selectively etched at tip apex using focused electron beam induced etching (FEBIE) with XeF2 The chromium layer acted not only as the conductive path from the tip, but also as an etch resistant layer. This insulated scanning probe fabrication process is compatible with any commercial AFM tip and can be used to easily tailor the scanning probe tip properties because FEBIE does not require lithography. The suitability of the fabricated probes is demonstrated by imaging of standard topographical calibration grid as well as piezoresponse force microscopy (PFM) and electrical measurements in ambient and liquid environments. PMID:20702930

Imaging and three-dimensional reconstruction of chemical groups inside a protein complex using atomic force microscopy

NASA Astrophysics Data System (ADS)

Kim, Duckhoe; Sahin, Ozgur

2015-03-01

Scanning probe microscopes can be used to image and chemically characterize surfaces down to the atomic scale. However, the localized tip-sample interactions in scanning probe microscopes limit high-resolution images to the topmost atomic layer of surfaces, and characterizing the inner structures of materials and biomolecules is a challenge for such instruments. Here, we show that an atomic force microscope can be used to image and three-dimensionally reconstruct chemical groups inside a protein complex. We use short single-stranded DNAs as imaging labels that are linked to target regions inside a protein complex, and T-shaped atomic force microscope cantilevers functionalized with complementary probe DNAs allow the labels to be located with sequence specificity and subnanometre resolution. After measuring pairwise distances between labels, we reconstruct the three-dimensional structure formed by the target chemical groups within the protein complex using simple geometric calculations. Experiments with the biotin-streptavidin complex show that the predicted three-dimensional loci of the carboxylic acid groups of biotins are within 2 Å of their respective loci in the corresponding crystal structure, suggesting that scanning probe microscopes could complement existing structural biological techniques in solving structures that are difficult to study due to their size and complexity.

Tunneling magnetic force microscopy

NASA Technical Reports Server (NTRS)

Burke, Edward R.; Gomez, Romel D.; Adly, Amr A.; Mayergoyz, Isaak D.

1993-01-01

We have developed a powerful new tool for studying the magnetic patterns on magnetic recording media. This was accomplished by modifying a conventional scanning tunneling microscope. The fine-wire probe that is used to image surface topography was replaced with a flexible magnetic probe. Images obtained with these probes reveal both the surface topography and the magnetic structure. We have made a thorough theoretical analysis of the interaction between the probe and the magnetic fields emanating from a typical recorded surface. Quantitative data about the constituent magnetic fields can then be obtained. We have employed these techniques in studies of two of the most important issues of magnetic record: data overwrite and maximizing data-density. These studies have shown: (1) overwritten data can be retrieved under certain conditions; and (2) improvements in data-density will require new magnetic materials. In the course of these studies we have developed new techniques to analyze magnetic fields of recorded media. These studies are both theoretical and experimental and combined with the use of our magnetic force scanning tunneling microscope should lead to further breakthroughs in the field of magnetic recording.

Nanomechanical and topographical imaging of living cells by atomic force microscopy with colloidal probes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Puricelli, Luca; Galluzzi, Massimiliano; Schulte, Carsten

Atomic Force Microscopy (AFM) has a great potential as a tool to characterize mechanical and morphological properties of living cells; these properties have been shown to correlate with cells’ fate and patho-physiological state in view of the development of novel early-diagnostic strategies. Although several reports have described experimental and technical approaches for the characterization of cellular elasticity by means of AFM, a robust and commonly accepted methodology is still lacking. Here, we show that micrometric spherical probes (also known as colloidal probes) are well suited for performing a combined topographic and mechanical analysis of living cells, with spatial resolution suitablemore » for a complete and accurate mapping of cell morphological and elastic properties, and superior reliability and accuracy in the mechanical measurements with respect to conventional and widely used sharp AFM tips. We address a number of issues concerning the nanomechanical analysis, including the applicability of contact mechanical models and the impact of a constrained contact geometry on the measured Young’s modulus (the finite-thickness effect). We have tested our protocol by imaging living PC12 and MDA-MB-231 cells, in order to demonstrate the importance of the correction of the finite-thickness effect and the change in Young’s modulus induced by the action of a cytoskeleton-targeting drug.« less

Carbon nanotube scanning probe for imaging in aqueous environment

NASA Technical Reports Server (NTRS)

Stevens, Ramsey M.; Nguyen, Cattien V.; Meyyappan, M.

2004-01-01

Carbon nanotubes (CNTs) used as a probe for scanning probe microscopy has become one of the many potential usages of CNTs that is finding real applications in scientific research and industrial communities. It has been proposed that the unique mechanical buckling properties of the CNT would lessen the imaging force exerted on the sample and, thus, make CNT scanning probes ideal for imaging soft materials, including biological samples in liquid environments. The hydrophobic nature of the CNT graphitic sidewall is clearly chemically incompatible with the aqueous solution requirements in some biological imaging applications. In this paper, we present electron micrograph results demonstrating the instability of CNT scanning probes when submerged in aqueous solution. Moreover, we also introduce a novel approach to resolve this chemical incompatibility problem. By coating the CNT probe with ethylenediamine, thus rendering the CNT probe less hydrophobic, we demonstrate the liquid imaging capability of treated CNT probes. Experimental data for imaging in aqueous solutions are presented, which include an ultrathin Ir film and DNA molecules on a mica surface.

Electrochemical and scanning probe microscopic characterization of spontaneously adsorbed organothiolate monolayers at gold

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wong, Sze-Shun Season

1999-12-10

This dissertation presented several results which add to the general knowledge base regarding organothiolates monolayer spontaneously adsorbed at gold films. Common to the body of this work is the use of voltammetric reductive resorption and variants of scanning probe microscopy to gain insight into the nature of the monolayer formation process as well as the resulting interface. The most significant result from this work is the success of using friction force microscopy to discriminate the end group orientation of monolayer chemisorbed at smooth gold surfaces with micrometer resolution (Chapter 4). The ability to detect the differences in the orientational dispositionmore » is demonstrated by the use PDMS polymer stamp to microcontact print an adlayer of n-alkanethiolate of length n in a predefine pattern onto a gold surface, followed by the solution deposition of a n-alkanethiol of n ± 1 to fill in the areas on the gold surface intentionally not coated by the stamping process. These two-component monolayers can be discriminated by using friction force microscopy which detects differences in friction contributed by the differences in the orientation of the terminal groups at surfaces. This success has recently led to the detection of the orientation differences at nanometer scale. Although the substrates examined in this work consisted entirely of smooth gold films, the same test can be performed on other smooth substrates and monolayer materials.« less

Nanoscale investigation of the piezoelectric properties of perovskite ferroelectrics and III-nitrides

NASA Astrophysics Data System (ADS)

Rodriguez, Brian Joseph

Nanoscale characterization of the piezoelectric and polarization related properties of III-Nitrides by piezoresponse force microscopy (PFM), electrostatic force microscopy (EFM) and scanning Kelvin probe microscopy (SKPM) resulted in the measurement of piezoelectric constants, surface charge and surface potential. Photo-electron emission microscopy (PEEM) was used to determine the local electronic band structure of a GaN-based lateral polarity heterostructure (GaN-LPH). Nanoscale characterization of the imprint and switching behavior of ferroelectric thin films by PFM resulted in the observation of domain pinning, while nanoscale characterization of the spatial variations in the imprint and switching behavior of integrated (111)-oriented PZT-based ferroelectric random access memory (FRAM) capacitors by PFM have revealed a significant difference in imprint and switching behavior between the inner and outer parts of capacitors. The inner regions of the capacitors are typically negatively imprinted and consequently tend to switch back after being poled by a positive bias, while regions at the edge of the capacitors tend to exhibit more symmetric hysteresis behavior. Evidence was obtained indicating that mechanical stress conditions in the central regions of the capacitors can lead to incomplete switching. A combination of vertical and lateral piezoresponse force microscopy (VPFM and LPFM, respectively) has been used to map the out-of-plane and in-plane polarization distribution, respectively, of integrated (111)-oriented PZT-based capacitors, which revealed poled capacitors are in a polydomain state.

Preparation and quality test of superparamagnetic iron oxide labeled antisense oligodeoxynucleotide probe: a preliminary study.

PubMed

Wen, Ming; Li, Bibo; Ouyang, Yu; Luo, Yi; Li, Shaolin

2009-06-01

Molecular imaging of tumor antisense gene techniques have been applied to the study of magnetic resonance (MR) gene imaging associated with malignant tumors. In this study, we designed, synthesized, and tested a novel molecular probe, in which the antisense oligodeoxynucleotide (ASODN) was labeled with superparamagnetic iron oxide (SPIO), and its efficiency was examined by in vitro MR imaging after SK-Br-3 mammary carcinoma cell lines (oncocytes) transfection. The SPIO-labeled ASODN probe was prepared through SPIO conjugated to ASODN using a chemical cross linking method. Its morphology and size were detected by atomic force microscope, size distribution were detected by laser granulometer, the conjugating rate and biological activity were determined by high performance liquid chromatography, and the stability was determined by polyacrylamide gel electrophoresis. After that, the probes were transfected into the SK-Br-3 oncocytes, cellular iron uptake was analyzed qualitatively at light and electron microscopy and was quantified at atomic absorption spectrometry, and the signal change of the transfected cells was observed and measured using MR imaging. The morphology of the SPIO-labeled ASODN probe was mostly spherical with well-distributed scattering, and the diameters were between 25 and 40 nm (95%) by atomic force microscope and laser granulometer, the conjugating rate of the probe was 99%. Moreover, this probe kept its activity under physiological conditions and could conjugate with antisense oligodeoxynucleotide. In addition, light microscopy revealed an intracellular uptake of iron oxides in the cytosol and electron microscopic studies revealed a lysosomal deposition of iron oxides in the transfected SK-Br-3 oncocytes by antisense probes, some of them gathered stacks, and the iron content of the group of transfected SK-Br-3 oncocytes by antisense probe is significantly higher (18.37 +/- 0.42 pg) than other contrast groups, the MR imaging showed that transfected SK-Br-3 oncocytes by antisense probe had the lowest signal of all. The SPIO-labeled ASODN probe shows unique features including well-distributed spherical morphology, high conjugating rate and loading efficiency, and the signal intensity of SPIO-labeled ASODN-transfected SK-Br-3 oncocytes is reduced in MR imaging. These results indicate that the SPIO-labeled ASODN probe is potentially useful as a MR targeting contrast enhancing agent to specifically diagnose tumors which had over-expression of the c-erbB2 oncogene at an early stage.

Magnetic force microscopy study on wide adjacent track erasure in perpendicular magnetic write heads

NASA Astrophysics Data System (ADS)

Ruksasakchai, P.; Saengkaew, K.; Cheowanish, I.; Damrongsak, B.

2017-09-01

We used a phase-contrast magnetic force microscopy (MFM) to observe and analyze the failure of magnetic write heads due to the WATEr problem, which limits the off-track performance. During MFM imaging, the magnetic write head was energized by a DC current. The induced out-of-plane magnetic field was then detected by scanning a MFM probe across the surface of the magnetic write head. MFM images were then mapped with WATEr measured results from a spin stand method. Results showed that WATEr effect can be generated by several factors, i.e. the structure of magnetic domains and walls from material discontinuities and the magnetic field leakage at different locations on magnetic write heads. Understanding WATEr mechanisms is useful for design and process development engineers.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kim, Jong Hun; Park, Jeong Young, E-mail: jhjung@inha.ac.kr, E-mail: jeongypark@kaist.ac.kr; Graduate School of EEWS, Korea Advanced Institute of Science and Technology

Study of the triboelectric charging effect has recently gained much attraction by proposing a new potential technical application in the field of energy harvesting. Transparent polydimethylsiloxane (PDMS) has some advantages in employing the triboelectric effect due to good conformity at nanometer scale and the simple fabrication process. In this study, we demonstrate that UV irradiation can enhance the performance of a PDMS-based nanotribogenerator. Contact atomic force microscopy combined with Kelvin probe force microscopy enables an in-depth investigation of the effect of UV illumination on local triboelectric charge generation and its decay in PDMS. We found that UV exposure not onlymore » facilitates triboelectric charge generation but also enhances charge redistribution, which is related to the wettability of the PDMS surface. This study provides insights into the fundamental understanding and design of triboelectric generator devices.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Patel, Sajan; Petty, Clayton W.; Krafcik, Karen Lee

Electrostatic modes of atomic force microscopy have shown to be non-destructive and relatively simple methods for imaging conductors embedded in insulating polymers. Here we use electrostatic force microscopy to image the dispersion of carbon nanotubes in a latex-based conductive composite, which brings forth features not observed in previously studied systems employing linear polymer films. A fixed-potential model of the probe-nanotube electrostatics is presented which in principle gives access to the conductive nanoparticle's depth and radius, and the polymer film dielectric constant. Comparing this model to the data results in nanotube depths that appear to be slightly above the film–air interface.more » Furthermore, this result suggests that water-mediated charge build-up at the film–air interface may be the source of electrostatic phase contrast in ambient conditions.« less

[Atomic force microscopy fishing of gp120 on immobilized aptamer and its mass spectrometry identification].

PubMed

Bukharina, N S; Ivanov, Yu D; Pleshakova, T O; Frantsuzov, P A; Andreeva, E Yu; Kaysheva, A L; Izotov, A A; Pavlova, T I; Ziborov, V S; Radko, S P; Archakov, A I

2015-01-01

A method of atomic force microscopy-based fishing (AFM fishing) has been developed for protein detection in the analyte solution using a chip with an immobilized aptamer. This method is based on the biospecific fishing of a target protein from a bulk solution onto the small AFM chip area with the immobilized aptamer to this protein used as the molecular probe. Such aptamer-based approach allows to increase an AFM image contrast compared to the antibody-based approach. Mass spectrometry analysis used after the biospecific fishing to identify the target protein on the AFM chip has proved complex formation. Use of the AFM chip with the immobilized aptamer avoids interference of the antibody and target protein peaks in a mass spectrum.

EDITORIAL: Three decades of scanning tunnelling microscopy that changed the course of surface science Three decades of scanning tunnelling microscopy that changed the course of surface science

NASA Astrophysics Data System (ADS)

Ramachandra Rao, M. S.; Margaritondo, Giorgio

2011-11-01

Three decades ago, with a tiny tip of platinum, the scientific world saw the real space imaging of single atoms with unprecedented spatial resolution. This signalled the birth of one of the most versatile surface probes, based on the physics of quantum mechanical tunnelling: the scanning tunnelling microscope (STM). Invented in 1981 by Gerd Binnig and Heinrich Rohrer of IBM, Zurich, it led to their award of the 1986 Nobel Prize. Atoms, once speculated to be abstract entities used by theoreticians for mere calculations, can be seen to exist for real with the nano-eye of an STM tip that also gives real-space images of molecules and adsorbed complexes on surfaces. From a very fundamental perspective, the STM changed the course of surface science and engineering. STM also emerged as a powerful tool to study various fundamental phenomena relevant to the properties of surfaces in technological applications such as tribology, medical implants, catalysis, sensors and biology—besides elucidating the importance of local bonding geometries and defects, non-periodic structures and the co-existence of nano-scale phases. Atom-level probing, once considered a dream, has seen the light with the evolution of STM. An important off-shoot of STM was the atomic force microscope (AFM) for surface mapping of insulating samples. Then followed the development of a flurry of techniques under the general name of scanning probe microscopy (SPM). These techniques (STM, AFM, MFM, PFM etc) designed for atomic-scale-resolution imaging and spectroscopy, have led to brand new developments in surface analysis. All of these novel methods enabled researchers in recent years to image and analyse complex surfaces on microscopic and nanoscopic scales. All of them utilize a small probe for sensing the surface. The invention of AFM by Gerd Binnig, Calvin Quate and Christopher Gerber opened up new opportunities for characterization of a variety of materials, and various industrial applications could be envisaged. AFM observations of thin-film surfaces give us a picture of surface topography and morphology and any visible defects. The growing importance of ultra-thin films for magnetic recording in hard disk drive systems requires an in-depth understanding of the fundamental mechanisms occurring during growth. This special issue of Journal of Physics D: Applied Physics covers all of the different aspects of SPM that illustrate the achievements of this methodology: nanoscale imaging and mapping (Chiang, and Douillard and Charra), piezoresponse force microscopy (Soergel) and STM engineering (Okuyama and Hamada, and Huang et al). Chiang takes the reader on a journey along the STM imaging of atoms and molecules on surfaces. Jesse and Kalinin explore the band excitations that occur during the corresponding processes. Jia et al propose STM and molecular beam epitaxy as a winning experimental combination at the interface of science and technology. Douillard and Charra describe the high-resolution mapping of plasmonic modes using photoemission and scanning tunnelling microscopy. Cricenti et al demonstrate the importance of SPM in material science and biology. Wiebe et al have probed atomic scale magnetism, revealed by spin polarized scanning tunnelling microscopy. In addition, Simon et al present Fourier transform scanning tunnelling spectroscopy and the possibility to obtain constant energy maps and band dispersion using local measurements. Lackinger and Heckl give a perspective of the use of STM to study covalent intermolecular coupling reactions on surfaces. Okuyama and Hamada investigated hydrogen bond imaging and engineering with STM. Soergel describes the study of substrate-dependent self-assembled CuPc molecules using piezo force microscope (PFM). We are very grateful to the authors and reviewers for the papers in this special issue of Journal of Physics D: Applied Physics. Their contributions have provided a comprehensive picture of the evolution, status and potential of scanning probe microscopy, conveying to the readers the full excitement of this forefront domain of physics.

Automated scanning probe lithography with n-alkanethiol self assembled monolayers on Au(111): Application for teaching undergraduate laboratories

PubMed Central

Brown, Treva T.; LeJeune, Zorabel M.; Liu, Kai; Hardin, Sean; Li, Jie-Ren; Rupnik, Kresimir; Garno, Jayne C.

2010-01-01

Controllers for scanning probe instruments can be programmed for automated lithography to generate desired surface arrangements of nanopatterns of organic thin films, such as n-alkanethiol self-assembled monolayers (SAMs). In this report, atomic force microscopy (AFM) methods of lithography known as nanoshaving and nanografting are used to write nanopatterns within organic thin films. Commercial instruments provide software to control the length, direction, speed, and applied force of the scanning motion of the tip. For nanoshaving, higher forces are applied to an AFM tip to selectively remove regions of the matrix monolayer, exposing bare areas of the gold substrate. Nanografting is accomplished by force-induced displacement of molecules of a matrix SAM, followed immediately by the surface self-assembly of n-alkanethiol molecules from solution. Advancements in AFM automation enable rapid protocols for nanolithography, which can be accomplished within the tight time restraints of undergraduate laboratories. Example experiments with scanning probe lithography (SPL) will be described in this report that were accomplished by undergraduate students during laboratory course activities and research internships in the chemistry department of Louisiana State University. Students were introduced to principles of surface analysis and gained “hands-on” experience with nanoscale chemistry. PMID:21483651

Study of adhesion and friction properties on a nanoparticle gradient surface: transition from JKR to DMT contact mechanics.

PubMed

Ramakrishna, Shivaprakash N; Nalam, Prathima C; Clasohm, Lucy Y; Spencer, Nicholas D

2013-01-08

We have previously investigated the dependence of adhesion on nanometer-scale surface roughness by employing a roughness gradient. In this study, we correlate the obtained adhesion forces on nanometer-scale rough surfaces to their frictional properties. A roughness gradient with varying silica particle (diameter ≈ 12 nm) density was prepared, and adhesion and frictional forces were measured across the gradient surface in perfluorodecalin by means of atomic force microscopy with a polyethylene colloidal probe. Similarly to the pull-off measurements, the frictional forces initially showed a reduction with decreasing particle density and later an abrupt increase as the colloidal sphere began to touch the flat substrate beneath, at very low particle densities. The friction-load relation is found to depend on the real contact area (A(real)) between the colloid probe and the underlying particles. At high particle density, the colloidal sphere undergoes large deformations over several nanoparticles, and the contact adhesion (JKR type) dominates the frictional response. However, at low particle density (before the colloidal probe is in contact with the underlying surface), the colloidal sphere is suspended by a few particles only, resulting in local deformations of the colloid sphere, with the frictional response to the applied load being dominated by long-range, noncontact (DMT-type) interactions with the substrate beneath.

Conductive atomic force microscopy measurements of nanopillar magnetic tunnel junctions

NASA Astrophysics Data System (ADS)

Evarts, E. R.; Hogg, C.; Bain, J. A.; Majetich, S. A.

2009-03-01

Magnetic tunnel junctions have been studied extensively for their magnetoresistance and potential uses in magnetic logic and data storage devices, but little is known about how their performance will scale with size. Here we examined the electronic behavior of 12 nm diameter magnetic tunnel junctions fabricated by a novel nanomasking process. Scanning electron microscopy images indicated feature diameter of 12 nm, and atomic force microscopy showed a height of 5 nm suggesting that unmasked regions have been milled on average to the oxide barrier layer, and areas should have the remnants of the free layer exposed with no remaining nanoparticle. Electrical contact was made to individual nanopillars using a doped-diamond-coated atomic force microscopy probe with a 40 nm radius of curvature at the tip. Off pillar we observed a resistance of 8.1 x 10^5 φ, while on pillar we found a resistance of 2.85 x 10^6 φ. Based on the RA product for this film, 120 φ-μm^2, a 12 nm diameter cylinder with perfect contact would have a resistance of 1.06 x 10^6 φ. The larger experimental value is consistent with a smaller contact area due to damaging the pillar during the ion milling process. The magnetoresistance characteristics of these magnetic tunnel junctions will be discussed.

Correlative atomic force microscopy quantitative imaging-laser scanning confocal microscopy quantifies the impact of stressors on live cells in real-time.

PubMed

Bhat, Supriya V; Sultana, Taranum; Körnig, André; McGrath, Seamus; Shahina, Zinnat; Dahms, Tanya E S

2018-05-29

There is an urgent need to assess the effect of anthropogenic chemicals on model cells prior to their release, helping to predict their potential impact on the environment and human health. Laser scanning confocal microscopy (LSCM) and atomic force microscopy (AFM) have each provided an abundance of information on cell physiology. In addition to determining surface architecture, AFM in quantitative imaging (QI) mode probes surface biochemistry and cellular mechanics using minimal applied force, while LSCM offers a window into the cell for imaging fluorescently tagged macromolecules. Correlative AFM-LSCM produces complimentary information on different cellular characteristics for a comprehensive picture of cellular behaviour. We present a correlative AFM-QI-LSCM assay for the simultaneous real-time imaging of living cells in situ, producing multiplexed data on cell morphology and mechanics, surface adhesion and ultrastructure, and real-time localization of multiple fluorescently tagged macromolecules. To demonstrate the broad applicability of this method for disparate cell types, we show altered surface properties, internal molecular arrangement and oxidative stress in model bacterial, fungal and human cells exposed to 2,4-dichlorophenoxyacetic acid. AFM-QI-LSCM is broadly applicable to a variety of cell types and can be used to assess the impact of any multitude of contaminants, alone or in combination.

Scanning MWCNT-Nanopipette and Probe Microscopy: Li Patterning and Transport Studies.

PubMed

Larson, Jonathan M; Bharath, Satyaveda C; Cullen, William G; Reutt-Robey, Janice E

2015-10-07

A carbon-nanotube-enabling scanning probe technique/nanotechnology for manipulating and measuring lithium at the nano/mesoscale is introduced. Scanning Li-nanopipette and probe microscopy (SLi-NPM) is based on a conductive atomic force microscope (AFM) cantilever with an open-ended multi-walled carbon nanotube (MWCNT) affixed to its apex. SLi-NPM operation is demonstrated with a model system consisting of a Li thin film on a Si(111) substrate. By control of bias, separation distance, and contact time, attograms of Li can be controllably pipetted to or from the MWCNT tip. Patterned surface Li features are then directly probed via noncontact AFM measurements with the MWCNT tip. The subsequent decay of Li features is simulated with a mesoscale continuum model, developed here. The Li surface diffusion coefficient for a four (two) Li layer thick film is measured as D=8(±1.2)×10(-15) cm(2) s(-1) (D=1.75(±0.15)×10(-15) cm(2) s(-1)). Dual-Li pipetting/measuring with SLi-NPM enables a broad range of time-dependent Li and nanoelectrode characterization studies of fundamental importance to energy-storage research. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Scanning thermo-ionic microscopy for probing local electrochemistry at the nanoscale

DOE Office of Scientific and Technical Information (OSTI.GOV)

Eshghinejad, Ahmadreza; Nasr Esfahani, Ehsan; Wang, Peiqi

2016-05-28

Conventional electrochemical characterization techniques based on voltage and current measurements only probe faradaic and capacitive rates in aggregate. In this work we develop a scanning thermo-ionic microscopy (STIM) to probe local electrochemistry at the nanoscale, based on imaging of Vegard strain induced by thermal oscillation. It is demonstrated from both theoretical analysis and experimental validation that the second harmonic response of thermally induced cantilever vibration, associated with thermal expansion, is present in all solids, whereas the fourth harmonic response, caused by local transport of mobile species, is only present in ionic materials. The origin of STIM response is further confirmedmore » by its reduced amplitude with respect to increased contact force, due to the coupling of stress to concentration of ionic species and/or electronic defects. The technique has been applied to probe Sm-doped Ceria and LiFePO{sub 4}, both of which exhibit higher concentrations of mobile species near grain boundaries. The STIM gives us a powerful method to study local electrochemistry with high sensitivity and spatial resolution for a wide range of ionic systems, as well as ability to map local thermomechanical response.« less

Improving nanoparticle dispersion and charge transfer in cadmium telluride tetrapod and conjugated polymer blends.

PubMed

Monson, Todd C; Hollars, Christopher W; Orme, Christine A; Huser, Thomas

2011-04-01

The dispersion of CdTe tetrapods in a conducting polymer and the resulting charge transfer is studied using a combination of confocal fluorescence microscopy and atomic force microscopy (AFM). The results of this work show that both the tetrapod dispersion and charge transfer between the CdTe and conducting polymer (P3HT) are greatly enhanced by exchanging the ligands on the surface of the CdTe and by choosing proper solvent mixtures. The ability to experimentally probe the relationship between particle dispersion and charge transfer through the combination of AFM and fluorescence microscopy provides another avenue to assess the performance of polymer/semiconductor nanoparticle composites. © 2011 American Chemical Society

STM, SECPM, AFM and Electrochemistry on Single Crystalline Surfaces

PubMed Central

Wolfschmidt, Holger; Baier, Claudia; Gsell, Stefan; Fischer, Martin; Schreck, Matthias; Stimming, Ulrich

2010-01-01

Scanning probe microscopy (SPM) techniques have had a great impact on research fields of surface science and nanotechnology during the last decades. They are used to investigate surfaces with scanning ranges between several 100 μm down to atomic resolution. Depending on experimental conditions, and the interaction forces between probe and sample, different SPM techniques allow mapping of different surface properties. In this work, scanning tunneling microscopy (STM) in air and under electrochemical conditions (EC-STM), atomic force microscopy (AFM) in air and scanning electrochemical potential microscopy (SECPM) under electrochemical conditions, were used to study different single crystalline surfaces in electrochemistry. Especially SECPM offers potentially new insights into the solid-liquid interface by providing the possibility to image the potential distribution of the surface, with a resolution that is comparable to STM. In electrocatalysis, nanostructured catalysts supported on different electrode materials often show behavior different from their bulk electrodes. This was experimentally and theoretically shown for several combinations and recently on Pt on Au(111) towards fuel cell relevant reactions. For these investigations single crystals often provide accurate and well defined reference and support systems. We will show heteroepitaxially grown Ru, Ir and Rh single crystalline surface films and bulk Au single crystals with different orientations under electrochemical conditions. Image studies from all three different SPM methods will be presented and compared to electrochemical data obtained by cyclic voltammetry in acidic media. The quality of the single crystalline supports will be verified by the SPM images and the cyclic voltammograms. Furthermore, an outlook will be presented on how such supports can be used in electrocatalytic studies. PMID:28883327

Novel nano-OLED based probes for very high resolution optical microscopy

NASA Astrophysics Data System (ADS)

Zhao, Yiying

Near-field scanning optical microscopy (NSOM) has been applied in the study of nanomaterials, microelectronics, photonics, plasmonics, cells, and molecules. However, conventional NSOM relies on optically pumped probes, suffering low optical transmission, heating of the tip, and poor reproducibility of probe fabrication, increasing the cost, impeding usability, reducing practical imaging resolution, and limiting NSOM's utility. In this thesis, I demonstrate a novel probe based on a nanoscale, electrically pumped organic light-emitting device (OLED) formed on the tip of a low-cost, commercially available atomic force microscopy (AFM) probe. I describe the structure, fabrication, and principles of this novel probe's operation, and discuss its potential to overcome the limitations of conventional NSOM probes. The broader significance of this work in the field of organic optoelectronics is also discussed. Briefly, OLEDs consist of organic thin films sandwiched between two electrodes. Under bias, electrons and holes are injected into the organic layers, leading to radiative recombination. Depositing a small molecular OLED in vacuum onto a pyramid-tipped AFM probe results in a laminar structure that is highly curved at the tip. Simple electrical modeling predicts concentration of electric field and localized electron injection into the organic layers at the tip, improving the local charge balance in an otherwise electron-starved OLED. Utilizing an "inverted" OLED structure (i.e. cathode on the "bottom"), light emission is localized to sub-200 nm sized, green light emitting regions on probe vertices; light output power in the range of 0.1-0.5 nanowatts was observed, comparable to that of typical fiber based NSOM probes but with greater power efficiency. Massive arrays of similar sub-micron OLEDs were also fabricated by depositing onto textured silicon substrates, demonstrating the superior scalability of the probe fabrication process (e.g. relative to pulled glass fibers). The investigation of the effect of non-planar substrate geometry on charge injection, transport and recombination provides broader insights into OLEDs made on rough substrates, general understanding of OLED operation (e.g. filamentary charge conduction) and degradation, and potentially helps to improve technologically important "inverted" OLED structures.

Study of modification methods of probes for critical-dimension atomic-force microscopy by the deposition of carbon nanotubes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ageev, O. A., E-mail: ageev@sfedu.ru; Bykov, Al. V.; Kolomiitsev, A. S.

2015-12-15

The results of an experimental study of the modification of probes for critical-dimension atomicforce microscopy (CD-AFM) by the deposition of carbon nanotubes (CNTs) to improve the accuracy with which the surface roughness of vertical walls is determined in submicrometer structures are presented. Methods of the deposition of an individual CNT onto the tip of an AFM probe via mechanical and electrostatic interaction between the probe and an array of vertically aligned carbon nanotubes (VACNTs) are studied. It is shown that, when the distance between the AFM tip and a VACNT array is 1 nm and the applied voltage is withinmore » the range 20–30 V, an individual carbon nanotube is deposited onto the tip. On the basis of the results obtained in the study, a probe with a carbon nanotube on its tip (CNT probe) with a radius of 7 nm and an aspect ratio of 1:15 is formed. Analysis of the CNT probe demonstrates that its use improves the resolution and accuracy of AFM measurements, compared with the commercial probe, and also makes it possible to determine the roughness of the vertical walls of high-aspect structures by CD-AFM. The results obtained can be used to develop technological processes for the fabrication and reconditioning of special AFM probes, including those for CD-AFM, and procedures for the interoperational express monitoring of technological process parameters in the manufacturing of elements for micro- and nanoelectronics and micro- and nanosystem engineering.« less

Mapping the distribution of emissive molecules in human ocular lipofuscin granules with near-field scanning optical microscopy.

PubMed

Krogmeier, J R; Clancy, C M; Pawlak, A; Rozanowska, M; Sarna, T; Simon, J D; Dunn, R C

2001-05-01

Several high resolution imaging techniques are utilized to probe the structure of human ocular lipofuscin granules. Atomic force microscopy reveals typical granule sizes to be about one micrometre in diameter and hundreds of nanometres in height, in agreement with previous electron microscopy results. For issues concerning the role of lipofuscin in age-related macular degeneration, recent attention has focused on the orange-emitting fluorophore, A2E. Confocal microscopy measurements are presented which reveal the presence of a highly emissive component in the granules, consistent with the presence of A2E. It is shown, however, that the interpretation of these results is complicated by the lack of structural details about the particles. To address these issues, near-field scanning optical microscopy (NSOM) measurements are presented which measure both the lipofuscin fluorescence and topography, simultaneously. These measurements reveal distinct structure in the fluorescence image which do not necessarily correlate with the topography of the granules. Moreover, direct comparison between the NSOM fluorescence and topography measurements suggests that A2E is not the major component in lipofuscin. These measurements illustrate the unique capabilities of NSOM for probing into the microstructure of lipofuscin and uncovering new insights into its phototoxicity.

Scanning probe recognition microscopy investigation of tissue scaffold properties

PubMed Central

Fan, Yuan; Chen, Qian; Ayres, Virginia M; Baczewski, Andrew D; Udpa, Lalita; Kumar, Shiva

2007-01-01

Scanning probe recognition microscopy is a new scanning probe microscopy technique which enables selective scanning along individual nanofibers within a tissue scaffold. Statistically significant data for multiple properties can be collected by repetitively fine-scanning an identical region of interest. The results of a scanning probe recognition microscopy investigation of the surface roughness and elasticity of a series of tissue scaffolds are presented. Deconvolution and statistical methods were developed and used for data accuracy along curved nanofiber surfaces. Nanofiber features were also independently analyzed using transmission electron microscopy, with results that supported the scanning probe recognition microscopy-based analysis. PMID:18203431

Scanning probe recognition microscopy investigation of tissue scaffold properties.

PubMed

Fan, Yuan; Chen, Qian; Ayres, Virginia M; Baczewski, Andrew D; Udpa, Lalita; Kumar, Shiva

2007-01-01

Scanning probe recognition microscopy is a new scanning probe microscopy technique which enables selective scanning along individual nanofibers within a tissue scaffold. Statistically significant data for multiple properties can be collected by repetitively fine-scanning an identical region of interest. The results of a scanning probe recognition microscopy investigation of the surface roughness and elasticity of a series of tissue scaffolds are presented. Deconvolution and statistical methods were developed and used for data accuracy along curved nanofiber surfaces. Nanofiber features were also independently analyzed using transmission electron microscopy, with results that supported the scanning probe recognition microscopy-based analysis.

Enhancing Ion Migration in Grain Boundaries of Hybrid Organic-Inorganic Perovskites by Chlorine

DOE PAGES

Yang, Bin; Brown, Chance C.; Huang, Jingsong; ...

2017-05-26

Ionicity plays an important role in determining material properties, as well as optoelectronic performance of organometallic trihalide perovskites (OTPs). Ion migration in OTP films has recently been under intensive investigation by various scanning probe microscopy (SPM) techniques. Controversial findings regarding the role of grain boundaries (GBs) associated with ion migration are often encountered, likely as a result of feedback errors and topographic effects common in to SPM. In this work, electron microscopy and spectroscopy (scanning transmission electron microscopy/electron energy loss spectroscopy) are combined with a novel, open-loop, band-excitation, (contact) Kelvin probe force microscopy (BE-KPFM and BE-cKPFM), in conjunction with abmore » initio molecular dynamics simulations to examine the ion behavior in the GBs of CH 3NH 3PbI 3 perovskite films. Furthermore, this combination of diverse techniques provides a deeper understanding of the differences between ion migration within GBs and interior grains in OTP films. Our work demonstrates that ion migration can be significantly enhanced by introducing additional mobile Cl - ions into GBs. The enhancement of ion migration may serve as the first step toward the development of high-performance electrically and optically tunable memristors and synaptic devices.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yang, Bin; Brown, Chance C.; Huang, Jingsong

Ionicity plays an important role in determining material properties, as well as optoelectronic performance of organometallic trihalide perovskites (OTPs). Ion migration in OTP films has recently been under intensive investigation by various scanning probe microscopy (SPM) techniques. Controversial findings regarding the role of grain boundaries (GBs) associated with ion migration are often encountered, likely as a result of feedback errors and topographic effects common in to SPM. In this work, electron microscopy and spectroscopy (scanning transmission electron microscopy/electron energy loss spectroscopy) are combined with a novel, open-loop, band-excitation, (contact) Kelvin probe force microscopy (BE-KPFM and BE-cKPFM), in conjunction with abmore » initio molecular dynamics simulations to examine the ion behavior in the GBs of CH 3NH 3PbI 3 perovskite films. Furthermore, this combination of diverse techniques provides a deeper understanding of the differences between ion migration within GBs and interior grains in OTP films. Our work demonstrates that ion migration can be significantly enhanced by introducing additional mobile Cl - ions into GBs. The enhancement of ion migration may serve as the first step toward the development of high-performance electrically and optically tunable memristors and synaptic devices.« less

Electron beam detection of a Nanotube Scanning Force Microscope.

PubMed

Siria, Alessandro; Niguès, Antoine

2017-09-14

Atomic Force Microscopy (AFM) allows to probe matter at atomic scale by measuring the perturbation of a nanomechanical oscillator induced by near-field interaction forces. The quest to improve sensitivity and resolution of AFM forced the introduction of a new class of resonators with dimensions at the nanometer scale. In this context, nanotubes are the ultimate mechanical oscillators because of their one dimensional nature, small mass and almost perfect crystallinity. Coupled to the possibility of functionalisation, these properties make them the perfect candidates as ultra sensitive, on-demand force sensors. However their dimensions make the measurement of the mechanical properties a challenging task in particular when working in cavity free geometry at ambient temperature. By using a focused electron beam, we show that the mechanical response of nanotubes can be quantitatively measured while approaching to a surface sample. By coupling electron beam detection of individual nanotubes with a custom AFM we image the surface topography of a sample by continuously measuring the mechanical properties of the nanoresonators. The combination of very small size and mass together with the high resolution of the electron beam detection method offers unprecedented opportunities for the development of a new class of nanotube-based scanning force microscopy.

Photo-Carrier Multi-Dynamical Imaging at the Nanometer Scale in Organic and Inorganic Solar Cells.

PubMed

Fernández Garrillo, Pablo A; Borowik, Łukasz; Caffy, Florent; Demadrille, Renaud; Grévin, Benjamin

2016-11-16

Investigating the photocarrier dynamics in nanostructured and heterogeneous energy materials is of crucial importance from both fundamental and technological points of view. Here, we demonstrate how noncontact atomic force microscopy combined with Kelvin probe force microscopy under frequency-modulated illumination can be used to simultaneously image the surface photopotential dynamics at different time scales with a sub-10 nm lateral resolution. The basic principle of the method consists in the acquisition of spectroscopic curves of the surface potential as a function of the illumination frequency modulation on a two-dimensional grid. We show how this frequency-spectroscopy can be used to probe simultaneously the charging rate and several decay processes involving short-lived and long-lived carriers. With this approach, dynamical images of the trap-filling, trap-delayed recombination and nongeminate recombination processes have been acquired in nanophase segregated organic donor-acceptor bulk heterojunction thin films. Furthermore, the spatial variation of the minority carrier lifetime has been imaged in polycrystalline silicon thin films. These results establish two-dimensional multidynamical photovoltage imaging as a universal tool for local investigations of the photocarrier dynamics in photoactive materials and devices.

Kelvin probe force microscopy studies of the charge effects upon adsorption of carbon nanotubes and C60 fullerenes on hydrogen-terminated diamond

NASA Astrophysics Data System (ADS)

Kölsch, S.; Fritz, F.; Fenner, M. A.; Kurch, S.; Wöhrl, N.; Mayne, A. J.; Dujardin, G.; Meyer, C.

2018-01-01

Hydrogen-terminated diamond is known for its unusually high surface conductivity that is ascribed to its negative electron affinity. In the presence of acceptor molecules, electrons are expected to transfer from the surface to the acceptor, resulting in p-type surface conductivity. Here, we present Kelvin probe force microscopy (KPFM) measurements on carbon nanotubes and C60 adsorbed onto a hydrogen-terminated diamond(001) surface. A clear reduction in the Kelvin signal is observed at the position of the carbon nanotubes and C60 molecules as compared with the bare, air-exposed surface. This result can be explained by the high positive electron affinity of carbon nanotubes and C60, resulting in electron transfer from the surface to the adsorbates. When an oxygen-terminated diamond(001) is used instead, no reduction in the Kelvin signal is obtained. While the presence of a charged adsorbate or a difference in work function could induce a change in the KPFM signal, a charge transfer effect of the hydrogen-terminated diamond surface, by the adsorption of the carbon nanotubes and the C60 fullerenes, is consistent with previous theoretical studies.

Work function measurement of multilayer electrodes using Kelvin probe force microscopy

NASA Astrophysics Data System (ADS)

Peres, L.; Bou, A.; Cornille, C.; Barakel, D.; Torchio, P.

2017-04-01

The workfunction of dielectric|metal|dielectric transparent and conductive electrodes, promising candidates for replacing ITO in thin film solar cells, is measured by Kelvin probe force microscopy (KPFM). Measurement on commercial ITO gives a workfunction of 4.74 eV, which is in agreement with the values reported in the literature. Measurements are then performed on optically optimised multilayer electrodes fabricated on glass by e-beam evaporation, using three different dielectrics. For TiO2(37 nm)|Ag(13 nm)|TiO2(42 nm), SnO x (45 nm)|Ag(10 nm)|SnO x (45 nm), and ZnS(47 nm)|Ag(12 nm)|ZnS(42 nm), workfunctions of 4.83 eV, 4.75 eV, and 4.48 eV are measured respectively. These values suggest that these transparent and conductive electrodes are well adapted to extract photo-generated charge carriers in photovoltaic devices in which ITO is normally used. Furthermore, the KPFM technique proves to be an efficient and relatively fast way to determine the work function values of such electrodes.

Enantiospecific Detection of Chiral Nanosamples Using Photoinduced Force

NASA Astrophysics Data System (ADS)

Kamandi, Mohammad; Albooyeh, Mohammad; Guclu, Caner; Veysi, Mehdi; Zeng, Jinwei; Wickramasinghe, Kumar; Capolino, Filippo

2017-12-01

We propose a high-resolution microscopy technique for enantiospecific detection of chiral samples down to sub-100-nm size based on force measurement. We delve into the differential photoinduced optical force Δ F exerted on an achiral probe in the vicinity of a chiral sample when left and right circularly polarized beams separately excite the sample-probe interactive system. We analytically prove that Δ F is entangled with the enantiomer type of the sample enabling enantiospecific detection of chiral inclusions. Moreover, we demonstrate that Δ F is linearly dependent on both the chiral response of the sample and the electric response of the tip and is inversely related to the quartic power of probe-sample distance. We provide physical insight into the transfer of optical activity from the chiral sample to the achiral tip based on a rigorous analytical approach. We support our theoretical achievements by several numerical examples highlighting the potential application of the derived analytic properties. Lastly, we demonstrate the sensitivity of our method to enantiospecify nanoscale chiral samples with chirality parameter on the order of 0.01 and discuss how the sensitivity of our proposed technique can be further improved.

Use of scanning near-field optical microscope with an aperture probe for detection of luminescent nanodiamonds

NASA Astrophysics Data System (ADS)

Shershulin, V. A.; Samoylenko, S. R.; Shenderova, O. A.; Konov, V. I.; Vlasov, I. I.

2017-02-01

The suitability of scanning near-field optical microscopy (SNOM) to image photoluminescent diamond nanoparticles with nanoscale resolution is demonstrated. Isolated diamond nanocrystals with an average size of 100 nm, containing negatively charged nitrogen-vacancy (NV-) centers, were chosen as tested material. The NV- luminescence was stimulated by continuous 532 nm laser light. Sizes of analyzed crystallites were monitored by an atomic force microscope. The lateral resolution of the order of 100 nm was reached in SNOM imaging of diamond nanoparticles using 150 nm square aperture of the probe.

p{sup +}-doping analysis of laser fired contacts for silicon solar cells by Kelvin probe force microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ebser, J., E-mail: Jan.Ebser@uni-konstanz.de; Sommer, D.; Fritz, S.

Local rear contacts for silicon passivated emitter and rear contact solar cells can be established by point-wise treating an Al layer with laser radiation and thereby establishing an electrical contact between Al and Si bulk through the dielectric passivation layer. In this laser fired contacts (LFC) process, Al can establish a few μm thick p{sup +}-doped Si region below the metal/Si interface and forms in this way a local back surface field which reduces carrier recombination at the contacts. In this work, the applicability of Kelvin probe force microscopy (KPFM) to the investigation of LFCs considering the p{sup +}-doping distributionmore » is demonstrated. The method is based on atomic force microscopy and enables the evaluation of the lateral 2D Fermi-level characteristics at sub-micrometer resolution. The distribution of the electrical potential and therefore the local hole concentration in and around the laser fired region can be measured. KPFM is performed on mechanically polished cross-sections of p{sup +}-doped Si regions formed by the LFC process. The sample preparation is of great importance because the KPFM signal is very surface sensitive. Furthermore, the measurement is responsive to sample illumination and the height of the applied voltage between tip and sample. With other measurement techniques like micro-Raman spectroscopy, electrochemical capacitance-voltage, and energy dispersive X-ray analysis, a high local hole concentration in the range of 10{sup 19 }cm{sup −3} is demonstrated in the laser fired region. This provides, in combination with the high spatial resolution of the doping distribution measured by KPFM, a promising approach for microscopic understanding and further optimization of the LFC process.« less

Nonlinear Dynamics of Cantilever-Sample Interactions in Atomic Force Microscopy

NASA Technical Reports Server (NTRS)

Cantrell, John H.; Cantrell, Sean A.

2010-01-01

The interaction of the cantilever tip of an atomic force microscope (AFM) with the sample surface is obtained by treating the cantilever and sample as independent systems coupled by a nonlinear force acting between the cantilever tip and a volume element of the sample surface. The volume element is subjected to a restoring force from the remainder of the sample that provides dynamical equilibrium for the combined systems. The model accounts for the positions on the cantilever of the cantilever tip, laser probe, and excitation force (if any) via a basis set of set of orthogonal functions that may be generalized to account for arbitrary cantilever shapes. The basis set is extended to include nonlinear cantilever modes. The model leads to a pair of coupled nonlinear differential equations that are solved analytically using a matrix iteration procedure. The effects of oscillatory excitation forces applied either to the cantilever or to the sample surface (or to both) are obtained from the solution set and applied to the to the assessment of phase and amplitude signals generated by various acoustic-atomic force microscope (A-AFM) modalities. The influence of bistable cantilever modes of on AFM signal generation is discussed. The effects on the cantilever-sample surface dynamics of subsurface features embedded in the sample that are perturbed by surface-generated oscillatory excitation forces and carried to the cantilever via wave propagation are accounted by the Bolef-Miller propagating wave model. Expressions pertaining to signal generation and image contrast in A-AFM are obtained and applied to amplitude modulation (intermittent contact) atomic force microscopy and resonant difference-frequency atomic force ultrasonic microscopy (RDF-AFUM). The influence of phase accumulation in A-AFM on image contrast is discussed, as is the effect of hard contact and maximum nonlinearity regimes of A-AFM operation.

Synthesis of a Far-Red Photoactivatable Silicon-Containing Rhodamine for Super-Resolution Microscopy.

PubMed

Grimm, Jonathan B; Klein, Teresa; Kopek, Benjamin G; Shtengel, Gleb; Hess, Harald F; Sauer, Markus; Lavis, Luke D

2016-01-26

The rhodamine system is a flexible framework for building small-molecule fluorescent probes. Changing N-substitution patterns and replacing the xanthene oxygen with a dimethylsilicon moiety can shift the absorption and fluorescence emission maxima of rhodamine dyes to longer wavelengths. Acylation of the rhodamine nitrogen atoms forces the molecule to adopt a nonfluorescent lactone form, providing a convenient method to make fluorogenic compounds. Herein, we take advantage of all of these structural manipulations and describe a novel photoactivatable fluorophore based on a Si-containing analogue of Q-rhodamine. This probe is the first example of a "caged" Si-rhodamine, exhibits higher photon counts compared to established localization microscopy dyes, and is sufficiently red-shifted to allow multicolor imaging. The dye is a useful label for super-resolution imaging and constitutes a new scaffold for far-red fluorogenic molecules. © 2015 The Authors. Published by Wiley-VCH Verlag GmbH & Co. KGaA.

Synthesis of a Far‐Red Photoactivatable Silicon‐Containing Rhodamine for Super‐Resolution Microscopy

PubMed Central

Grimm, Jonathan B.; Klein, Teresa; Kopek, Benjamin G.; Shtengel, Gleb; Hess, Harald F.; Sauer, Markus

2015-01-01

Abstract The rhodamine system is a flexible framework for building small‐molecule fluorescent probes. Changing N‐substitution patterns and replacing the xanthene oxygen with a dimethylsilicon moiety can shift the absorption and fluorescence emission maxima of rhodamine dyes to longer wavelengths. Acylation of the rhodamine nitrogen atoms forces the molecule to adopt a nonfluorescent lactone form, providing a convenient method to make fluorogenic compounds. Herein, we take advantage of all of these structural manipulations and describe a novel photoactivatable fluorophore based on a Si‐containing analogue of Q‐rhodamine. This probe is the first example of a “caged” Si‐rhodamine, exhibits higher photon counts compared to established localization microscopy dyes, and is sufficiently red‐shifted to allow multicolor imaging. The dye is a useful label for super‐resolution imaging and constitutes a new scaffold for far‐red fluorogenic molecules. PMID:26661345

Influence of smectite suspension structure on sheet orientation in dry sediments: XRD and AFM applications.

PubMed

Zbik, Marek S; Frost, Ray L

2010-06-15

The structure-building phenomena within clay aggregates are governed by forces acting between clay particles. Measurements of such forces are important to understand in order to manipulate the aggregate structure for applications such as dewatering of mineral processing tailings. A parallel particle orientation is required when conducting XRD investigation on the oriented samples and conduct force measurements acting between basal planes of clay mineral platelets using atomic force microscopy (AFM). To investigate how smectite clay platelets were oriented on silicon wafer substrate when dried from suspension range of methods like SEM, XRD and AFM were employed. From these investigations, we conclude that high clay concentrations and larger particle diameters (up to 5 microm) in suspension result in random orientation of platelets in the substrate. The best possible laminar orientation in the clay dry film, represented in the XRD 001/020 intensity ratio of 47 was obtained by drying thin layers from 0.02 wt.% clay suspensions of the natural pH. Conducted AFM investigations show that smectite studied in water based electrolytes show very long-range repulsive forces lower in strength than electrostatic forces from double-layer repulsion. It was suggested that these forces may have structural nature. Smectite surface layers rehydrate in water environment forms surface gel with spongy and cellular texture which cushion approaching AFM probe. This structural effect can be measured in distances larger than 1000 nm from substrate surface and when probe penetrate this gel layer, structural linkages are forming between substrate and clay covered probe. These linkages prevent subsequently smooth detachments of AFM probe on way back when retrieval. This effect of tearing new formed structure apart involves larger adhesion-like forces measured in retrieval. It is also suggested that these effect may be enhanced by the nano-clay particles interaction. 2010 Elsevier Inc. All rights reserved.

Ferroelectric or non-ferroelectric: Why so many materials exhibit “ferroelectricity” on the nanoscale

DOE PAGES

Vasudevan, Rama K.; Balke, Nina; Maksymovych, Peter; ...

2017-05-01

Here, ferroelectric materials have remained one of the major focal points of condensed matter physics and materials science for over 50 years. In the last 20 years, the development of voltage-modulated scanning probe microscopy techniques, exemplified by Piezoresponse force microscopy (PFM) and associated time- and voltage spectroscopies, opened a pathway to explore these materials on a single-digit nanometer level. Consequently, domain structures and walls and polarization dynamics can now be imaged in real space. More generally, PFM has allowed studying electromechanical coupling in a broad variety of materials ranging from ionics to biological systems.

Domain wall magnetoresistance in BiFeO3 thin films measured by scanning probe microscopy

NASA Astrophysics Data System (ADS)

Domingo, N.; Farokhipoor, S.; Santiso, J.; Noheda, B.; Catalan, G.

2017-08-01

We measure the magnetotransport properties of individual 71° domain walls in multiferroic BiFeO3 by means of conductive—atomic force microscopy (C-AFM) in the presence of magnetic fields up to one Tesla. The results suggest anisotropic magnetoresistance at room temperature, with the sign of the magnetoresistance depending on the relative orientation between the magnetic field and the domain wall plane. A consequence of this finding is that macroscopically averaged magnetoresistance measurements for domain wall bunches are likely to underestimate the magnetoresistance of each individual domain wall.

Dielectrophoretic positioning of single nanoparticles on atomic force microscope tips for tip-enhanced Raman spectroscopy.

PubMed

Leiterer, Christian; Deckert-Gaudig, Tanja; Singh, Prabha; Wirth, Janina; Deckert, Volker; Fritzsche, Wolfgang

2015-05-01

Tip-enhanced Raman spectroscopy, a combination of Raman spectroscopy and scanning probe microscopy, is a powerful technique to detect the vibrational fingerprint of molecules at the nanometer scale. A metal nanoparticle at the apex of an atomic force microscope tip leads to a large enhancement of the electromagnetic field when illuminated with an appropriate wavelength, resulting in an increased Raman signal. A controlled positioning of individual nanoparticles at the tip would improve the reproducibility of the probes and is quite demanding due to usually serial and labor-intensive approaches. In contrast to commonly used submicron manipulation techniques, dielectrophoresis allows a parallel and scalable production, and provides a novel approach toward reproducible and at the same time affordable tip-enhanced Raman spectroscopy tips. We demonstrate the successful positioning of an individual plasmonic nanoparticle on a commercial atomic force microscope tip by dielectrophoresis followed by experimental proof of the Raman signal enhancing capabilities of such tips. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Nanoscale elasticity mappings of micro-constituents of abalone shell by band excitation-contact resonance force microscopy

NASA Astrophysics Data System (ADS)

Li, Tao; Zeng, Kaiyang

2014-01-01

The macroscopic mechanical properties of the abalone shell have been studied extensively in the literature, but the in situ nanoscale elasticity of various micro-constituents in the shell have not been characterized and reported yet. In this study, the nanoscale elasticity mappings including different micro-constituents in abalone shell were observed by using the Contact Resonance Force Microscopy (CR-FM) technique. CR-FM is one of the advanced scanning probe microscopy techniques that is able to quantify the local elastic moduli of various materials in a non-destructive manner. Instead of an average value, an elasticity mapping that reveals the nanoscale variations of elastic moduli with location can be extracted and correlated with the topography of the structure. Therefore in this study, by adopting the CR-FM technique that is incorporated with the band excitation technique, the elasticity variations of the abalone shell caused by different micro-constituents and crystal orientations are reported, and the elasticity values of the aragonite and calcite nanograins are quantified.The macroscopic mechanical properties of the abalone shell have been studied extensively in the literature, but the in situ nanoscale elasticity of various micro-constituents in the shell have not been characterized and reported yet. In this study, the nanoscale elasticity mappings including different micro-constituents in abalone shell were observed by using the Contact Resonance Force Microscopy (CR-FM) technique. CR-FM is one of the advanced scanning probe microscopy techniques that is able to quantify the local elastic moduli of various materials in a non-destructive manner. Instead of an average value, an elasticity mapping that reveals the nanoscale variations of elastic moduli with location can be extracted and correlated with the topography of the structure. Therefore in this study, by adopting the CR-FM technique that is incorporated with the band excitation technique, the elasticity variations of the abalone shell caused by different micro-constituents and crystal orientations are reported, and the elasticity values of the aragonite and calcite nanograins are quantified. Electronic supplementary information (ESI) available. See DOI: 10.1039/c3nr05292c

High-resolution imaging of silicene on an Ag(111) surface by atomic force microscopy

NASA Astrophysics Data System (ADS)

Onoda, Jo; Yabuoshi, Keisuke; Miyazaki, Hiroki; Sugimoto, Yoshiaki

2017-12-01

Silicene, a two-dimensional (2D) honeycomb arrangement of Si atoms, is expected to have better electronic properties than graphene and has been mostly synthesized on Ag surfaces. Although scanning tunneling microscopy (STM) has been used for visualizing its atomic structure in real space, the interpretation of STM contrast is not straightforward and only the topmost Si atoms were observed on the (4 ×4 ) silicene/Ag(111) surface. Here, we demonstrate that high-resolution atomic force microscopy (AFM) can resolve all constituent Si atoms in the buckled honeycomb arrangement of the (4 ×4 ) silicene. Site-specific force spectroscopy attributes the origin of the high-resolution AFM images to chemical bonds between the AFM probe apex and the individual Si atoms on the (4 ×4 ) silicene. A detailed analysis of the geometric parameters suggests that the pulling up of lower-buckled Si atoms by the AFM tip could be a key for high-resolution AFM, implying a weakening of the Si-Ag interactions at the interface. We expect that high-resolution AFM will also unveil atomic structures of edges and defects of silicene, or other emerging 2D materials.

Probing viscoelastic surfaces with bimodal tapping-mode atomic force microscopy: Underlying physics and observables for a standard linear solid model.

PubMed

Solares, Santiago D

2014-01-01

This paper presents computational simulations of single-mode and bimodal atomic force microscopy (AFM) with particular focus on the viscoelastic interactions occurring during tip-sample impact. The surface is modeled by using a standard linear solid model, which is the simplest system that can reproduce creep compliance and stress relaxation, which are fundamental behaviors exhibited by viscoelastic surfaces. The relaxation of the surface in combination with the complexities of bimodal tip-sample impacts gives rise to unique dynamic behaviors that have important consequences with regards to the acquisition of quantitative relationships between the sample properties and the AFM observables. The physics of the tip-sample interactions and its effect on the observables are illustrated and discussed, and a brief research outlook on viscoelasticity measurement with intermittent-contact AFM is provided.

Anomalous domain inversion in LiNbO3 single crystals investigated by scanning probe microscopy

NASA Astrophysics Data System (ADS)

Lilienblum, M.; Soergel, E.

2011-09-01

Ferroelectric domains were written in lithium niobate (LiNbO3) single crystals by applying voltage pulses to the tip of a scanning force microscope. The generated domains are subsequently imaged by piezoresponse force microscopy. As it has been previously observed not only full domains but also doughnut-shaped ones arise from tip-based domain formation. In this contribution, we present our experiments which were carried out with 10-20 μm thin LiNbO3 single crystals. We show that by choosing appropriate writing parameters, domains of predetermined shape (full or doughnut) can be reliably generated. In addition to the duration and the amplitude of the voltage pulse the moment of the retraction of the tip from the sample surface was found to be a crucial parameter for reproducible domain formation.

Effect of calcium concentration on the structure of casein micelles in thin films.

PubMed

Müller-Buschbaum, P; Gebhardt, R; Roth, S V; Metwalli, E; Doster, W

2007-08-01

The structure of thin casein films prepared with spin-coating is investigated as a function of the calcium concentration. Grazing incidence small-angle x-ray scattering and atomic force microscopy are used to probe the micelle structure. For comparison, the corresponding casein solutions are investigated with dynamic light-scattering experiments. In the thin films with added calcium three types of casein structures, aggregates, micelles, and mini-micelles, are observed in coexistence with atomic force microscopy and grazing incidence small-angle x-ray scattering. With increasing calcium concentration, the size of the aggregates strongly increases, while the size of micelles slightly decreases and the size of the mini-micelles increases. This effect is explained in the framework of the particle-stabilizing properties of the hairy layer of kappa-casein surrounding the casein micelles.

Effect of Calcium Concentration on the Structure of Casein Micelles in Thin Films

PubMed Central

Müller-Buschbaum, P.; Gebhardt, R.; Roth, S. V.; Metwalli, E.; Doster, W.

2007-01-01

The structure of thin casein films prepared with spin-coating is investigated as a function of the calcium concentration. Grazing incidence small-angle x-ray scattering and atomic force microscopy are used to probe the micelle structure. For comparison, the corresponding casein solutions are investigated with dynamic light-scattering experiments. In the thin films with added calcium three types of casein structures, aggregates, micelles, and mini-micelles, are observed in coexistence with atomic force microscopy and grazing incidence small-angle x-ray scattering. With increasing calcium concentration, the size of the aggregates strongly increases, while the size of micelles slightly decreases and the size of the mini-micelles increases. This effect is explained in the framework of the particle-stabilizing properties of the hairy layer of κ-casein surrounding the casein micelles. PMID:17496032

Atomic force microscopy-based characterization and design of biointerfaces

NASA Astrophysics Data System (ADS)

Alsteens, David; Gaub, Hermann E.; Newton, Richard; Pfreundschuh, Moritz; Gerber, Christoph; Müller, Daniel J.

2017-03-01

Atomic force microscopy (AFM)-based methods have matured into a powerful nanoscopic platform, enabling the characterization of a wide range of biological and synthetic biointerfaces ranging from tissues, cells, membranes, proteins, nucleic acids and functional materials. Although the unprecedented signal-to-noise ratio of AFM enables the imaging of biological interfaces from the cellular to the molecular scale, AFM-based force spectroscopy allows their mechanical, chemical, conductive or electrostatic, and biological properties to be probed. The combination of AFM-based imaging and spectroscopy structurally maps these properties and allows their 3D manipulation with molecular precision. In this Review, we survey basic and advanced AFM-related approaches and evaluate their unique advantages and limitations in imaging, sensing, parameterizing and designing biointerfaces. It is anticipated that in the next decade these AFM-related techniques will have a profound influence on the way researchers view, characterize and construct biointerfaces, thereby helping to solve and address fundamental challenges that cannot be addressed with other techniques.

Probing the stiffness of isolated nucleoli by atomic force microscopy.

PubMed

Louvet, Emilie; Yoshida, Aiko; Kumeta, Masahiro; Takeyasu, Kunio

2014-04-01

In eukaryotic cells, ribosome biogenesis occurs in the nucleolus, a membraneless nuclear compartment. Noticeably, the nucleolus is also involved in several nuclear functions, such as cell cycle regulation, non-ribosomal ribonucleoprotein complex assembly, aggresome formation and some virus assembly. The most intriguing question about the nucleolus is how such dynamics processes can occur in such a compact compartment. We hypothesized that its structure may be rather flexible. To investigate this, we used atomic force microscopy (AFM) on isolated nucleoli. Surface topography imaging revealed the beaded structure of the nucleolar surface. With the AFM's ability to measure forces, we were able to determine the stiffness of isolated nucleoli. We could establish that the nucleolar stiffness varies upon drastic morphological changes induced by transcription and proteasome inhibition. Furthermore, upon ribosomal proteins and LaminB1 knockdowns, the nucleolar stiffness was increased. This led us to propose a model where the nucleolus has steady-state stiffness dependent on ribosome biogenesis activity and requires LaminB1 for its flexibility.

Angle-Dependent Atomic Force Microscopy Single-Chain Pulling of Adsorbed Macromolecules from Planar Surfaces Unveils the Signature of an Adsorption-Desorption Transition.

PubMed

Grebíková, Lucie; Whittington, Stuart G; Vancso, Julius G

2018-05-23

The adsorption-desorption behavior of polymer chains is at the heart of macromolecular surface science and technology. With the current developments in atomic force microscopy (AFM), it has now become possible to address the desorption problem from the perspective of a single macromolecule. Here, we report on desorption of single polymer chains on planar surfaces by AFM-based single molecule force spectroscopy (SMFS) as a function of the pulling angle with respect to the surface-normal direction. SMFS experiments were performed in water with various substrates using different polymers covalently attached to the AFM probe tip. End-grafting at the AFM tip was achieved by surface-initiated polymerization using initiator functionalized tips. We found that the desorption force increases with a decreasing pulling angle, i.e., an enhanced adhesion of the polymer chain was observed. The magnitude of the desorption force shows a weak angular dependence at pulling angles close to the surface normal. A significant increase of the force is observed at shallower pulling from a certain pulling angle. This behavior carries the signature of an adsorption-desorption transition. The angular dependence of the normalized desorption force exhibits a universal behavior. We compared and interpreted our results using theoretical predictions for single-chain adsorption-desorption transitions.

Angle-Dependent Atomic Force Microscopy Single-Chain Pulling of Adsorbed Macromolecules from Planar Surfaces Unveils the Signature of an Adsorption–Desorption Transition

PubMed Central

2018-01-01

The adsorption–desorption behavior of polymer chains is at the heart of macromolecular surface science and technology. With the current developments in atomic force microscopy (AFM), it has now become possible to address the desorption problem from the perspective of a single macromolecule. Here, we report on desorption of single polymer chains on planar surfaces by AFM-based single molecule force spectroscopy (SMFS) as a function of the pulling angle with respect to the surface-normal direction. SMFS experiments were performed in water with various substrates using different polymers covalently attached to the AFM probe tip. End-grafting at the AFM tip was achieved by surface-initiated polymerization using initiator functionalized tips. We found that the desorption force increases with a decreasing pulling angle, i.e., an enhanced adhesion of the polymer chain was observed. The magnitude of the desorption force shows a weak angular dependence at pulling angles close to the surface normal. A significant increase of the force is observed at shallower pulling from a certain pulling angle. This behavior carries the signature of an adsorption–desorption transition. The angular dependence of the normalized desorption force exhibits a universal behavior. We compared and interpreted our results using theoretical predictions for single-chain adsorption–desorption transitions. PMID:29712430

Artifacts in time-resolved Kelvin probe force microscopy

DOE PAGES

Sadewasser, Sascha; Nicoara, Nicoleta; Solares, Santiago D.

2018-04-24

Kelvin probe force microscopy (KPFM) has been used for the characterization of metals, insulators, and semiconducting materials on the nanometer scale. Especially in semiconductors, the charge dynamics are of high interest. Recently, several techniques for time-resolved measurements with time resolution down to picoseconds have been developed, many times using a modulated excitation signal, e.g. light modulation or bias modulation that induces changes in the charge carrier distribution. For fast modulation frequencies, the KPFM controller measures an average surface potential, which contains information about the involved charge carrier dynamics. Here, we show that such measurements are prone to artifacts due tomore » frequency mixing, by performing numerical dynamics simulations of the cantilever oscillation in KPFM subjected to a bias-modulated signal. For square bias pulses, the resulting time-dependent electrostatic forces are very complex and result in intricate mixing of frequencies that may, in some cases, have a component at the detection frequency, leading to falsified KPFM measurements. Additionally, we performed fast Fourier transform (FFT) analyses that match the results of the numerical dynamics simulations. Small differences are observed that can be attributed to transients and higher-order Fourier components, as a consequence of the intricate nature of the cantilever driving forces. These results are corroborated by experimental measurements on a model system. In the experimental case, additional artifacts are observed due to constructive or destructive interference of the bias modulation with the cantilever oscillation. Also, in the case of light modulation, we demonstrate artifacts due to unwanted illumination of the photodetector of the beam deflection detection system. Lastly, guidelines for avoiding such artifacts are given.« less

Artifacts in time-resolved Kelvin probe force microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sadewasser, Sascha; Nicoara, Nicoleta; Solares, Santiago D.

Kelvin probe force microscopy (KPFM) has been used for the characterization of metals, insulators, and semiconducting materials on the nanometer scale. Especially in semiconductors, the charge dynamics are of high interest. Recently, several techniques for time-resolved measurements with time resolution down to picoseconds have been developed, many times using a modulated excitation signal, e.g. light modulation or bias modulation that induces changes in the charge carrier distribution. For fast modulation frequencies, the KPFM controller measures an average surface potential, which contains information about the involved charge carrier dynamics. Here, we show that such measurements are prone to artifacts due tomore » frequency mixing, by performing numerical dynamics simulations of the cantilever oscillation in KPFM subjected to a bias-modulated signal. For square bias pulses, the resulting time-dependent electrostatic forces are very complex and result in intricate mixing of frequencies that may, in some cases, have a component at the detection frequency, leading to falsified KPFM measurements. Additionally, we performed fast Fourier transform (FFT) analyses that match the results of the numerical dynamics simulations. Small differences are observed that can be attributed to transients and higher-order Fourier components, as a consequence of the intricate nature of the cantilever driving forces. These results are corroborated by experimental measurements on a model system. In the experimental case, additional artifacts are observed due to constructive or destructive interference of the bias modulation with the cantilever oscillation. Also, in the case of light modulation, we demonstrate artifacts due to unwanted illumination of the photodetector of the beam deflection detection system. Lastly, guidelines for avoiding such artifacts are given.« less

Early Adhesion of Candida albicans onto Dental Acrylic Surfaces.

PubMed

Aguayo, S; Marshall, H; Pratten, J; Bradshaw, D; Brown, J S; Porter, S R; Spratt, D; Bozec, L

2017-07-01

Denture-associated stomatitis is a common candidal infection that may give rise to painful oral symptoms, as well as be a reservoir for infection at other sites of the body. As poly (methyl methacrylate) (PMMA) remains the main material employed in the fabrication of dentures, the aim of this research was to evaluate the adhesion of Candida albicans cells onto PMMA surfaces by employing an atomic force microscopy (AFM) single-cell force spectroscopy (SCFS) technique. For experiments, tipless AFM cantilevers were functionalized with PMMA microspheres and probed against C. albicans cells immobilized onto biopolymer-coated substrates. Both a laboratory strain and a clinical isolate of C. albicans were used for SCFS experiments. Scanning electron microscopy (SEM) and AFM imaging of C. albicans confirmed the polymorphic behavior of both strains, which was dependent on growth culture conditions. AFM force-spectroscopy results showed that the adhesion of C. albicans to PMMA is morphology dependent, as hyphal tubes had increased adhesion compared with yeast cells ( P < 0.05). C. albicans budding mother cells were found to be nonadherent, which contrasts with the increased adhesion observed in the tube region. Comparison between strains demonstrated increased adhesion forces for a clinical isolate compared with the lab strain. The clinical isolate also had increased survival in blood and reduced sensitivity to complement opsonization, providing additional evidence of strain-dependent differences in Candida-host interactions that may affect virulence. In conclusion, PMMA-modified AFM probes have shown to be a reliable technique to characterize the adhesion of C. albicans to acrylic surfaces.

An active one-particle microrheometer: incorporating magnetic tweezers to total internal reflection microscopy.

PubMed

Gong, Xiangjun; Hua, Li; Wu, Chi; Ngai, To

2013-03-01

We present a novel microrheometer by incorporating magnetic tweezers in the total internal reflection microscopy (TIRM) that enables measuring of viscoelastic properties of materials near solid surface. An evanescent wave generated by a solid∕liquid interface in the TIRM is used as the incident light source in the microrheometer. When a probe particle (of a few micrometers diameter) moves near the interface, it can interact with the evanescent field and reflect its position with respect to the interface by the scattered light intensity. The exponential distance dependence of the evanescent field, on the one hand, makes this technique extremely sensitive to small changes from z-fluctuations of the probe (with a resolution of several nanometers), and on the other, it does not require imaging of the probe with high lateral resolution. Another distinct advantage is the high sensitivity in determining the z position of the probe in the absence of any labeling. The incorporated magnetic tweezers enable us to effectively manipulate the distance of the embedded particle from the interface either by a constant or an oscillatory force. The force ramp is easy to implement through a coil current ramp. In this way, the local viscous and elastic properties of a given system under different confinements can therefore be measured by resolving the near-surface particle motion. To test the feasibility of applying this microrheology to soft materials, we measured the viscoelastic properties of sucrose and poly(ethylene glycol) solutions and compared the results to bulk rheometry. In addition, we applied this technique in monitoring the structure and properties of deformable microgel particles near the flat surface.

Bi-harmonic cantilever design for improved measurement sensitivity in tapping-mode atomic force microscopy.

PubMed

Loganathan, Muthukumaran; Bristow, Douglas A

2014-04-01

This paper presents a method and cantilever design for improving the mechanical measurement sensitivity in the atomic force microscopy (AFM) tapping mode. The method uses two harmonics in the drive signal to generate a bi-harmonic tapping trajectory. Mathematical analysis demonstrates that the wide-valley bi-harmonic tapping trajectory is as much as 70% more sensitive to changes in the sample topography than the standard single-harmonic trajectory typically used. Although standard AFM cantilevers can be driven in the bi-harmonic tapping trajectory, they require large forcing at the second harmonic. A design is presented for a bi-harmonic cantilever that has a second resonant mode at twice its first resonant mode, thereby capable of generating bi-harmonic trajectories with small forcing signals. Bi-harmonic cantilevers are fabricated by milling a small cantilever on the interior of a standard cantilever probe using a focused ion beam. Bi-harmonic drive signals are derived for standard cantilevers and bi-harmonic cantilevers. Experimental results demonstrate better than 30% improvement in measurement sensitivity using the bi-harmonic cantilever. Images obtained through bi-harmonic tapping exhibit improved sharpness and surface tracking, especially at high scan speeds and low force fields.

AFM Colloidal Probe Measurements Implicate Capillary Condensation in Punch-Particle Surface Interactions during Tableting.

PubMed

Badal Tejedor, Maria; Nordgren, Niklas; Schuleit, Michael; Millqvist-Fureby, Anna; Rutland, Mark W

2017-11-21

Adhesion of the powders to the punches is a common issue during tableting. This phenomenon is known as sticking and affects the quality of the manufactured tablets. Defective tablets increase the cost of the manufacturing process. Thus, the ability to predict the tableting performance of the formulation blend before the process is scaled-up is important. The adhesive propensity of the powder to the tableting tools is mostly governed by the surface-surface adhesive interactions. Atomic force microscopy (AFM) colloidal probe is a surface characterization technique that allows the measurement of the adhesive interactions between two materials of interest. In this study, AFM steel colloidal probe measurements were performed on ibuprofen, MCC (microcrystalline cellulose), α-lactose monohydrate, and spray-dried lactose particles as an approach to modeling the punch-particle surface interactions during tableting. The excipients (lactose and MCC) showed constant, small, attractive, and adhesive forces toward the steel surface after a repeated number of contacts. In comparison, ibuprofen displayed a much larger attractive and adhesive interaction increasing over time both in magnitude and in jump-in/jump-out separation distance. The type of interaction acting on the excipient-steel interface can be related to a van der Waals force, which is relatively weak and short-ranged. By contrast, the ibuprofen-steel interaction is described by a capillary force profile. Even though ibuprofen is not highly hydrophilic, the relatively smooth surfaces of the crystals allow "contact flooding" upon contact with the steel probe. Capillary forces increase because of the "harvesting" of moisture-due to the fast condensation kinetics-leaving a residual condensate that contributes to increase the interaction force after each consecutive contact. Local asperity contacts on the more hydrophilic surface of the excipients prevent the flooding of the contact zone, and there is no such adhesive effect under the same ambient conditions. The markedly different behavior detected by force measurements clearly shows the sticky and nonsticky propensity of the materials and allows a mechanistic description.

Covalent immobilization of native biomolecules onto Au(111) via N-hydroxysuccinimide ester functionalized self-assembled monolayers for scanning probe microscopy.

PubMed Central

Wagner, P; Hegner, M; Kernen, P; Zaugg, F; Semenza, G

1996-01-01

We have worked out a procedure for covalent binding of native biomacromolecules on flat gold surfaces for scanning probe microscopy in aqueous buffer solutions and for other nanotechnological applications, such as the direct measurement of interaction forces between immobilized macromolecules, of their elastomechanical properties, etc. It is based on the covalent immobilization of amino group-containing biomolecules (e.g., proteins, phospholipids) onto atomically flat gold surfaces via omega-functionalized self-assembled monolayers. We present the synthesis of the parent compound, dithio-bis(succinimidylundecanoate) (DSU), and a detailed study of the chemical and physical properties of the monolayer it forms spontaneously on Au(111). Scanning tunneling microscopy and atomic force microscopy (AFM) revealed a monolayer arrangement with the well-known depressions that are known to stem from an etch process during the self-assembly. The total density of the omega-N-hydroxysuccinimidyl groups on atomically flat gold was 585 pmol/cm(2), as determined by chemisorption of (14)C-labeled DSU. This corresponded to approximately 75% of the maximum density of the omega-unsubstituted alkanethiol. Measurements of the kinetics of monolayer formation showed a very fast initial phase, with total coverage within 30 S. A subsequent slower rearrangement of the chemisorbed molecules, as indicated by AFM, led to a decrease in the number of monolayer depressions in approximately 60 min. The rate of hydrolysis of the omega-N-hydroxysuccinimide groups at the monolayer/water interface was found to be very slow, even at moderately alkaline pH values. Furthermore, the binding of low-molecular-weight amines and of a model protein was investigated in detail. Images FIGURE 1 FIGURE 2 FIGURE 9 PMID:9172730

Full information acquisition in scanning probe microscopy and spectroscopy

DOEpatents

Jesse, Stephen; Belianinov, Alex; Kalinin, Sergei V.; Somnath, Suhas

2017-04-04

Apparatus and methods are described for scanning probe microscopy and spectroscopy based on acquisition of full probe response. The full probe response contains valuable information about the probe-sample interaction that is lost in traditional scanning probe microscopy and spectroscopy methods. The full probe response is analyzed post data acquisition using fast Fourier transform and adaptive filtering, as well as multivariate analysis. The full response data is further compressed to retain only statistically significant components before being permanently stored.

Modeling and boundary force control of microcantilevers utilized in atomic force microscopy for cellular imaging and characterization

NASA Astrophysics Data System (ADS)

Eslami, Sohrab

This dissertation undertakes the theoretical and experimental developments microcantilevers utilized in Atomic Force Microscopy (AFM) with applications to cellular imaging and characterization. The capability of revealing the inhomogeneties or interior of ultra-small materials has been of most interest to many researchers. However, the fundamental concept of signal and image formation remains unexplored and not fully understood. For his, a semi-empirical nonlinear force model is proposed to show that virtual frequency generation, regarded as the simplest synthesized subsurface probe, occurs optimally when the force is tuned to the van der Waals form. This is the first-time observation of a novel theoretical dynamic multi-frequency force microscopy that has not been already reported. Owing to the broad applications of microcantilevers in the nanoscale imaging and microscopic techniques, there is an essential feeling to study and propose a comprehensive model of such systems. Therefore, in the theoretical part of this dissertation, a distributed-parameters representation modeling of the microcantilever along with a general interaction force comprising of two attractive and repulsive components with general amplitude and power terms is studied. This model is investigated in a general 2D Cartesian coordinate to consider the motions of the probe with a tip mass. There is an excitation at the microcantilever's base such that the end of the beam is subject to the proposed general force. These forces are very sensitive to the amplitude and power terms of these parts; on the other hand, atomic intermolecular force is a function of the distance such that this distance itself is also a function of the interaction force that will result in a nonlinear implicit equation. From a parametric study in the probe-sample excitation, it is shown that the predicted behavior of the generated difference-frequency oscillation amplitude agrees well with experimental measurements. Following the proposed Euler-Bernoulli model, a more comprehensive model is developed by modeling the probe dynamics and including the effects of the rotary inertia and shear deformation under the same proposed tip-sample interaction force. An extensive comparative study between the Euler-Bernoulli and Timoshenko beam assumptions is conducted for different conditions including different base-excitation amplitudes and higher modes. The results underline that the comprehensive Timoshenko model unveils the effects of the nonlinear interaction force better than the Euler-Bernoulli beam model. In addition to extensive modeling efforts on the microcantilever and its interaction with sample, an adaptive control framework is developed in order to make the microcantilever's tip follow a desired trajectory. This trajectory can further be considered as an important path acquired by the path planning techniques to manipulate the nanoparticles. There is a base excitation considered for this model and can be considered as an input force control to excite the probe by taking advantage of flexibility of the cantilever despite its complexity and under existence of the external nonlinear interaction forces between the tip and sample's surface. When building such complicated controller on top of the proposed comprehensive model, the results could be extended to study a macro-micro hybrid rigid-flexible model of a microrobot to mimic the realistic behavior of the MM3ARTM microrobot. The MM3ARTM microrobot is equipped with a piezoresistive layer which functions as a force sensor and is capable of measuring very slight forces as small as micro to nano-Newton. Two types of controllers are investigated for the case of the tip force control. Lyapunov-based PD and robust adaptive controllers are developed for this purpose and their performances and stabilities are compared. In the experimental part, a platform for performing the automated nanomanipulation and real-time cellular imaging is developed by integrating a microrobot, digital signal processor platform (dSPACERTM), computer, and a state-of-the-art light microscope. The closed-loop boundary force control framework is additionally developed for the autonomous in-situ applications. Since the incoming and outgoing signals of the piezoresistive microrobot are in the form of the electrical voltage and the string commands (ASCII code), respectively, an intuitive programming code for interfacing the MATLAB and dSPACE RTM has been written for the online quasi-data acquisition. As a result, the height of the corneal cell has been obtained and additionally, the microcantilever's tip force has been automatically controlled by taking advantage of the proposed control framework.

History, rare, and multiple events of mechanical unfolding of repeat proteins

NASA Astrophysics Data System (ADS)

Sumbul, Fidan; Marchesi, Arin; Rico, Felix

2018-03-01

Mechanical unfolding of proteins consisting of repeat domains is an excellent tool to obtain large statistics. Force spectroscopy experiments using atomic force microscopy on proteins presenting multiple domains have revealed that unfolding forces depend on the number of folded domains (history) and have reported intermediate states and rare events. However, the common use of unspecific attachment approaches to pull the protein of interest holds important limitations to study unfolding history and may lead to discarding rare and multiple probing events due to the presence of unspecific adhesion and uncertainty on the pulling site. Site-specific methods that have recently emerged minimize this uncertainty and would be excellent tools to probe unfolding history and rare events. However, detailed characterization of these approaches is required to identify their advantages and limitations. Here, we characterize a site-specific binding approach based on the ultrastable complex dockerin/cohesin III revealing its advantages and limitations to assess the unfolding history and to investigate rare and multiple events during the unfolding of repeated domains. We show that this approach is more robust, reproducible, and provides larger statistics than conventional unspecific methods. We show that the method is optimal to reveal the history of unfolding from the very first domain and to detect rare events, while being more limited to assess intermediate states. Finally, we quantify the forces required to unfold two molecules pulled in parallel, difficult when using unspecific approaches. The proposed method represents a step forward toward more reproducible measurements to probe protein unfolding history and opens the door to systematic probing of rare and multiple molecule unfolding mechanisms.

Peering at Brain Polysomes with Atomic Force Microscopy

PubMed Central

Lunelli, Lorenzo; Bernabò, Paola; Bolner, Alice; Vaghi, Valentina; Marchioretto, Marta; Viero, Gabriella

2016-01-01

The translational machinery, i.e., the polysome or polyribosome, is one of the biggest and most complex cytoplasmic machineries in cells. Polysomes, formed by ribosomes, mRNAs, several proteins and non-coding RNAs, represent integrated platforms where translational controls take place. However, while the ribosome has been widely studied, the organization of polysomes is still lacking comprehensive understanding. Thus much effort is required in order to elucidate polysome organization and any novel mechanism of translational control that may be embedded. Atomic force microscopy (AFM) is a type of scanning probe microscopy that allows the acquisition of 3D images at nanoscale resolution. Compared to electron microscopy (EM) techniques, one of the main advantages of AFM is that it can acquire thousands of images both in air and in solution, enabling the sample to be maintained under near physiological conditions without any need for staining and fixing procedures. Here, a detailed protocol for the accurate purification of polysomes from mouse brain and their deposition on mica substrates is described. This protocol enables polysome imaging in air and liquid with AFM and their reconstruction as three-dimensional objects. Complementary to cryo-electron microscopy (cryo-EM), the proposed method can be conveniently used for systematically analyzing polysomes and studying their organization. PMID:27023752

High-speed adaptive contact-mode atomic force microscopy imaging with near-minimum-force

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ren, Juan; Zou, Qingze, E-mail: qzzou@rci.rutgers.edu

In this paper, an adaptive contact-mode imaging approach is proposed to replace the traditional contact-mode imaging by addressing the major concerns in both the speed and the force exerted to the sample. The speed of the traditional contact-mode imaging is largely limited by the need to maintain precision tracking of the sample topography over the entire imaged sample surface, while large image distortion and excessive probe-sample interaction force occur during high-speed imaging. In this work, first, the image distortion caused by the topography tracking error is accounted for in the topography quantification. Second, the quantified sample topography is utilized inmore » a gradient-based optimization method to adjust the cantilever deflection set-point for each scanline closely around the minimal level needed for maintaining stable probe-sample contact, and a data-driven iterative feedforward control that utilizes a prediction of the next-line topography is integrated to the topography feeedback loop to enhance the sample topography tracking. The proposed approach is demonstrated and evaluated through imaging a calibration sample of square pitches at both high speeds (e.g., scan rate of 75 Hz and 130 Hz) and large sizes (e.g., scan size of 30 μm and 80 μm). The experimental results show that compared to the traditional constant-force contact-mode imaging, the imaging speed can be increased by over 30 folds (with the scanning speed at 13 mm/s), and the probe-sample interaction force can be reduced by more than 15% while maintaining the same image quality.« less

The influence of crystal habit on the prediction of dry powder inhalation formulation performance using the cohesive-adhesive force balance approach.

PubMed

Hooton, Jennifer C; Jones, Matthew D; Harris, Haggis; Shur, Jagdeep; Price, Robert

2008-09-01

The aim of this investigation was to study the influence of crystalline habit of active pharmaceutical ingredients on the cohesive-adhesive force balance within model dry powder inhaler (DPI) formulations and the corresponding affect on DPI formulation performance. The cohesive-adhesive balance (CAB) approach to colloid probe atomic force microscopy (AFM) was employed to determine the cohesive and adhesive interactions of micronized budesonide particles against the {102} and {002} faces of budesonide single crystals and crystalline substrates of different sugars (cyclodextrin, lactose, trehalose, raffinose, and xylitol), respectively. These data were used to measure the relative level of cohesion and adhesion via CAB and the possible influence on in vitro performance of a carrier-based DPI formulation. Varying the crystal habit of the drug had a significant effect on the cohesive measurement of micronized budesonide probes, with the cohesive values on the {102} faces being approximately twice that on the {002} crystal faces. However, although different CAB values were measured with the sugars with respect to the crystal faces chosen for the cohesive-based measurement, the overall influence on the rank order of the CAB values was not directly influenced. For these data sets, the CAB gradient indicated that a decrease in the dominance of the adhesive forces led to a concomitant increase in fine particle delivery, reaching a plateau as the cohesive forces became dominant. The study suggested that crystal habit of the primary drug crystals influences the cohesive interactions and the resulting force balance measurements of colloid probe CAB analysis.

High-speed adaptive contact-mode atomic force microscopy imaging with near-minimum-force.

PubMed

Ren, Juan; Zou, Qingze

2014-07-01

In this paper, an adaptive contact-mode imaging approach is proposed to replace the traditional contact-mode imaging by addressing the major concerns in both the speed and the force exerted to the sample. The speed of the traditional contact-mode imaging is largely limited by the need to maintain precision tracking of the sample topography over the entire imaged sample surface, while large image distortion and excessive probe-sample interaction force occur during high-speed imaging. In this work, first, the image distortion caused by the topography tracking error is accounted for in the topography quantification. Second, the quantified sample topography is utilized in a gradient-based optimization method to adjust the cantilever deflection set-point for each scanline closely around the minimal level needed for maintaining stable probe-sample contact, and a data-driven iterative feedforward control that utilizes a prediction of the next-line topography is integrated to the topography feeedback loop to enhance the sample topography tracking. The proposed approach is demonstrated and evaluated through imaging a calibration sample of square pitches at both high speeds (e.g., scan rate of 75 Hz and 130 Hz) and large sizes (e.g., scan size of 30 μm and 80 μm). The experimental results show that compared to the traditional constant-force contact-mode imaging, the imaging speed can be increased by over 30 folds (with the scanning speed at 13 mm/s), and the probe-sample interaction force can be reduced by more than 15% while maintaining the same image quality.

Visualization of molecular packing and tilting domains and interface effects in tetracene thin films on H/Si(001)

DOE PAGES

Tersigni, Andrew; Sadowski, Jerzy T.; Qin, Xiao-Rong

2017-03-27

Visualizing molecular crystalline domains and influence of substrate defects are important in understanding the charge transport in organic thin film devices. Vacuum evaporated tetracene films of four monolayers on hydrogen-terminated Si(001)-2x1 substrate, as a prototypical system, have been studied with ex situ atomic force microscopy (AFM), transverse shear microscopy (TSM), friction force microscopy (FFM), and low-energy electron microscopy (LEEM). Two differently oriented in-plane lattice domains are found due to the symmetry of the substrate lattice, with no visible azimuthal twist between adjacent molecular layers in surface islands, indicating significant bulk-like crystallization in the film. Meanwhile, two types of subdomains aremore » observed inside of each in-plane lattice domain. The subdomains are anisotropic in shape, and their sizes and distribution are highly influenced by the substrate atomic steps. TSM and FFM measurements indicate that these subdomains result from molecule-tilt orderings within the bulk-like lattice domains. Lastly, TSM evidently shows a sensitivity to probe vertical molecule-tilt anisotropy for the molecular crystals, in addition to its known ability to map the lateral lattice orientations.« less

Atomic force microscopy-guided fractionation reveals the influence of cranberry phytochemicals on adhesion of Escherichia coli.

PubMed

Gupta, Prachi; Song, Biqin; Neto, Catherine; Camesano, Terri A

2016-06-15

Cranberry juice has been long used to prevent infections because of its effect on the adhesion of the bacteria to the host surface. Proanthocyanidins (PACs) comprise of one of the major classes of phytochemicals found in cranberry, which have been extensively studied and found effective in combating adhesion of pathogenic bacteria. The role of other cranberry constituents in impacting bacterial adhesion haven't been studied very well. In this study, cranberry juice fractions were prepared, characterized and tested for their effect on the surface adhesion of the pathogenic clinical bacterial strain E. coli B78 and non-pathogenic control E. coli HB101. The preparations tested included crude cranberry juice extract (CCE); three fractions containing flavonoid classes including proanthocyanidins, anthocyanins and flavonols; selected sub-fractions, and commercially available flavonol glycoside, quercetin-3-O-galactoside. Atomic force microscopy (AFM) was used to quantify the adhesion forces between the bacterial surface and the AFM probe after the treatment with the cranberry fractions. Adhesion forces of the non-pathogenic, non fimbriated lab strain HB101 are small (average force 0.19 nN) and do not change with cranberry treatments, whereas the adhesion forces of the pathogenic, Dr adhesion E. coli strain B78 (average force of 0.42 nN) show a significant decrease when treated with cranberry juice extract or fractions (average force of 0.31 nN, 0.37 nN and 0.39 nN with CCE, Fraction 7 and Fraction 4 respectively). In particular, the fractions that contained flavonols in addition to PACs were more efficient at lowering the force of adhesion (average force of 0.31 nN-0.18 nN between different sub-fractions containing flavonols and PACs). The sub-fractions containing flavonol glycosides (from juice, fruit and commercial quercetin) all resulted in reduced adhesion of the pathogenic bacteria to the model probe. This strongly suggests the anti adhesive role of other classes of cranberry compounds in conjunction with already known PACs and may have implications for development of alternative anti bacterial treatments.

Nano-Localized Thermal Analysis and Mapping of Surface and Sub-Surface Thermal Properties Using Scanning Thermal Microscopy (SThM).

PubMed

Pereira, Maria J; Amaral, Joao S; Silva, Nuno J O; Amaral, Vitor S

2016-12-01

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.

Atomic Force Microscopy Thermally-Assisted Microsampling with Atmospheric Pressure Temperature Ramped Thermal Desorption/Ionization-Mass Spectrometry Analysis

DOE PAGES

Hoffmann, William D.; Kertesz, Vilmos; Srijanto, Bernadeta R.; ...

2017-02-20

The use of atomic force microscopy controlled nano-thermal analysis probes for reproducible spatially resolved thermally-assisted sampling of micrometer-sized areas (ca. 11 m 17 m wide 2.4 m deep) from relatively low number average molecular weight (M n < 3000) polydisperse thin films of poly(2-vinylpyridine) (P2VP) is presented. Following sampling, the nano-thermal analysis probes were moved up from the surface and the probe temperature ramped to liberate the sampled materials into the gas phase for atmospheric pressure chemical ionization and mass spectrometric analysis. Furthermore, the procedure and mechanism for material pickup, the sampling reproducibility and sampling size are discussed and themore » oligomer distribution information available from slow temperature ramps versus ballistic temperature jumps is presented. For the M n = 970 P2VP, the Mn and polydispersity index determined from the mass spectrometric data were in line with both the label values from the sample supplier and the value calculated from the simple infusion of a solution of polymer into the commercial atmospheric pressure chemical ionization source on this mass spectrometer. With a P2VP sample of higher Mn (M n = 2070 and 2970), intact oligomers were still observed (as high as m/z 2793 corresponding to the 26-mer), but a significant abundance of thermolysis products were also observed. In addition, the capability for confident identification of the individual oligomers by slowly ramping the probe temperature and collecting data dependent tandem mass spectra was also demonstrated. We also discuss the material type limits to the current sampling and analysis approach as well as possible improvements in nano-thermal analysis probe design to enable smaller area sampling and to enable controlled temperature ramps beyond the present upper limit of about 415°C.« less

Atomic Force Microscopy Thermally-Assisted Microsampling with Atmospheric Pressure Temperature Ramped Thermal Desorption/Ionization-Mass Spectrometry Analysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hoffmann, William D.; Kertesz, Vilmos; Srijanto, Bernadeta R.

The use of atomic force microscopy controlled nano-thermal analysis probes for reproducible spatially resolved thermally-assisted sampling of micrometer-sized areas (ca. 11 m 17 m wide 2.4 m deep) from relatively low number average molecular weight (M n < 3000) polydisperse thin films of poly(2-vinylpyridine) (P2VP) is presented. Following sampling, the nano-thermal analysis probes were moved up from the surface and the probe temperature ramped to liberate the sampled materials into the gas phase for atmospheric pressure chemical ionization and mass spectrometric analysis. Furthermore, the procedure and mechanism for material pickup, the sampling reproducibility and sampling size are discussed and themore » oligomer distribution information available from slow temperature ramps versus ballistic temperature jumps is presented. For the M n = 970 P2VP, the Mn and polydispersity index determined from the mass spectrometric data were in line with both the label values from the sample supplier and the value calculated from the simple infusion of a solution of polymer into the commercial atmospheric pressure chemical ionization source on this mass spectrometer. With a P2VP sample of higher Mn (M n = 2070 and 2970), intact oligomers were still observed (as high as m/z 2793 corresponding to the 26-mer), but a significant abundance of thermolysis products were also observed. In addition, the capability for confident identification of the individual oligomers by slowly ramping the probe temperature and collecting data dependent tandem mass spectra was also demonstrated. We also discuss the material type limits to the current sampling and analysis approach as well as possible improvements in nano-thermal analysis probe design to enable smaller area sampling and to enable controlled temperature ramps beyond the present upper limit of about 415°C.« less

Coupling of conservative and dissipative forces in frequency-modulation atomic force microscopy

NASA Astrophysics Data System (ADS)

Sader, John E.; Jarvis, Suzanne P.

2006-11-01

Frequency modulation atomic force microscopy (FM-AFM) utilizes the principle of self-excitation to ensure the cantilever probe vibrates at its resonant frequency, regardless of the tip-sample interaction. Practically, this is achieved by fixing the phase difference between tip deflection and driving force at precisely 90° . This, in turn, decouples the frequency shift and excitation amplitude signals, enabling quantitative interpretation in terms of conservative and dissipative tip-sample interaction forces. In this article, we theoretically investigate the effect of phase detuning in the self-excitation mechanism on the coupling between conservative and dissipative forces in FM-AFM. We find that this coupling depends only on the relative difference in the drive and resonant frequencies far from the surface, and is thus very weakly dependent on the actual phase error particularly for high quality factors. This establishes that FM-AFM is highly robust with respect to phase detuning, and enables quantitative interpretation of the measured frequency shift and excitation amplitude, even while operating away from the resonant frequency with the use of appropriate replacements in the existing formalism. We also examine the calibration of phase shifts in FM-AFM measurements and demonstrate that the commonly used approach of minimizing the excitation amplitude can lead to significant phase detuning, particularly in liquid environments.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pal, Sambit Bikas; Haldar, Arijit; Roy, Basudev

A photonic force microscope comprises of an optically trapped micro-probe and a position detection system to track the motion of the probe. Signal collection for motion detection is often carried out using the backscattered light off the probe-however, this mode has problems of low S/N due to the small backscattering cross sections of the micro-probes typically used. The position sensors often used in these cases are quadrant photodetectors. To ensure maximum sensitivity of such detectors, it would help if the detector size matched with the detection beam radius after the condenser lens (which for backscattered detection would be the trappingmore » objective itself). To suit this condition, we have used a miniature displacement sensor whose dimensions makes it ideal to work with 1:1 images of micrometer-sized trapped probes in the backscattering detection mode. The detector is based on the quadrant photo-integrated chip in the optical pick-up head of a compact disc player. Using this detector, we measured absolute displacements of an optically trapped 1.1 {mu}m probe with a resolution of {approx}10 nm for a bandwidth of 10 Hz at 95% significance without any sample or laser stabilization. We characterized our optical trap for different sized probes by measuring the power spectrum for each probe to 1% accuracy, and found that for 1.1 {mu}m diameter probes, the noise in our position measurement matched the thermal resolution limit for averaging times up to 10 ms. We also achieved a linear response range of around 385 nm with cross talk between axes {approx_equal}4% for 1.1 {mu}m diameter probes. The detector has extremely high bandwidth (few MHz) and low optical power threshold-other factors that can lead to its widespread use in photonic force microscopy.« less

Optical imaging beyond the diffraction limit by SNEM: effects of AFM tip modifications with thiol monolayers on imaging quality.

PubMed

Cumurcu, Aysegul; Diaz, Jordi; Lindsay, Ian D; de Beer, Sissi; Duvigneau, Joost; Schön, Peter; Julius Vancso, G

2015-03-01

Tip-enhanced nanoscale optical imaging techniques such as apertureless scanning near-field optical microscopy (a-SNOM) and scanning near-field ellipsometric microscopy (SNEM) applications can suffer from a steady degradation in performance due to adhesion of atmospheric contaminants to the metal coated tip. Here, we demonstrate that a self-assembled monolayer (SAM) of ethanethiol (EtSH) is an effective means of protecting gold-coated atomic force microscopy (AFM) probe tips from accumulation of surface contaminants during prolonged exposure to ambient air. The period over which they yield consistent and reproducible results for scanning near-field ellipsometric microscopy (SNEM) imaging is thus extended. SNEM optical images of a microphase separated polystyrene-block-poly (methylmethacrylate) (PS-b-PMMA) diblock copolymer film, which were captured with bare and SAM-protected gold-coated AFM probes, both immediately after coating and following five days of storage in ambient air, were compared. During this period the intensity of the optical signals from the untreated gold tip fell by 66%, while those from the SAM protected tip fell by 14%. Additionally, gold coated AFM probe tips were modified with various lengths of alkanethiols to measure the change in intensity variation in the optical images with SAM layer thickness. The experimental results were compared to point dipole model calculations. While a SAM of 1-dodecanethiol (DoSH) was found to strongly suppress field enhancement we find that it can be locally removed from the tip apex by deforming the molecules under load, restoring SNEM image contrast. Copyright © 2014 Elsevier B.V. All rights reserved.

Characterization of structural and electrostatic complexity in pentacene thin films by scanning probe microscopy

NASA Astrophysics Data System (ADS)

Puntambekar, Kanan Prakash

The advancement of organic electronics for applications in solar energy conversion, printed circuitry, displays, and solid-state lighting depends upon optimization of structure and properties for a variety of organic semiconductor interfaces. Organic semiconductor/insulator (O/I) and organic-metal (O/M) interfaces, in particular, are critical to the operation of organic thin film transistors (OTFTs) currently being developed for printed flexible electronics. Scanning probe microscopy (SPM) is a powerful tool to isolate and characterize the bottlenecks to charge transport at these interfaces. This thesis establishes a direct correlation between the structural disorder and electrical complexity at these interfaces, using various SPM based methods and discusses the implications of such complexity on device performance. To examine the O/M interfaces, surface potentials of operating pentacene TFTs with two different contact geometries (bottom or top) were mapped by Kelvin probe force microscopy (KFM). The surface potential distribution was used to isolate the potential drops at the source and drain contacts. Simultaneously obtained topography and surface potential maps elucidated the correlation between the morphology and contact resistance at the O/M interface; the bottom contact TFTs were observed to be contact limited at large gate voltages, while the top contact TFTs were not contact limited. A direct correlation between structural defects and electric potential variations at the pentacene and silicon dioxide, a common insulator, is demonstrated. Lateral force microscopy (LFM) generates striking images of the polycrystalline microstructure of a monolayer thick pentacene film, allowing clear visualization of the grain boundary network. Further more, surface potential wells localized at the grain boundaries were observed by KFM, suggesting that the grain boundaries may serve as charge carrier (hole) traps. Line dislocations were also revealed in the second monolayer by chemical etching and SPM and produce strong variations in the surface potential that must affect the interfacial charge conductance. Structural disorder at the O/I and O/M interfaces degrades both injection and transport of charge, and therefore needs to be minimized. Thus both visualization and correlation of structural and electrical complexity at these interfaces have important implications for understanding electrical transport in OTFTs and for defining strategies to improve device performance.

Attractive forces between hydrophobic solid surfaces measured by AFM on the first approach in salt solutions and in the presence of dissolved gases.

PubMed

Azadi, Mehdi; Nguyen, Anh V; Yakubov, Gleb E

2015-02-17

Interfacial gas enrichment of dissolved gases (IGE) has been shown to cover hydrophobic solid surfaces in water. The atomic force microscopy (AFM) data has recently been supported by molecular dynamics simulation. It was demonstrated that IGE is responsible for the unexpected stability and large contact angle of gaseous nanobubbles at the hydrophobic solid-water interface. Here we provide further evidence of the significant effect of IGE on an attractive force between hydrophobic solid surfaces in water. The force in the presence of dissolved gas, i.e., in aerated and nonaerated NaCl solutions (up to 4 M), was measured by the AFM colloidal probe technique. The effect of nanobubble bridging on the attractive force was minimized or eliminated by measuring forces on the first approach of the AFM probe toward the flat hydrophobic surface and by using high salt concentrations to reduce gas solubility. Our results confirm the presence of three types of forces, two of which are long-range attractive forces of capillary bridging origin as caused by either surface nanobubbles or gap-induced cavitation. The third type is a short-range attractive force observed in the absence of interfacial nanobubbles that is attributed to the IGE in the form of a dense gas layer (DGL) at hydrophobic surfaces. Such a force was found to increase with increasing gas saturation and to decrease with decreasing gas solubility.

Frequency modulation detection atomic force microscopy in the liquid environment

NASA Astrophysics Data System (ADS)

Jarvis, S. P.; Ishida, T.; Uchihashi, T.; Nakayama, Y.; Tokumoto, H.

True atomic resolution imaging using frequency modulation detection is already well established in ultra-high vacuum. In this paper we demonstrate that it also has great potential in the liquid environment. Using a combination of magnetic activation and high-aspect-ratio carbon nanotube probes, we show that imaging can be readily combined with point spectroscopy, revealing both the tip-sample interaction and the structure of the intermediate liquid.

Actuation of atomic force microscopy microcantilevers using contact acoustic nonlinearities

DOE Office of Scientific and Technical Information (OSTI.GOV)

Torello, D.; Degertekin, F. Levent, E-mail: levent.degertekin@me.gatech.edu

2013-11-15

A new method of actuating atomic force microscopy (AFM) cantilevers is proposed in which a high frequency (>5 MHz) wave modulated by a lower frequency (∼300 kHz) wave passes through a contact acoustic nonlinearity at the contact interface between the actuator and the cantilever chip. The nonlinearity converts the high frequency, modulated signal to a low frequency drive signal suitable for actuation of tapping-mode AFM probes. The higher harmonic content of this signal is filtered out mechanically by the cantilever transfer function, providing for clean output. A custom probe holder was designed and constructed using rapid prototyping technologies and off-the-shelfmore » components and was interfaced with an Asylum Research MFP-3D AFM, which was then used to evaluate the performance characteristics with respect to standard hardware and linear actuation techniques. Using a carrier frequency of 14.19 MHz, it was observed that the cantilever output was cleaner with this actuation technique and added no significant noise to the system. This setup, without any optimization, was determined to have an actuation bandwidth on the order of 10 MHz, suitable for high speed imaging applications. Using this method, an image was taken that demonstrates the viability of the technique and is compared favorably to images taken with a standard AFM setup.« less

Differentiating Ferroelectric and Nonferroelectric Electromechanical Effects with Scanning Probe Microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Balke, Nina; Maksymovych, Petro; Jesse, Stephen

Ferroelectricity in functional materials remains one of the most fascinating areas of modern science in the past several decades. In the last several years, the rapid development of piezoresponse force microscopy (PFM) and spectroscopy revealed the presence of electromechanical hysteresis loops and bias-induced remnant polar states in a broad variety of materials including many inorganic oxides, polymers, and biosystems. In many cases, this behavior was interpreted as the ample evidence for ferroelectric nature of the system. Here, we systematically analyze PFM responses on ferroelectric and nonferroelectric materials and demonstrate that mechanisms unrelated to ferroelectricity can induce ferroelectric-like characteristics through chargemore » injection and electrostatic forces on the tip. In this paper, we will focus on similarities and differences in various PFM measurement characteristics to provide an experimental guideline to differentiate between ferroelectric material properties and charge injection. In conclusion, we apply the developed measurement protocols to an unknown ferroelectric material.« less

Differentiating Ferroelectric and Nonferroelectric Electromechanical Effects with Scanning Probe Microscopy

DOE PAGES

Balke, Nina; Maksymovych, Petro; Jesse, Stephen; ...

2015-06-02

Ferroelectricity in functional materials remains one of the most fascinating areas of modern science in the past several decades. In the last several years, the rapid development of piezoresponse force microscopy (PFM) and spectroscopy revealed the presence of electromechanical hysteresis loops and bias-induced remnant polar states in a broad variety of materials including many inorganic oxides, polymers, and biosystems. In many cases, this behavior was interpreted as the ample evidence for ferroelectric nature of the system. Here, we systematically analyze PFM responses on ferroelectric and nonferroelectric materials and demonstrate that mechanisms unrelated to ferroelectricity can induce ferroelectric-like characteristics through chargemore » injection and electrostatic forces on the tip. In this paper, we will focus on similarities and differences in various PFM measurement characteristics to provide an experimental guideline to differentiate between ferroelectric material properties and charge injection. In conclusion, we apply the developed measurement protocols to an unknown ferroelectric material.« less

Changes in lipid membranes may trigger amyloid toxicity in Alzheimer's disease

PubMed Central

Drolle, Elizabeth; Negoda, Alexander; Hammond, Keely; Pavlov, Evgeny

2017-01-01

Amyloid-beta peptides (Aβ), implicated in Alzheimer’s disease (AD), interact with the cellular membrane and induce amyloid toxicity. The composition of cellular membranes changes in aging and AD. We designed multi-component lipid models to mimic healthy and diseased states of the neuronal membrane. Using atomic force microscopy (AFM), Kelvin probe force microscopy (KPFM) and black lipid membrane (BLM) techniques, we demonstrated that these model membranes differ in their nanoscale structure and physical properties, and interact differently with Aβ1–42. Based on our data, we propose a new hypothesis that changes in lipid membrane due to aging and AD may trigger amyloid toxicity through electrostatic mechanisms, similar to the accepted mechanism of antimicrobial peptide action. Understanding the role of the membrane changes as a key activating amyloid toxicity may aid in the development of a new avenue for the prevention and treatment of AD. PMID:28767712

Trapping charges at grain boundaries and degradation of CH3NH3Pb(I1-x Br x )3 perovskite solar cells.

PubMed

Nguyen, Bich Phuong; Kim, Gee Yeong; Jo, William; Kim, Byeong Jo; Jung, Hyun Suk

2017-08-04

The electrical properties of CH 3 NH 3 Pb(I 1-x Br x ) 3 (x = 0.13) perovskite materials were investigated under ambient conditions. The local work function and the local current were measured using Kelvin probe force microscopy and conductive atomic force microscopy, respectively. The degradation of the perovskite layers depends on their grain size. As the material degrades, an additional peak in the surface potential appears simultaneously with a sudden increase and subsequent relaxation of the local current. The potential bending at the grain boundaries and the intragrains is the most likely reason for the change of the local current surface of the perovskite layers. The improved understanding of the degradation mechanism garnered from this study helps pave the way toward an improved photo-conversion efficiency in perovskite solar cells.

Trapping charges at grain boundaries and degradation of CH3NH3Pb(I1-x Br x )3 perovskite solar cells

NASA Astrophysics Data System (ADS)

Phuong Nguyen, Bich; Kim, Gee Yeong; Jo, William; Kim, Byeong Jo; Jung, Hyun Suk

2017-08-01

The electrical properties of CH3NH3Pb(I1-x Br x )3 (x = 0.13) perovskite materials were investigated under ambient conditions. The local work function and the local current were measured using Kelvin probe force microscopy and conductive atomic force microscopy, respectively. The degradation of the perovskite layers depends on their grain size. As the material degrades, an additional peak in the surface potential appears simultaneously with a sudden increase and subsequent relaxation of the local current. The potential bending at the grain boundaries and the intragrains is the most likely reason for the change of the local current surface of the perovskite layers. The improved understanding of the degradation mechanism garnered from this study helps pave the way toward an improved photo-conversion efficiency in perovskite solar cells.

Carbon nanotube modified probes for stable and high sensitivity conductive atomic force microscopy

NASA Astrophysics Data System (ADS)

Slattery, Ashley D.; Shearer, Cameron J.; Gibson, Christopher T.; Shapter, Joseph G.; Lewis, David A.; Stapleton, Andrew J.

2016-11-01

Conductive atomic force microscopy (C-AFM) is used to characterise the nanoscale electrical properties of many conducting and semiconducting materials. We investigate the effect of single walled carbon nanotube (SWCNT) modification of commercial Pt/Ir cantilevers on the sensitivity and image stability during C-AFM imaging. Pt/Ir cantilevers were modified with small bundles of SWCNTs via a manual attachment procedure and secured with a conductive platinum pad. AFM images of topography and current were collected from heterogeneous polymer and nanomaterial samples using both standard and SWCNT modified cantilevers. Typically, achieving a good current image comes at the cost of reduced feedback stability. In part, this is due to electrostatic interaction and increased tip wear upon applying a bias between the tip and the sample. The SWCNT modified tips displayed superior current sensitivity and feedback stability which, combined with superior wear resistance of SWCNTs, is a significant advancement for C-AFM.

Understanding Pt-ZnO:In Schottky nanocontacts by conductive atomic force microscopy

NASA Astrophysics Data System (ADS)

Chirakkara, Saraswathi; Choudhury, Palash Roy; Nanda, K. K.; Krupanidhi, S. B.

2016-04-01

Undoped and In doped ZnO (IZO) thin films are grown on Pt coated silicon substrates Pt/Si by pulsed laser deposition to fabricate Pt/ZnO:In Schottky diodes. The Schottky diodes were investigated by conventional two-probe current-voltage (I-V) measurements and by the I-V spectroscopy tool of conductive atomic force microscopy (C-AFM). The large deviation of the ideality factor from unity and the temperature dependent Schottky barrier heights (SBHs) obtained from the conventional method imply the presence of inhomogeneous interfaces. The inhomogeneity of SBHs is confirmed by C-AFM. Interestingly, the I-V curves at different points are found to be different, and the SBHs deduced from the point diodes reveal inhomogeneity at the nanoscale at the metal-semiconductor interface. A reduction in SBH and turn-on voltage along with enhancement in forward current are observed with increasing indium concentration.

Surface electrical properties of stainless steel fibres: An AFM-based study

NASA Astrophysics Data System (ADS)

Yin, Jun; D'Haese, Cécile; Nysten, Bernard

2015-03-01

Atomic force microscopy (AFM) electrical modes were used to study the surface electrical properties of stainless steel fibres. The surface electrical conductivity was studied by current sensing AFM and I-V spectroscopy. Kelvin probe force microscopy was used to measure the surface contact potential. The oxide film, known as passivation layer, covering the fibre surface gives rise to the observation of an apparently semiconducting behaviour. The passivation layer generally exhibits a p-type semiconducting behaviour, which is attributed to the predominant formation of chromium oxide on the surface of the stainless steel fibres. At the nanoscale, different behaviours are observed from points to points, which may be attributed to local variations of the chemical composition and/or thickness of the passivation layer. I-V curves are well fitted with an electron tunnelling model, indicating that electron tunnelling may be the predominant mechanism for electron transport.

Probing viscoelastic surfaces with bimodal tapping-mode atomic force microscopy: Underlying physics and observables for a standard linear solid model

PubMed Central

2014-01-01

Summary This paper presents computational simulations of single-mode and bimodal atomic force microscopy (AFM) with particular focus on the viscoelastic interactions occurring during tip–sample impact. The surface is modeled by using a standard linear solid model, which is the simplest system that can reproduce creep compliance and stress relaxation, which are fundamental behaviors exhibited by viscoelastic surfaces. The relaxation of the surface in combination with the complexities of bimodal tip–sample impacts gives rise to unique dynamic behaviors that have important consequences with regards to the acquisition of quantitative relationships between the sample properties and the AFM observables. The physics of the tip–sample interactions and its effect on the observables are illustrated and discussed, and a brief research outlook on viscoelasticity measurement with intermittent-contact AFM is provided. PMID:25383277

Friction imprint effect in mechanically cleaved BaTiO{sub 3} (001)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Long, Christian J.; Maryland Nanocenter, University of Maryland, College Park, Maryland 20742; Ebeling, Daniel

2014-09-28

Adsorption, chemisorption, and reconstruction at the surfaces of ferroelectric materials can all contribute toward the pinning of ferroelectric polarization, which is called the electrical imprint effect. Here, we show that the opposite is also true: freshly cleaved, atomically flat surfaces of (001) oriented BaTiO{sub 3} exhibit a persistent change in surface chemistry that is driven by ferroelectric polarization. This surface modification is explored using lateral force microscopy (LFM), while the ferroelectric polarization is probed using piezoresponse force microscopy. We find that immediately after cleaving BaTiO{sub 3}, LFM reveals friction contrast between ferroelectric domains. We also find that this surface modificationmore » remains after the ferroelectric domain distribution is modified, resulting in an imprint of the original ferroelectric domain distribution on the sample surface. This friction imprint effect has implications for surface patterning as well as ferroelectric device operation and failure.« less

Study the friction behaviour of poly[2-(dimethylamino)ethyl methacrylate] brush with AFM probes in contact mechanics

NASA Astrophysics Data System (ADS)

Raftari, Maryam; Zhang, Zhenyu; Leggett, Graham J.; Geoghegan, Mark

2011-10-01

We have studied the frictional behaviour of grafted poly[2-(dimethylamino)ethyl methacrylate] (PDMAEMA) films using friction force microscopy (FFM). The films were prepared on native oxide-terminated silicon substrates using the technique of atom transfer radical polymerization (ATRP). We show that single asperity contact mechanics (Johnson-Kendall-Roberts(JKR) and Derjaguin-Muller-Toporov(DMT)) as well as a linear (Amontons) relation between applied load and frictional load depending on the pH of the FFM probe. Measurements were made using functionalized and unfunctionalized silicon nitride triangular probes. Functionalized probes included gold-coated probes, and ones coated with a self-assembled monolayer of dodecanethiol (DDT). The frictional behaviour between PDMAEMA and all tips immersed in pH from 3 to 11 are corresponded to the DMT or JKR model and are linear in pH=1, 2, and 12. These results show that contact mechanics of polyelectrolytes in water is complex and strongly dependent on the environmental pH.

Interactions between silica particles in the presence of multivalent coions.

PubMed

Uzelac, Biljana; Valmacco, Valentina; Trefalt, Gregor

2017-08-30

Forces between charged silica particles in solutions of multivalent coions are measured with colloidal probe technique based on atomic force microscopy. The concentration of 1 : z electrolytes is systematically varied to understand the behavior of electrostatic interactions and double-layer properties in these systems. Although the coions are multivalent the Derjaguin, Landau, Verwey, and Overbeek (DLVO) theory perfectly describes the measured force profiles. The diffuse-layer potentials and regulation properties are extracted from the forces profiles by using the DLVO theory. The dependencies of the diffuse-layer potential and regulation parameter shift to lower concentration with increasing coion valence when plotted as a function of concentration of 1 : z salt. Interestingly, these profiles collapse to a master curve if plotted as a function of monovalent counterion concentration.

Multifarious applications of atomic force microscopy in forensic science investigations.

PubMed

Pandey, Gaurav; Tharmavaram, Maithri; Rawtani, Deepak; Kumar, Sumit; Agrawal, Y

2017-04-01

Forensic science is a wide field comprising of several subspecialties and uses methods derived from natural sciences for finding criminals and other evidence valid in a legal court. A relatively new area; Nano-forensics brings a new era of investigation in forensic science in which instantaneous results can be produced that determine various agents such as explosive gasses, biological agents and residues in different crime scenes and terrorist activity investigations. This can be achieved by applying Nanotechnology and its associated characterization techniques in forensic sciences. Several characterization techniques exist in Nanotechnology and nano-analysis is one such technique that is used in forensic science which includes Electron microscopes (EM) like Transmission (TEM) and Scanning (SEM), Raman microscopy (Micro -Raman) and Scanning Probe Microscopes (SPMs) like Atomic Force Microscope (AFM). Atomic force microscopy enables surface characterization of different materials by examining their morphology and mechanical properties. Materials that are immeasurable such as hair, body fluids, textile fibers, documents, polymers, pressure sensitive adhesives (PSAs), etc. are often encountered during forensic investigations. This review article will mainly focus on the use of AFM in the examination of different evidence such as blood stains, forged documents, human hair samples, ammunitions, explosives, and other such applications in the field of Forensic Science. Copyright © 2017 Elsevier B.V. All rights reserved.

Micromachined Chip Scale Thermal Sensor for Thermal Imaging.

PubMed

Shekhawat, Gajendra S; Ramachandran, Srinivasan; Jiryaei Sharahi, Hossein; Sarkar, Souravi; Hujsak, Karl; Li, Yuan; Hagglund, Karl; Kim, Seonghwan; Aden, Gary; Chand, Ami; Dravid, Vinayak P

2018-02-27

The lateral resolution of scanning thermal microscopy (SThM) has hitherto never approached that of mainstream atomic force microscopy, mainly due to poor performance of the thermal sensor. Herein, we report a nanomechanical system-based thermal sensor (thermocouple) that enables high lateral resolution that is often required in nanoscale thermal characterization in a wide range of applications. This thermocouple-based probe technology delivers excellent lateral resolution (∼20 nm), extended high-temperature measurements >700 °C without cantilever bending, and thermal sensitivity (∼0.04 °C). The origin of significantly improved figures-of-merit lies in the probe design that consists of a hollow silicon tip integrated with a vertically oriented thermocouple sensor at the apex (low thermal mass) which interacts with the sample through a metallic nanowire (50 nm diameter), thereby achieving high lateral resolution. The efficacy of this approach to SThM is demonstrated by imaging embedded metallic nanostructures in silica core-shell, metal nanostructures coated with polymer films, and metal-polymer interconnect structures. The nanoscale pitch and extremely small thermal mass of the probe promise significant improvements over existing methods and wide range of applications in several fields including semiconductor industry, biomedical imaging, and data storage.

Determination of the electrical resistivity of vertically aligned carbon nanotubes by scanning probe microscopy

NASA Astrophysics Data System (ADS)

Ageev, O. A.; Il'in, O. I.; Rubashkina, M. V.; Smirnov, V. A.; Fedotov, A. A.; Tsukanova, O. G.

2015-07-01

Techniques are developed to determine the resistance per unit length and the electrical resistivity of vertically aligned carbon nanotubes (VA CNTs) using atomic force microscopy (AFM) and scanning tunneling microscopy (STM). These techniques are used to study the resistance of VA CNTs. The resistance of an individual VA CNT calculated with the AFM-based technique is shown to be higher than the resistance of VA CNTs determined by the STM-based technique by a factor of 200, which is related to the influence of the resistance of the contact of an AFM probe to VA CNTs. The resistance per unit length and the electrical resistivity of an individual VA CNT 118 ± 39 nm in diameter and 2.23 ± 0.37 μm in height that are determined by the STM-based technique are 19.28 ± 3.08 kΩ/μm and 8.32 ± 3.18 × 10-4 Ω m, respectively. The STM-based technique developed to determine the resistance per unit length and the electrical resistivity of VA CNTs can be used to diagnose the electrical parameters of VA CNTs and to create VA CNT-based nanoelectronic elements.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Balke, Nina; Bassiri-Gharb, Nazanin; Lichtensteiger, Céline

Almost two decades beyond the inception of piezoresponse force microscopy (PFM) and the seminal papers by G€uthner and Dransfeld1 and Gruverman et al., the technique has become the prevailing approach for nanoscale functional characterization of polar materials and has been extended to the probing of other electromechanical effects through the advent of electrochemical strain microscopy (ESM). This focus issue celebrates some of the recent advances in the field and offers a wider outlook of polar materials and their overall characterization. In this paper, we cover topics that include discussions of the properties of traditional ferroelectrics, such as lead zirconate titanatemore » (PZT) and lithium niobate, relaxorferroelectrics, as well as more “exotic” ferroelectric oxides such as hafnia, ferroelectric biological matter, and multiferroic materials. Technique-oriented contributions include papers on the coupling of PFM with other characterization methods such as x-ray diffraction (XRD) and superconducting quantum interface device (SQUID), in addition to considerations on the open questions on the electromechanical response in biased scanning probe microscopy (SPM) techniques, including the effects of the laser spot placement on the readout cantilever displacement, the influence of the tip on the creation of the domain shapes, and the impact of ionic and electronic dynamics on the observed nanoscale hysteretic phenomena.« less

Biomechanics and dynamics of red blood cells probed by optical tweezers and digital holographic microscopy

NASA Astrophysics Data System (ADS)

Cardenas, Nelson; Thomas, Pattrick; Yu, Lingfeng; Mohanty, Samarendra

2011-03-01

Red blood cells (RBC), with their unique viscoelastic properties, can undergo large deformations during interaction with fluid flow and migration through narrow capillaries. Both local and overall viscoelastic property is important for cellular function and change in these properties indicate diseased condition. Though biomechanics of the cells have been studied using variety of physical techniques (AFM, optically-trapped anchoring beads and microcapilary aspiration) in force regime 10pN, little is studied at low force regime <1pN. Such perturbations are not only hard to exercise on the cell membrane, but quantification of such deformations becomes extremely difficult. By application of low power optical tweezers directly on cell membrane, we could locally perturb discotic RBC along the axial direction, which was monitored dynamically by digital holographic microscopy-a real time, wide-field imaging method having nm axial resolution. The viscoelastic property of the RBC at low force regime was found to be significantly different from that of high-force regime. The results were found to be in good agreement with the simulation results obtained using finite element model of the axially-stretched RBC. The simulations and results of viscoelestic measurements will be presented.

Atomic Force Microscopy for Soil Analysis

NASA Astrophysics Data System (ADS)

gazze, andrea; doerr, stefan; dudley, ed; hallin, ingrid; matthews, peter; quinn, gerry; van keulen, geertje; francis, lewis

2016-04-01

Atomic Force Microscopy (AFM) is a high-resolution surface-sensitive technique, which provides 3-dimensional topographical information and material properties of both stiff and soft samples in their natural environments. Traditionally AFM has been applied to samples with low roughness: hence its use for soil analysis has been very limited so far. Here we report the optimization settings required for a standardization of high-resolution and artefact-free analysis of natural soil with AFM: soil immobilization, AFM probe selection, artefact recognition and minimization. Beyond topography, AFM can be used in a spectroscopic mode to evaluate nanomechanical properties, such as soil viscosity, stiffness, and deformation. In this regards, Bruker PeakForce-Quantitative NanoMechanical (QNM) AFM provides a fast and convenient way to extract physical properties from AFM force curves in real-time to obtain soil nanomechanical properties. Here we show for the first time the ability of AFM to describe the topography of natural soil at nanometre resolution, with observation of micro-components, such as clays, and of nano-structures, possibly of biotic origin, the visualization of which would prove difficult with other instrumentations. Finally, nanomechanical profiling has been applied to different wettability states in soil and the respective physical patterns are discussed.

Investigating cell mechanics with atomic force microscopy

PubMed Central

Haase, Kristina; Pelling, Andrew E.

2015-01-01

Transmission of mechanical force is crucial for normal cell development and functioning. However, the process of mechanotransduction cannot be studied in isolation from cell mechanics. Thus, in order to understand how cells ‘feel’, we must first understand how they deform and recover from physical perturbations. Owing to its versatility, atomic force microscopy (AFM) has become a popular tool to study intrinsic cellular mechanical properties. Used to directly manipulate and examine whole and subcellular reactions, AFM allows for top-down and reconstitutive approaches to mechanical characterization. These studies show that the responses of cells and their components are complex, and largely depend on the magnitude and time scale of loading. In this review, we generally describe the mechanotransductive process through discussion of well-known mechanosensors. We then focus on discussion of recent examples where AFM is used to specifically probe the elastic and inelastic responses of single cells undergoing deformation. We present a brief overview of classical and current models often used to characterize observed cellular phenomena in response to force. Both simple mechanistic models and complex nonlinear models have been used to describe the observed cellular behaviours, however a unifying description of cell mechanics has not yet been resolved. PMID:25589563

Single molecule atomic force microscopy and force spectroscopy of chitosan.

PubMed

Kocun, Marta; Grandbois, Michel; Cuccia, Louis A

2011-02-01

Atomic force microscopy (AFM) and AFM-based force spectroscopy was used to study the desorption of individual chitosan polymer chains from substrates with varying chemical composition. AFM images of chitosan adsorbed onto a flat mica substrate show elongated single strands or aggregated bundles. The aggregated state of the polymer is consistent with the high level of flexibility and mobility expected for a highly positively charged polymer strand. Conversely, the visualization of elongated strands indicated the presence of stabilizing interactions with the substrate. Surfaces with varying chemical composition (glass, self-assembled monolayer of mercaptoundecanoic acid/decanethiol and polytetrafluoroethylene (PTFE)) were probed with chitosan modified AFM tips and the corresponding desorption energies, calculated from plateau-like features, were attributed to the desorption of individual polymer strands. Desorption energies of 2.0±0.3×10(-20)J, 1.8±0.3×10(-20)J and 3.5±0.3×10(-20)J were obtained for glass, SAM of mercaptoundecanoic/dodecanethiol and PTFE, respectively. These single molecule level results can be used as a basis for investigating chitosan and chitosan-based materials for biomaterial applications. Copyright © 2010 Elsevier B.V. All rights reserved.

Identifying the charge generation dynamics in Cs+-based triple cation mixed perovskite solar cells.

PubMed

Salado, Manuel; Kokal, Ramesh K; Calio, Laura; Kazim, Samrana; Deepa, Melepurath; Ahmad, Shahzada

2017-08-30

Triple cation based perovskite solar cells offer enhanced moisture tolerance and stability compared to mixed perovskites. Slight substitution of methyl ammonium or formamidinium cation by cesium (Cs + ), was also reported to eliminate halide segregation due to its smaller size. To elucidate the device kinetics and understand the role of the Cs, we undertook different modes of scanning probe microscopy and electrochemical impedance spectroscopy (EIS) experiments. Kelvin probe force microscopy revealed that the incorporation of the Cs cation increases the contact potential difference (CPD), this CPD further increases when Spiro-OMeTAD is used as a hole transport material. The current at the nanoscale level shows improvement with Cs inclusion and further enhancement by the Spiro-OMeTAD deposition, studied under light illumination, which supports the high photocurrent density obtained from the cells. EIS demonstrates that in a triple cation environment, reduced carrier recombination at the TiO 2 /perovskite interface was also obtained which in turn allow us to achieve a higher V oc value.

Probing the probe: AFM tip-profiling via nanotemplates to determine Hamaker constants from phase-distance curves.

PubMed

Rodriguez, Raul D; Lacaze, Emmanuelle; Jupille, Jacques

2012-10-01

A method to determine the van der Waals forces from phase-distance curves recorded by atomic force microscopy (AFM) in tapping mode is presented. The relationship between the phase shift and the tip-sample distance is expressed as a function of the product of the Hamaker constant by tip radius. Silica-covered silicon tips are used to probe silica-covered silicon substrate in dry conditions to avoid capillary effects. Tips being assumed spherical, radii are determined in situ by averaging profiles recorded in different directions on hematite nanocrystals acting as nanotemplates, thus accounting for tip anisotropy. Through a series of reproducible measurements performed with tips of various radii (including the in-situ characterization of a damaged tip), a value of (6.3±0.4)×10(-20) J is found for the Hamaker constant of interacting silica surfaces in air, in good agreement with tabulated data. The results demonstrate that the onset of the tip-surface interaction is dominated by the van der Waals forces and that the total force can be modeled in the framework of the harmonic approximation. Based on the tip radius and the Hamaker constant associated to the tip-substrate system, the model is quite flexible. Once the Hamaker constant is known, a direct estimate of the tip size can be achieved whereas when the tip size is known, a quantitative evaluation of the van der Waals force becomes possible on different substrates with a spatial resolution at the nanoscale. Copyright © 2012 Elsevier B.V. All rights reserved.

Origins of phase contrast in the atomic force microscope in liquids

PubMed Central

Melcher, John; Carrasco, Carolina; Xu, Xin; Carrascosa, José L.; Gómez-Herrero, Julio; José de Pablo, Pedro; Raman, Arvind

2009-01-01

We study the physical origins of phase contrast in dynamic atomic force microscopy (dAFM) in liquids where low-stiffness microcantilever probes are often used for nanoscale imaging of soft biological samples with gentle forces. Under these conditions, we show that the phase contrast derives primarily from a unique energy flow channel that opens up in liquids due to the momentary excitation of higher eigenmodes. Contrary to the common assumption, phase-contrast images in liquids using soft microcantilevers are often maps of short-range conservative interactions, such as local elastic response, rather than tip-sample dissipation. The theory is used to demonstrate variations in local elasticity of purple membrane and bacteriophage ϕ29 virions in buffer solutions using the phase-contrast images. PMID:19666560

Origins of phase contrast in the atomic force microscope in liquids.

PubMed

Melcher, John; Carrasco, Carolina; Xu, Xin; Carrascosa, José L; Gómez-Herrero, Julio; José de Pablo, Pedro; Raman, Arvind

2009-08-18

We study the physical origins of phase contrast in dynamic atomic force microscopy (dAFM) in liquids where low-stiffness microcantilever probes are often used for nanoscale imaging of soft biological samples with gentle forces. Under these conditions, we show that the phase contrast derives primarily from a unique energy flow channel that opens up in liquids due to the momentary excitation of higher eigenmodes. Contrary to the common assumption, phase-contrast images in liquids using soft microcantilevers are often maps of short-range conservative interactions, such as local elastic response, rather than tip-sample dissipation. The theory is used to demonstrate variations in local elasticity of purple membrane and bacteriophage 29 virions in buffer solutions using the phase-contrast images.

DNA combing on low-pressure oxygen plasma modified polysilsesquioxane substrates for single-molecule studies

PubMed Central

Sriram, K. K.; Chang, Chun-Ling; Rajesh Kumar, U.; Chou, Chia-Fu

2014-01-01

Molecular combing and flow-induced stretching are the most commonly used methods to immobilize and stretch DNA molecules. While both approaches require functionalization steps for the substrate surface and the molecules, conventionally the former does not take advantage of, as the latter, the versatility of microfluidics regarding robustness, buffer exchange capability, and molecule manipulation using external forces for single molecule studies. Here, we demonstrate a simple one-step combing process involving only low-pressure oxygen (O2) plasma modified polysilsesquioxane (PSQ) polymer layer to facilitate both room temperature microfluidic device bonding and immobilization of stretched single DNA molecules without molecular functionalization step. Atomic force microscopy and Kelvin probe force microscopy experiments revealed a significant increase in surface roughness and surface potential on low-pressure O2 plasma treated PSQ, in contrast to that with high-pressure O2 plasma treatment, which are proposed to be responsible for enabling effective DNA immobilization. We further demonstrate the use of our platform to observe DNA-RNA polymerase complexes and cancer drug cisplatin induced DNA condensation using wide-field fluorescence imaging. PMID:25332730

A method for the direct measurement of surface tension of collected atmospherically relevant aerosol particles using atomic force microscopy

NASA Astrophysics Data System (ADS)

Hritz, Andrew D.; Raymond, Timothy M.; Dutcher, Dabrina D.

2016-08-01

Accurate estimates of particle surface tension are required for models concerning atmospheric aerosol nucleation and activation. However, it is difficult to collect the volumes of atmospheric aerosol required by typical instruments that measure surface tension, such as goniometers or Wilhelmy plates. In this work, a method that measures, ex situ, the surface tension of collected liquid nanoparticles using atomic force microscopy is presented. A film of particles is collected via impaction and is probed using nanoneedle tips with the atomic force microscope. This micro-Wilhelmy method allows for direct measurements of the surface tension of small amounts of sample. This method was verified using liquids, whose surface tensions were known. Particles of ozone oxidized α-pinene, a well-characterized system, were then produced, collected, and analyzed using this method to demonstrate its applicability for liquid aerosol samples. It was determined that oxidized α-pinene particles formed in dry conditions have a surface tension similar to that of pure α-pinene, and oxidized α-pinene particles formed in more humid conditions have a surface tension that is significantly higher.

Bacterial adhesion force quantification by fluidic force microscopy

NASA Astrophysics Data System (ADS)

Potthoff, Eva; Ossola, Dario; Zambelli, Tomaso; Vorholt, Julia A.

2015-02-01

Quantification of detachment forces between bacteria and substrates facilitates the understanding of the bacterial adhesion process that affects cell physiology and survival. Here, we present a method that allows for serial, single bacterial cell force spectroscopy by combining the force control of atomic force microscopy with microfluidics. Reversible bacterial cell immobilization under physiological conditions on the pyramidal tip of a microchanneled cantilever is achieved by underpressure. Using the fluidic force microscopy technology (FluidFM), we achieve immobilization forces greater than those of state-of-the-art cell-cantilever binding as demonstrated by the detachment of Escherichia coli from polydopamine with recorded forces between 4 and 8 nN for many cells. The contact time and setpoint dependence of the adhesion forces of E. coli and Streptococcus pyogenes, as well as the sequential detachment of bacteria out of a chain, are shown, revealing distinct force patterns in the detachment curves. This study demonstrates the potential of the FluidFM technology for quantitative bacterial adhesion measurements of cell-substrate and cell-cell interactions that are relevant in biofilms and infection biology.Quantification of detachment forces between bacteria and substrates facilitates the understanding of the bacterial adhesion process that affects cell physiology and survival. Here, we present a method that allows for serial, single bacterial cell force spectroscopy by combining the force control of atomic force microscopy with microfluidics. Reversible bacterial cell immobilization under physiological conditions on the pyramidal tip of a microchanneled cantilever is achieved by underpressure. Using the fluidic force microscopy technology (FluidFM), we achieve immobilization forces greater than those of state-of-the-art cell-cantilever binding as demonstrated by the detachment of Escherichia coli from polydopamine with recorded forces between 4 and 8 nN for many cells. The contact time and setpoint dependence of the adhesion forces of E. coli and Streptococcus pyogenes, as well as the sequential detachment of bacteria out of a chain, are shown, revealing distinct force patterns in the detachment curves. This study demonstrates the potential of the FluidFM technology for quantitative bacterial adhesion measurements of cell-substrate and cell-cell interactions that are relevant in biofilms and infection biology. Electronic supplementary information (ESI) available: Video S1. Detachment of a S. pyogenes cell chain from glass substrate. The cantilever is approached on the outermost adherent cell of a chain and four bacteria were then sequentially detached. The sequential cell detachment suddenly stopped after four bacteria. This possibly occurred because bacteria-glass interactions became too strong or the maximal probe retraction was reached. The cells spontaneously detached from the cantilever flipping back on the surface. Fig. S1. (A) Adhesion force-distance and (B) adhesion force-detaching work correlation of E.coli on PLL for setpoints of 1 and 10 nN. Circle: 1 nN setpoint, square: 10 nN. See DOI: 10.1039/c4nr06495j

Measuring bacterial cells size with AFM

PubMed Central

Osiro, Denise; Filho, Rubens Bernardes; Assis, Odilio Benedito Garrido; Jorge, Lúcio André de Castro; Colnago, Luiz Alberto

2012-01-01

Atomic Force Microscopy (AFM) can be used to obtain high-resolution topographical images of bacteria revealing surface details and cell integrity. During scanning however, the interactions between the AFM probe and the membrane results in distortion of the images. Such distortions or artifacts are the result of geometrical effects related to bacterial cell height, specimen curvature and the AFM probe geometry. The most common artifact in imaging is surface broadening, what can lead to errors in bacterial sizing. Several methods of correction have been proposed to compensate for these artifacts and in this study we describe a simple geometric model for the interaction between the tip (a pyramidal shaped AFM probe) and the bacterium (Escherichia coli JM-109 strain) to minimize the enlarging effect. Approaches to bacteria immobilization and examples of AFM images analysis are also described. PMID:24031837

Atomic force microscopy of RNA: State of the art and recent advancements.

PubMed

Schön, Peter

2018-01-01

The atomic force microscope (AFM) has become a powerful tool for the visualization, probing and manipulation of RNA at the single molecule level. AFM measurements can be carried out in buffer solution in a physiological medium, which is crucial to study the structure and function of biomolecules, also allowing studying them at work. Imaging the specimen in its native state is a great advantage compared to other high resolution methods such as electron microscopy and X-ray diffraction. There is no need to stain, freeze or crystallize biological samples. Moreover, compared to NMR spectroscopy for instance, for AFM studies the size of the biomolecules is not limiting. Consequently the AFM allows one also to investigate larger RNA molecules. In particular, structural studies of nucleic acids and assemblies thereof, have been carried out by AFM routinely including ssRNA, dsRNA and nucleoprotein complexes thereof, as well as RNA aggregates and 2D RNA assemblies. These are becoming increasingly important as novel unique building blocks in the emerging field of RNA nanotechnology. In particular by AFM unique information can be obtained on these RNA based assemblies. Moreover, the AFM is of fundamental relevance to study biological relevant RNA interactions and dynamics. In this short review a brief overview will be given on structural studies that have been done related to AFM topographic imaging of RNA, RNA assemblies and aggregates. Finally, an overview on AFM beyond imaging will be provided. This includes force spectroscopy of RNA under physiological conditions in aqueous buffer to probe RNA interaction with proteins and ligands as well as other AFM tip based RNA probing. Important applications include the detection and quantification of RNA in biological samples. A selection of recent highlights and breakthroughs will be provided related to structural and functional studies by AFM. The main intention of this short review to provide the reader with a flavor of what AFM is able to contribute to RNA research and engineering. Copyright © 2017 Elsevier Ltd. All rights reserved.

[Ultrastructural changes of human dental hard tissues during orthodontic treatment with fixed appliances].

PubMed

Antonova, I N; Goncharov, V D; Bobrova, E A

The aim of the study was to evaluate ultrastructural changes of dental enamel after fixation of orthodontic appliances, initial influence of orthodontic forces and removal of braces. Five intact permanent tooth extracted for orthodontic reasons were included in the experimental study. Scanning probe microscopy was conducted in 4 random enamel points in each tooth (20 points overall) in semi-contact mode with standard 10 nm probes. The study showed ultrastructural enamel changes such as nanofractures up to 1 mm along the braces locks. The changes correlated with surface morphological features and teeth anatomy and may play an important role in dental decay and non-carious lesions occurring in the course of orthodontic treatment.

Invited Review Article: Tip modification methods for tip-enhanced Raman spectroscopy (TERS) and colloidal probe technique: A 10 year update (2006-2016) review

NASA Astrophysics Data System (ADS)

Yuan, C. C.; Zhang, D.; Gan, Y.

2017-03-01

Engineering atomic force microscopy tips for reliable tip enhanced Raman spectroscopy (TERS) and colloidal probe technique are becoming routine practices in many labs. In this 10 year update review, various new tip modification methods developed over the past decade are briefly reviewed to help researchers select the appropriate method. The perspective is put in a large context to discuss the opportunities and challenges in this area, including novel combinations of seemingly different methods, potential applications of some methods which were not originally intended for TERS tip fabrication, and the problems of high cost and poor reproducibility of tip fabrication.

Nanospectrofluorometry inside single living cell by scanning near-field optical microscopy

NASA Astrophysics Data System (ADS)

Lei, F. H.; Shang, G. Y.; Troyon, M.; Spajer, M.; Morjani, H.; Angiboust, J. F.; Manfait, M.

2001-10-01

Near-field fluorescence spectra with subdiffraction limit spatial resolution have been taken in the proximity of mitochondrial membrane inside breast adenocarcinoma cells (MCF7) treated with the fluorescent dye (JC-1) by using a scanning near-field optical microscope coupled with a confocal laser microspectrofluorometer. The probe-sample distance control is based on a piezoelectric bimorph shear force sensor having a static spring constant k=5 μN/nm and a quality factor Q=40 in a physiological medium of viscosity η=1.0 cp. The sensitivity of the force sensor has been tested by imaging a MCF7 cell surface.

Fungus-mediated biological synthesis of gold nanoparticles: potential in detection of liver cancer

PubMed Central

Chauhan, Arun; Zubair, Swaleha; Tufail, Saba; Sherwani, Asif; Sajid, Mohammad; Raman, Suri C; Azam, Amir; Owais, Mohammad

2011-01-01

Background Nanomaterials are considered to be the pre-eminent component of the rapidly advancing field of nanotechnology. However, developments in the biologically inspired synthesis of nanoparticles are still in their infancy and consequently attracting the attention of material scientists throughout the world. Keeping in mind the fact that microorganism-assisted synthesis of nanoparticles is a safe and economically viable prospect, in the current study we report Candida albicans-mediated biological synthesis of gold nanoparticles. Methods and results Transmission electron microscopy, atomic force microscopy, and various spectrophotometric analyses were performed to characterize the gold nanoparticles. The morphology of the synthesized gold particles depended on the abundance of C. albicans cytosolic extract. Transmission electron microscopy, nanophox particle analysis, and atomic force microscopy revealed the size of spherical gold nanoparticles to be in the range of 20–40 nm and nonspherical gold particles were found to be 60–80 nm. We also evaluated the potential of biogenic gold nanoparticles to probe liver cancer cells by conjugating them with liver cancer cell surface-specific antibodies. The antibody-conjugated gold particles were found to bind specifically to the surface antigens of the cancer cells. Conclusion The antibody-conjugated gold particles synthesized in this study could successfully differentiate normal cell populations from cancerous cells. PMID:22072868

Electrical transport and structural characterization of epitaxial monolayer MoS2 /n- and p-doped GaN vertical lattice-matched heterojunctions

NASA Astrophysics Data System (ADS)

Ruzmetov, D.; O'Regan, T.; Zhang, K.; Herzing, A.; Mazzoni, A.; Chin, M.; Huang, S.; Zhang, Z.; Burke, R.; Neupane, M.; Birdwell, Ag; Shah, P.; Crowne, F.; Kolmakov, A.; Leroy, B.; Robinson, J.; Davydov, A.; Ivanov, T.

We investigate vertical semiconductor junctions consisting of monolayer MoS2 that is epitaxially grown on n- and p-doped GaN crystals. Such a junction represents a building block for 2D/3D vertical semiconductor heterostructures. Epitaxial, lattice-matched growth of MoS2 on GaN is important to ensure high quality interfaces that are crucial for the efficient vertical transport. The MoS2/GaN junctions were characterized with cross-sectional and planar scanning transmission electron microscopy (STEM), scanning tunneling microscopy, and atomic force microscopy. The MoS2/GaN lattice mismatch is measured to be near 1% using STEM. The electrical transport in the out-of-plane direction across the MoS2/GaN junctions was measured using conductive atomic force microscopy and mechanical nano-probes inside a scanning electron microscope. Nano-disc metal contacts to MoS2 were fabricated by e-beam lithography and evaporation. The current-voltage curves of the vertical MoS2/GaN junctions exhibit rectification with opposite polarities for n-doped and p-doped GaN. The metal contact determines the general features of the current-voltage curves, and the MoS2 monolayer modifies the electrical transport across the contact/GaN interface.

Scanning Probe Microscopy on heterogeneous CaCu3Ti4O12 thin films

PubMed Central

2011-01-01

The conductive atomic force microscopy provided a local characterization of the dielectric heterogeneities in CaCu3Ti4O12 (CCTO) thin films deposited by MOCVD on IrO2 bottom electrode. In particular, both techniques have been employed to clarify the role of the inter- and sub-granular features in terms of conductive and insulating regions. The microstructure and the dielectric properties of CCTO thin films have been studied and the evidence of internal barriers in CCTO thin films has been provided. The role of internal barriers and the possible explanation for the extrinsic origin of the giant dielectric response in CCTO has been evaluated. PMID:21711646

Scanning Probe Microscopy on heterogeneous CaCu3Ti4O12 thin films

NASA Astrophysics Data System (ADS)

Fiorenza, Patrick; Lo Nigro, Raffaella; Raineri, Vito

2011-12-01

The conductive atomic force microscopy provided a local characterization of the dielectric heterogeneities in CaCu3Ti4O12 (CCTO) thin films deposited by MOCVD on IrO2 bottom electrode. In particular, both techniques have been employed to clarify the role of the inter- and sub-granular features in terms of conductive and insulating regions. The microstructure and the dielectric properties of CCTO thin films have been studied and the evidence of internal barriers in CCTO thin films has been provided. The role of internal barriers and the possible explanation for the extrinsic origin of the giant dielectric response in CCTO has been evaluated.

Scanning Probe Microscopy on heterogeneous CaCu3Ti4O12 thin films.

PubMed

Fiorenza, Patrick; Lo Nigro, Raffaella; Raineri, Vito

2011-02-04

The conductive atomic force microscopy provided a local characterization of the dielectric heterogeneities in CaCu3Ti4O12 (CCTO) thin films deposited by MOCVD on IrO2 bottom electrode. In particular, both techniques have been employed to clarify the role of the inter- and sub-granular features in terms of conductive and insulating regions. The microstructure and the dielectric properties of CCTO thin films have been studied and the evidence of internal barriers in CCTO thin films has been provided. The role of internal barriers and the possible explanation for the extrinsic origin of the giant dielectric response in CCTO has been evaluated.

Electrical conduction at domain walls in multiferroic BiFeO3

NASA Astrophysics Data System (ADS)

Seidel, Jan; Martin, Lane; He, Qing; Zhan, Qian; Chu, Ying-Hao; Rother, Axel; Hawkridge, Michael; Maksymovych, Peter; Yu, Pu; Gajek, Martin; Balke, Nina; Kalinin, Sergei; Gemming, Sybille; Wang, Feng; Catalán, Gustau; Scott, James; Spaldin, Nicola; Orenstein, Joseph; Ramesh, Ramamoorthy

2009-03-01

We report the observation of room temperature electronic conductivity at ferroelectric domain walls in BiFeO3. The origin and nature of the observed conductivity is probed using a combination of conductive atomic force microscopy, high resolution transmission electron microscopy and first-principles density functional computations. We show that a structurally driven change in both the electrostatic potential and local electronic structure (i.e., a decrease in band gap) at the domain wall leads to the observed electrical conductivity. We estimate the conductivity in the wall to be several orders of magnitude higher than for the bulk material. Additionally we demonstrate the potential for device applications of such conducting nanoscale features.

Thrombin-induced contraction in alveolar epithelial cells probed by traction microscopy.

PubMed

Gavara, Núria; Sunyer, Raimon; Roca-Cusachs, Pere; Farré, Ramon; Rotger, Mar; Navajas, Daniel

2006-08-01

Contractile tension of alveolar epithelial cells plays a major role in the force balance that regulates the structural integrity of the alveolar barrier. The aim of this work was to study thrombin-induced contractile forces of alveolar epithelial cells. A549 alveolar epithelial cells were challenged with thrombin, and time course of contractile forces was measured by traction microscopy. The cells exhibited basal contraction with total force magnitude 55.0 +/- 12.0 nN (mean +/- SE, n = 12). Traction forces were exerted predominantly at the cell periphery and pointed to the cell center. Thrombin (1 U/ml) induced a fast and sustained 2.5-fold increase in traction forces, which maintained peripheral and centripetal distribution. Actin fluorescent staining revealed F-actin polymerization and enhancement of peripheral actin rim. Disruption of actin cytoskeleton with cytochalasin D (5 microM, 30 min) and inhibition of myosin light chain kinase with ML-7 (10 microM, 30 min) and Rho kinase with Y-27632 (10 microM, 30 min) markedly depressed basal contractile tone and abolished thrombin-induced cell contraction. Therefore, the contractile response of alveolar epithelial cells to the inflammatory agonist thrombin was mediated by actin cytoskeleton remodeling and actomyosin activation through myosin light chain kinase and Rho kinase signaling pathways. Thrombin-induced contractile tension might further impair alveolar epithelial barrier integrity in the injured lung.

Molecular Velcro constructed from polymer loop brushes showing enhanced adhesion force

NASA Astrophysics Data System (ADS)

Zhou, Tian; Han, Biao; Han, Lin; Li, Christopher; Department of Materials Science; Engineering Team; School of Biomedical Engineering, Science; Health Systems Team

2015-03-01

Molecular Velcro is commonly seen in biological systems as the formation of strong physical entanglement at molecular scale could induce strong adhesion, which is crucial to many biological processes. To mimic this structure, we designed, and fabricated polymer loop brushes using polymer single crystals with desired surface functionality and controlled chain folding. Compared with reported loop brushes fabricated using triblock copolymers, the present loop bushes have precise loop sizes, loop grafting density, and well controlled tethering locations on the solid surface. Atomic force microscopy-based force spectroscopy measurements using a polymer chain coated probe reveal that the adhesion force are significantly enhanced on the loop brush surface as compared with its single-strand counterpart. This study directly shows the effect of polymer brush conformation on their properties, and suggests a promising strategy for advanced polymer surface design.

Atomic force microscopy capable of vibration isolation with low-stiffness Z-axis actuation.

PubMed

Ito, Shingo; Schitter, Georg

2018-03-01

For high-resolution imaging without bulky external vibration isolation, this paper presents an atomic force microscope (AFM) capable of vibration isolation with its internal Z-axis (vertical) actuators moving the AFM probe. Lorentz actuators (voice coil actuators) are used for the Z-axis actuation, and flexures guiding the motion are designed to have a low stiffness between the mover and the base. The low stiffness enables a large Z-axis actuation of more than 700 µm and mechanically isolates the probe from floor vibrations at high frequencies. To reject the residual vibrations, the probe tracks the sample by using a displacement sensor for feedback control. Unlike conventional AFMs, the Z-axis actuation attains a closed-loop control bandwidth that is 35 times higher than the first mechanical resonant frequency. The closed-loop AFM system has robustness against the flexures' nonlinearity and uses the first resonance for better sample tracking. For further improvement, feedforward control with a vibration sensor is combined, and the resulting system rejects 98.4% of vibrations by turning on the controllers. The AFM system is demonstrated by successful AFM imaging in a vibrational environment. Copyright © 2017 Elsevier B.V. All rights reserved.

Advances in engineering nanometrology at the National Physical Laboratory

NASA Astrophysics Data System (ADS)

Leach, Richard K.; Claverley, James; Giusca, Claudiu; Jones, Christopher W.; Nimishakavi, Lakshmi; Sun, Wenjuan; Tedaldi, Matthew; Yacoot, Andrew

2012-07-01

The National Physical Laboratory, UK, has been active in the field of engineering nanometrology for a number of years. A summary of progress over the last five years is presented in this paper and the following research projects discussed in detail. (1) Development of an infrastructure for the calibration of instruments for measuring areal surface topography, along with the development of areal software measurement standards. This work comprises the use of the optical transfer function and a technique for the simultaneous measurement of topography and the phase change on reflection, allowing composite materials to be measured. (2) Development of a vibrating micro-CMM probe with isotropic probing reaction and the ability to operate in a non-contact mode. (3) A review of x-ray computed tomography and its use in dimensional metrology. (4) The further development of a metrology infrastructure for atomic force microscopy and the development of an instrument for the measurement of the effect of the probe-surface interaction. (5) Traceable measurement of displacement using optical and x-ray interferometry to picometre accuracy. (6) Development of an infrastructure for low-force metrology, including the development of appropriate transfer artefacts.

Investigating cell-substrate and cell-cell interactions by means of single-cell-probe force spectroscopy.

PubMed

Moreno-Cencerrado, Alberto; Iturri, Jagoba; Pecorari, Ilaria; D M Vivanco, Maria; Sbaizero, Orfeo; Toca-Herrera, José L

2017-01-01

Cell adhesion forces are typically a mixture of specific and nonspecific cell-substrate and cell-cell interactions. In order to resolve these phenomena, Atomic Force Microscopy appears as a powerful device which can measure cell parameters by means of manipulation of single cells. This method, commonly known as cell-probe force spectroscopy, allows us to control the force applied, the area of interest, the approach/retracting speed, the force rate, and the time of interaction. Here, we developed a novel approach for in situ cantilever cell capturing and measurement of specific cell interactions. In particular, we present a new setup consisting of two different half-surfaces coated either with recrystallized SbpA bacterial cell surface layer proteins (S-layers) or integrin binding Fibronectin, on which MCF-7 breast cancer cells are incubated. The presence of a clear physical boundary between both surfaces benefits for a quick detection of the region under analysis. Thus, quantitative results about SbpA-cell and Fibronectin-cell adhesion forces as a function of the contact time are described. Additionally, the importance of the cell spreading in cell-cell interactions has been studied for surfaces coated with two different Fibronectin concentrations: 20 μg/mL (FN20) and 100 μg/mL (FN100), which impact the number of substrate receptors. Microsc. Res. Tech. 80:124-130, 2017. © 2016 Wiley Periodicals, Inc. © 2016 Wiley Periodicals, Inc.

Force measurements on the molecular interactions between ligand (RGD) and human platelet α IIbβ 3 receptor system

NASA Astrophysics Data System (ADS)

Lee, ImShik; Marchant, Roger E.

2001-10-01

The peptide sequence arginine-glycine-aspartate (RGD) found in fibrinogen, von Willebrand factor, fibronectin, and vitronectin, plays a critical role in platelet adhesion and thrombus formation, when bound to the platelet α IIbβ 3 integrin receptor. Using atomic force microscopy (AFM), we have measured the debonding interaction between an RGD peptide-modified AFM probe tip and a human platelet surface from pN to nN levels of force. The peptide sequence, GSSSGRGDSPA, which contains the biologically active RGDSP sequence with a hydrophilic spacer sequence (GSSSG), was covalently coupled to AFM probe tips. Direct measurements on the debonding force for the RGD ligand - α IIbβ 3 platelet receptor system were carried out in Tyrode buffer at room temperature. Our results show three distinct distributions of debonding forces at a loading rate of 12 nN/s, from which we estimate the debonding force for the single ligand-receptor to be ˜93 pN. The results also show evidence for considerable extension in the flexible sample surface during the debonding process, and a linear correlation between the debonding force and the logarithm of the rate of loading. From our analysis, the zero kinetic off-rate Koff(0), the single molecular binding energy Eb, and the transition state xB, assuming rigid binding, were extracted from the data, and estimated to be 22.6 s -1, -2.64×10 -20 J and 0.1 nm, respectively.

Junction formation of Cu3BiS3 investigated by Kelvin probe force microscopy and surface photovoltage measurements

PubMed Central

Mesa, Fredy; Chamorro, William; Vallejo, William; Baier, Robert; Dittrich, Thomas; Grimm, Alexander; Lux-Steiner, Martha C

2012-01-01

Summary Recently, the compound semiconductor Cu3BiS3 has been demonstrated to have a band gap of ~1.4 eV, well suited for photovoltaic energy harvesting. The preparation of polycrystalline thin films was successfully realized and now the junction formation to the n-type window needs to be developed. We present an investigation of the Cu3BiS3 absorber layer and the junction formation with CdS, ZnS and In2S3 buffer layers. Kelvin probe force microscopy shows the granular structure of the buffer layers with small grains of 20–100 nm, and a considerably smaller work-function distribution for In2S3 compared to that of CdS and ZnS. For In2S3 and CdS buffer layers the KPFM experiments indicate negatively charged Cu3BiS3 grain boundaries resulting from the deposition of the buffer layer. Macroscopic measurements of the surface photovoltage at variable excitation wavelength indicate the influence of defect states below the band gap on charge separation and a surface-defect passivation by the In2S3 buffer layer. Our findings indicate that Cu3BiS3 may become an interesting absorber material for thin-film solar cells; however, for photovoltaic application the band bending at the charge-selective contact has to be increased. PMID:22497001

Atomic Force Microscopy Probing of Receptor–Nanoparticle Interactions for Riboflavin Receptor Targeted Gold–Dendrimer Nanocomposites

PubMed Central

2015-01-01

Riboflavin receptors are overexpressed in malignant cells from certain human breast and prostate cancers, and they constitute a group of potential surface markers important for cancer targeted delivery of therapeutic agents and imaging molecules. Here we report on the fabrication and atomic force microscopy (AFM) characterization of a core–shell nanocomposite consisting of a gold nanoparticle (AuNP) coated with riboflavin receptor-targeting poly(amido amine) dendrimer. We designed this nanocomposite for potential applications such as a cancer targeted imaging material based on its surface plasmon resonance properties conferred by AuNP. We employed AFM as a technique for probing the binding interaction between the nanocomposite and riboflavin binding protein (RfBP) in solution. AFM enabled precise measurement of the AuNP height distribution before (13.5 nm) and after chemisorption of riboflavin-conjugated dendrimer (AuNP–dendrimer; 20.5 nm). Binding of RfBP to the AuNP–dendrimer caused a height increase to 26.7 nm, which decreased to 22.8 nm when coincubated with riboflavin as a competitive ligand, supporting interaction of AuNP–dendrimer and its target protein. In summary, physical determination of size distribution by AFM imaging can serve as a quantitative approach to monitor and characterize the nanoscale interaction between a dendrimer-covered AuNP and target protein molecules in vitro. PMID:24571134

Junction formation of Cu(3)BiS(3) investigated by Kelvin probe force microscopy and surface photovoltage measurements.

PubMed

Mesa, Fredy; Chamorro, William; Vallejo, William; Baier, Robert; Dittrich, Thomas; Grimm, Alexander; Lux-Steiner, Martha C; Sadewasser, Sascha

2012-01-01

Recently, the compound semiconductor Cu(3)BiS(3) has been demonstrated to have a band gap of ~1.4 eV, well suited for photovoltaic energy harvesting. The preparation of polycrystalline thin films was successfully realized and now the junction formation to the n-type window needs to be developed. We present an investigation of the Cu(3)BiS(3) absorber layer and the junction formation with CdS, ZnS and In(2)S(3) buffer layers. Kelvin probe force microscopy shows the granular structure of the buffer layers with small grains of 20-100 nm, and a considerably smaller work-function distribution for In(2)S(3) compared to that of CdS and ZnS. For In(2)S(3) and CdS buffer layers the KPFM experiments indicate negatively charged Cu(3)BiS(3) grain boundaries resulting from the deposition of the buffer layer. Macroscopic measurements of the surface photovoltage at variable excitation wavelength indicate the influence of defect states below the band gap on charge separation and a surface-defect passivation by the In(2)S(3) buffer layer. Our findings indicate that Cu(3)BiS(3) may become an interesting absorber material for thin-film solar cells; however, for photovoltaic application the band bending at the charge-selective contact has to be increased.

A 4 K cryogenic probe for use in magnetic resonance force microscopy experiments

NASA Astrophysics Data System (ADS)

Smith, Doran D.; Alexson, Dimitri A.; Garbini, Joseph L.

2013-09-01

The detailed design of a mechanically detected nuclear magnetic resonance probe using the SPAM (Springiness Preservation by Aligning Magnetization) geometry, operating at 4 K, in vacuum, and a several-Tesla magnetic field is described. The probe head is vibration-isolated well enough from the environment by a three-spring suspension system that the cantilever achieves thermal equilibrium with the environment without the aid of eddy current damping. The probe uses an ultra-soft Si cantilever with a Ni sphere attached to its tip, and magnetic resonance is registered as a change in the resonant frequency of the driven cantilever. The RF system uses frequency sweeps for adiabatic rapid passage using a 500 μm diameter RF coil wound around a sapphire rod. The RF coil and optical fiber of the interferometer used to sense the cantilever's position are both located with respect to the cantilever using a Garbini micropositioner, and the sample stage is mounted on an Attocube nanopositioner.

Noncontact viscoelastic measurement of polymer thin films in a liquid medium using a long-needle AFM

NASA Astrophysics Data System (ADS)

Guan, Dongshi; Barraud, Chloe; Charlaix, Elisabeth; Tong, Penger

We report noncontact measurement of the viscoelastic property of polymer thin films in a liquid medium using frequency-modulation atomic force microscopy (FM-AFM) with a newly developed long-needle probe. The probe contains a long vertical glass fiber with one end adhered to a cantilever beam and the other end with a sharp tip placed near the liquid-film interface. The nanoscale flow generated by the resonant oscillation of the needle tip provides a precise hydrodynamic force acting on the soft surface of the thin film. By accurately measuring the mechanical response of the thin film, we obtain the elastic and loss moduli of the thin film using the linear response theory of elasto-hydrodynamics. The experiment verifies the theory and demonstrates its applications. The technique can be used to accurately measure the viscoelastic property of soft surfaces, such as those made of polymers, nano-bubbles, live cells and tissues. This work was supported by the Research Grants Council of Hong Kong SAR.

Effect of cholesterol on electrostatics in lipid-protein films of a pulmonary surfactant.

PubMed

Finot, Eric; Leonenko, Yuri; Moores, Brad; Eng, Lukas; Amrein, Matthias; Leonenko, Zoya

2010-02-02

We report the changes in the electrical properties of the lipid-protein film of pulmonary surfactant produced by excess cholesterol. Pulmonary surfactant (PS) is a complex lipid-protein mixture that forms a molecular film at the interface of the lung's epithelia. The defined molecular arrangement of the lipids and proteins of the surfactant film gives rise to the locally highly variable electrical surface potential of the interface, which becomes considerably altered in the presence of cholesterol. With frequency modulation Kelvin probe force microscopy (FM-KPFM) and force measurements, complemented by theoretical analysis, we showed that excess cholesterol significantly changes the electric field around a PS film because of the presence of nanometer-sized electrostatic domains and affects the electrostatic interaction of an AFM probe with a PS film. These changes in the local electrical field would greatly alter the interaction of the surfactant film with charged species and would immediately impact the manner in which inhaled (often charged) airborne nanoparticles and fibers might interact with the lung interface.

SPM for functional identification of individual biomolecules

NASA Astrophysics Data System (ADS)

Ros, Robert; Schwesinger, Falk; Padeste, Celestino; Plueckthun, Andreas; Anselmetti, Dario; Guentherodt, Hans-Joachim; Tiefenauer, Louis

1999-06-01

The identification of specific binding molecules is of increasing interest in the context of drug development based on combinatorial libraries. Scanning Probe Microscopy (SPM) is the method of choice to image and probe individual biomolecules on a surface. Functional identification of biomolecules is a first step towards screening on a single molecule level. As a model system we use recombinant single- chain Fv fragment (scFv) antibody molecules directed against the antigen fluorescein. The scFv's are covalently immobilized on a flat gold surface via the C-terminal cysteine, resulting in a high accessibility of the binding site. The antigen is immobilized covalently via a long hydrophilic spacer to the silicon nitride SPM-tip. This arrangement allows a direct measurement of binding forces. Thus, closely related antibody molecules differing in only one amino acid at their binding site could be distinguished. A novel SPM-software has been developed which combines imaging, force spectroscopic modes, and online analysis. This is a major prerequisite for future screening methods.

Frictional behavior of atomically thin sheets: hexagonal-shaped graphene islands grown on copper by chemical vapor deposition.

PubMed

Egberts, Philip; Han, Gang Hee; Liu, Xin Z; Johnson, A T Charlie; Carpick, Robert W

2014-05-27

Single asperity friction experiments using atomic force microscopy (AFM) have been conducted on chemical vapor deposited (CVD) graphene grown on polycrystalline copper foils. Graphene substantially lowers the friction force experienced by the sliding asperity of a silicon AFM tip compared to the surrounding oxidized copper surface by a factor ranging from 1.5 to 7 over loads from the adhesive minimum up to 80 nN. No damage to the graphene was observed over this range, showing that friction force microscopy serves as a facile, high contrast probe for identifying the presence of graphene on Cu. Consistent with studies of epitaxially grown, thermally grown, and mechanically exfoliated graphene films, the friction force measured between the tip and these CVD-prepared films depends on the number of layers of graphene present on the surface and reduces friction in comparison to the substrate. Friction results on graphene indicate that the layer-dependent friction properties result from puckering of the graphene sheet around the sliding tip. Substantial hysteresis in the normal force dependence of friction is observed with repeated scanning without breaking contact with a graphene-covered region. Because of the hysteresis, friction measured on graphene changes with time and maximum applied force, unless the tip slides over the edge of the graphene island or contact with the surface is broken. These results also indicate that relatively weak binding forces exist between the copper foil and these CVD-grown graphene sheets.

Direct Determination of the Equilibrium Unbinding Potential Profile for a Short DNA Duplex from Force Spectroscopy Data

DOE Office of Scientific and Technical Information (OSTI.GOV)

Noy, A

2004-05-04

Modern force microscopy techniques allow researchers to use mechanical forces to probe interactions between biomolecules. However, such measurements often happen in non-equilibrium regime, which precludes straightforward extraction of the equilibrium energy information. Here we use the work averaging method based on Jarzynski equality to reconstruct the equilibrium interaction potential from the unbinding of a complementary 14-mer DNA duplex from the results of non-equilibrium single-molecule measurements. The reconstructed potential reproduces most of the features of the DNA stretching transition, previously observed only in equilibrium stretching of long DNA sequences. We also compare the reconstructed potential with the thermodynamic parameters of DNAmore » duplex unbinding and show that the reconstruction accurately predicts duplex melting enthalpy.« less

Optical and force nanoscopy in microbiology.

PubMed

Xiao, Jie; Dufrêne, Yves F

2016-10-26

Microbial cells have developed sophisticated multicomponent structures and machineries to govern basic cellular processes, such as chromosome segregation, gene expression, cell division, mechanosensing, cell adhesion and biofilm formation. Because of the small cell sizes, subcellular structures have long been difficult to visualize using diffraction-limited light microscopy. During the last three decades, optical and force nanoscopy techniques have been developed to probe intracellular and extracellular structures with unprecedented resolutions, enabling researchers to study their organization, dynamics and interactions in individual cells, at the single-molecule level, from the inside out, and all the way up to cell-cell interactions in microbial communities. In this Review, we discuss the principles, advantages and limitations of the main optical and force nanoscopy techniques available in microbiology, and we highlight some outstanding questions that these new tools may help to answer.

Control of Nanoscale Friction on Gold in an Ionic Liquid by a Potential-Dependent Ionic Lubricant Layer

NASA Astrophysics Data System (ADS)

Sweeney, James; Hausen, Florian; Hayes, Robert; Webber, Grant B.; Endres, Frank; Rutland, Mark W.; Bennewitz, Roland; Atkin, Rob

2012-10-01

The lubricating properties of an ionic liquid on gold surfaces can be controlled through application of an electric potential to the sliding contact. A nanotribology approach has been used to study the frictional behavior of 1-butyl-1-methylpyrrolidinium tris(pentafluoroethyl) trifluorophosphate ([Py1,4]FAP) confined between silica colloid probes or sharp silica tips and a Au(111) substrate using atomic force microscopy. Friction forces vary with potential because the composition of a confined ion layer between the two surfaces changes from cation-enriched (at negative potentials) to anion-enriched (at positive potentials). This offers a new approach to tuning frictional forces reversibly at the molecular level without changing the substrates, employing a self-replenishing boundary lubricant of low vapor pressure.

Quantifying the adhesion and interaction forces between Pseudomonas aeruginosa and natural organic matter.

PubMed

Abu-Lail, Laila I; Liu, Yatao; Atabek, Arzu; Camesano, Terri A

2007-12-01

Atomic force microscopy (AFM) was used to characterize interactions between natural organic matter (NOM), and glass or bacteria. Poly(methacrylic acid) (PMA), soil humic Acid (SHA), and Suwannee River humic Acid (SRHA), were adsorbed to silica AFM probes. Adhesion forces (Fadh) for the interaction of organic-probes and glass slides correlated with organic molecular weight (MW), but not with radius of the organic aggregate (R), charge density (Q), or zeta potential (zeta). Two Pseudomonas aeruginosa strains with different lipopolysaccharides (LPS) were chosen: PAO1 (A+B+), whose LPS have common antigen (A-band) + O-antigen (B-band); and mutant AK1401 (A+B-). Fadh between bacteria and organics correlated with organic MW, R, and Q, but not zeta. PAO1 had lower Fadh with silica than NOM, which was attributed to negative charges from the B-band polymers causing electrostatic repulsion. AK1401 adhered stronger to silica than to the organics, perhaps because the absence of the B-band exposed underlying positively charged proteins. DLVO calculations could not explain the differences in the two bacteria or predict qualitative or quantitative trends in interaction forces in these systems. Molecular-level information from AFM studies can bring us closer to understanding the complex nature of bacterial-NOM interactions.

Nanoscale structural and functional mapping of nacre by scanning probe microscopy techniques

NASA Astrophysics Data System (ADS)

Zhou, Xilong; Miao, Hongchen; Li, Faxin

2013-11-01

Nacre has received great attention due to its nanoscale hierarchical structure and extraordinary mechanical properties. Meanwhile, the nanoscale piezoelectric properties of nacre have also been investigated but the structure-function relationship has never been addressed. In this work, firstly we realized quantitative nanomechanical mapping of nacre of a green abalone using atomic force acoustic microscopy (AFAM). The modulus of the mineral tablets is determined to be ~80 GPa and that of the organic biopolymer no more than 23 GPa, and the organic-inorganic interface width is determined to be about 34 +/- 9 nm. Then, we conducted both AFAM and piezoresponse force microscopy (PFM) mapping in the same scanning area to explore the correlations between the nanomechanical and piezoelectric properties. The PFM testing shows that the organic biopolymer exhibits a significantly stronger piezoresponse than the mineral tablets, and they permeate each other, which is very difficult to reproduce in artificial materials. Finally, the phase hysteresis loops and amplitude butterfly loops were also observed using switching spectroscopy PFM, implying that nacre may also be a bio-ferroelectric material. The obtained nanoscale structural and functional properties of nacre could be very helpful in understanding its deformation mechanism and designing biomimetic materials of extraordinary properties.

Atomic force microscopy of chromatin arrays reveal non-monotonic salt dependence of array compaction in solution

PubMed Central

Krzemien, Katarzyna M.; Beckers, Maximilian; Quack, Salina; Michaelis, Jens

2017-01-01

Compaction of DNA in chromatin is a hallmark of the eukaryotic cell and unravelling its structure is required for an understanding of DNA involving processes. Despite strong experimental efforts, many questions concerning the DNA packing are open. In particular, it is heavily debated whether an ordered structure referred to as the “30 nm fibre” exist in vivo. Scanning probe microscopy has become a cutting edge technology for the high-resolution imaging of DNA- protein complexes. Here, we perform high-resolution atomic force microscopy of non-cross-linked chromatin arrays in liquid, under different salt conditions. A statistical analysis of the data reveals that array compaction is salt dependent in a non-monotonic fashion. A simple physical model can qualitatively explain the observed findings due to the opposing effects of salt dependent stiffening of DNA, nucleosome stability and histone-histone interactions. While for different salt concentrations different compaction states are observed, our data do not provide support for the existence of regular chromatin fibres. Our studies add new insights into chromatin structure, and with that contribute to a further understanding of the DNA condensation. PMID:28296908

HDL particles incorporate into lipid bilayers - a combined AFM and single molecule fluorescence microscopy study.

PubMed

Plochberger, Birgit; Röhrl, Clemens; Preiner, Johannes; Rankl, Christian; Brameshuber, Mario; Madl, Josef; Bittman, Robert; Ros, Robert; Sezgin, Erdinc; Eggeling, Christian; Hinterdorfer, Peter; Stangl, Herbert; Schütz, Gerhard J

2017-11-21

The process, how lipids are removed from the circulation and transferred from high density lipoprotein (HDL) - a main carrier of cholesterol in the blood stream - to cells, is highly complex. HDL particles are captured from the blood stream by the scavenger receptor, class B, type I (SR-BI), the so-called HDL receptor. The details in subsequent lipid-transfer process, however, have not yet been completely understood. The transfer has been proposed to occur directly at the cell surface across an unstirred water layer, via a hydrophobic channel in the receptor, or after HDL endocytosis. The role of the target lipid membrane for the transfer process, however, has largely been overlooked. Here, we studied at the single molecule level how HDL particles interact with synthetic lipid membranes. Using (high-speed) atomic force microscopy and fluorescence correlation spectroscopy (FCS) we found out that, upon contact with the membrane, HDL becomes integrated into the lipid bilayer. Combined force and single molecule fluorescence microscopy allowed us to directly monitor the transfer process of fluorescently labelled amphiphilic lipid probe from HDL particles to the lipid bilayer upon contact.

Microfabrication of Silicon/Ceramic Hybrid Cantilever for Scanning Probe Microscope and Sensor Applications

NASA Astrophysics Data System (ADS)

Wakayama, Takayuki; Kobayashi, Toshinari; Iwata, Nobuya; Tanifuji, Nozomi; Matsuda, Yasuaki; Yamada, Syoji

2003-12-01

We present here new cantilevers for scanning probe microscopy (SPM) and sensor applications, which consist of silicon cantilever beam and ceramic pedestal. Silicon is only used to make cantilever beams and tips. Precision-machinery-made ceramics replaces silicon pedestal part. The ceramics was recently developed by Sumikin Ceramics and Quarts Co., Ltd. and can be machined precisely with end mill cutting. Many silicon beams are fabricated at once from a wafer using batch fabrication method. Therefore, SPM probes can be fabricated in high productivity and in low cost. These beams are transferred with transfer technique and are bonded on the ceramic pedestal with epoxy glue. We demonstrate here atomic force microscope (AFM) and gas sensor applications of the hybrid structure. In a gas sensor application, the ends of the cantilever are selectively modified with zeolite crystals as a sensitive layer. The bonding strength is enough for each application.

A new non-destructive readout by using photo-recovered surface potential contrast

NASA Astrophysics Data System (ADS)

Wang, Le; Jin, Kui-Juan; Gu, Jun-Xing; Ma, Chao; He, Xu; Zhang, Jiandi; Wang, Can; Feng, Yu; Wan, Qian; Shi, Jin-An; Gu, Lin; He, Meng; Lu, Hui-Bin; Yang, Guo-Zhen

2014-11-01

Ferroelectric random access memory is still challenging in the feature of combination of room temperature stability, non-destructive readout and high intensity storage. As a non-contact and non-destructive information readout method, surface potential has never been paid enough attention because of the unavoidable decay of the surface potential contrast between oppositely polarized domains. That is mainly due to the recombination of the surface movable charges around the domain walls. Here, by introducing a laser beam into the combination of piezoresponse force microscopy and Kelvin probe force microscopy, we demonstrate that the surface potential contrast of BiFeO3 films can be recovered under light illumination. The recovering mechanism is understood based on the redistribution of the photo-induced charges driven by the internal electric field. Furthermore, we have created a 12-cell memory pattern based on BiFeO3 films to show the feasibility of such photo-assisted non-volatile and non-destructive readout of the ferroelectric memory.

High flexibility of DNA on short length scales probed by atomic force microscopy.

PubMed

Wiggins, Paul A; van der Heijden, Thijn; Moreno-Herrero, Fernando; Spakowitz, Andrew; Phillips, Rob; Widom, Jonathan; Dekker, Cees; Nelson, Philip C

2006-11-01

The mechanics of DNA bending on intermediate length scales (5-100 nm) plays a key role in many cellular processes, and is also important in the fabrication of artificial DNA structures, but previous experimental studies of DNA mechanics have focused on longer length scales than these. We use high-resolution atomic force microscopy on individual DNA molecules to obtain a direct measurement of the bending energy function appropriate for scales down to 5 nm. Our measurements imply that the elastic energy of highly bent DNA conformations is lower than predicted by classical elasticity models such as the worm-like chain (WLC) model. For example, we found that on short length scales, spontaneous large-angle bends are many times more prevalent than predicted by the WLC model. We test our data and model with an interlocking set of consistency checks. Our analysis also shows how our model is compatible with previous experiments, which have sometimes been viewed as confirming the WLC.

Bipolarization and Poleward Flux Correlate during Xenopus Extract Spindle AssemblyV⃞

PubMed Central

Mitchison, T.J.; Maddox, P.; Groen, A.; Cameron, L.; Perlman, Z.; Ohi, R.; Desai, A.; Salmon, E.D.; Kapoor, T.M.

2004-01-01

We investigated the mechanism by which meiotic spindles become bipolar and the correlation between bipolarity and poleward flux, using Xenopus egg extracts. By speckle microscopy and computational alignment, we find that monopolar sperm asters do not show evidence for flux, partially contradicting previous work. We account for the discrepancy by describing spontaneous bipolarization of sperm asters that was missed previously. During spontaneous bipolarization, onset of flux correlated with onset of bipolarity, implying that antiparallel microtubule organization may be required for flux. Using a probe for TPX2 in addition to tubulin, we describe two pathways that lead to spontaneous bipolarization, new pole assembly near chromatin, and pole splitting. By inhibiting the Ran pathway with excess importin-alpha, we establish a role for chromatin-derived, antiparallel overlap bundles in generating the sliding force for flux, and we examine these bundles by electron microscopy. Our results highlight the importance of two processes, chromatin-initiated microtubule nucleation, and sliding forces generated between antiparallel microtubules, in self-organization of spindle bipolarity and poleward flux. PMID:15385629

Nanoparticle-Cell Interaction: A Cell Mechanics Perspective.

PubMed

Septiadi, Dedy; Crippa, Federica; Moore, Thomas Lee; Rothen-Rutishauser, Barbara; Petri-Fink, Alke

2018-05-01

Progress in the field of nanoparticles has enabled the rapid development of multiple products and technologies; however, some nanoparticles can pose both a threat to the environment and human health. To enable their safe implementation, a comprehensive knowledge of nanoparticles and their biological interactions is needed. In vitro and in vivo toxicity tests have been considered the gold standard to evaluate nanoparticle safety, but it is becoming necessary to understand the impact of nanosystems on cell mechanics. Here, the interaction between particles and cells, from the point of view of cell mechanics (i.e., bionanomechanics), is highlighted and put in perspective. Specifically, the ability of intracellular and extracellular nanoparticles to impair cell adhesion, cytoskeletal organization, stiffness, and migration are discussed. Furthermore, the development of cutting-edge, nanotechnology-driven tools based on the use of particles allowing the determination of cell mechanics is emphasized. These include traction force microscopy, colloidal probe atomic force microscopy, optical tweezers, magnetic manipulation, and particle tracking microrheology. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ultra-violet absorption induced modifications in bulk and nanoscale electrical transport properties of Al-doped ZnO thin films

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Mohit; Basu, Tanmoy; Som, Tapobrata, E-mail: tsom@iopb.res.in

Using conductive atomic force microscopy and Kelvin probe force microscopy, we study local electrical transport properties in aluminum-doped zinc oxide (ZnO:Al or AZO) thin films. Current mapping shows a spatial variation in conductivity which corroborates well with the local mapping of donor concentration (∼10{sup 20 }cm{sup −3}). In addition, a strong enhancement in the local current at grains is observed after exposing the film to ultra-violet (UV) light which is attributed to persistent photocurrent. Further, it is shown that UV absorption gives a smooth conduction in AZO film which in turn gives rise to an improvement in the bulk photoresponsivity ofmore » an n-AZO/p-Si heterojunction diode. This finding is in contrast to the belief that UV absorption in an AZO layer leads to an optical loss for the underneath absorbing layer of a heterojunction solar cell.« less

Towards nano-physiology of insects with atomic force microscopy.

PubMed

Dokukin, M E; Guz, N V; Sokolov, I

2011-02-01

Little study of insects with modern nanotechnology tools has been done so far. Here we use one of such tool, atomic force microscopy (AFM) to study surface oscillations of the ladybird beetles (Hippodamia convergens) measured in different parts of the insect at picometer level. This allows us to record a much broader spectral range of possible surface vibrations (up to several kHz) than the previously studied oscillations due to breathing, heartbeat cycles, coelopulses, etc. (up to 5-10Hz). Here we demonstrate three different ways with which one can identify the origins of the observed peaks - by physical positioning the probe near a specific organ, and by using biological or chemical stimuli. We report on identification of high frequency peaks associated with H. convergens heart, spiracular closer muscles, and oscillations associated with muscles activated while drinking. The method, being a relatively non-invasive technique providing a new type of information, may be useful in developing "nanophysiology" of insects. Copyright © 2010 Elsevier Ltd. All rights reserved.

Optical detection of ultrasound using an apertureless near-field scanning optical microscopy system

NASA Astrophysics Data System (ADS)

Ahn, Phillip; Zhang, Zhen; Sun, Cheng; Balogun, Oluwaseyi

2013-01-01

Laser ultrasonics techniques are power approaches for non-contact generation and detection of high frequency ultrasound on a local scale. In these techniques, optical diffraction limits the spatial information that can be accessed from a measurement. In order to improve the lateral spatial resolution, we incorporate an apertureless near-field scanning optical microscope (aNSOM) into laser ultrasonics setup for local detection of laser generated ultrasound. The aNSOM technique relies on the measurement of a weak backscattered near-field light intensity resulting from the oblique illumination of a nanoscale probe-tip positioned close to a sample surface. We enhance the optical near-field intensity by coupling light to surface plasmon polaritons (SPPs) on the shaft of an atomic force microscopy (AFM) cantilever. The SPPs propagate down the AFM shaft, localize at the tip apex, and are backscattered to the far-field when the separation distance between the probe tip and the sample surface is comparable to the probe-tip radius. The backscattered near-field intensity is dynamically modulated when an ultrasonic wave arrives at the sample surface leading to a transient change in the tip-sample separation distance. We present experimental results detailing measurement of broadband and narrowband laser generated ultrasound in solids with frequencies reaching up to 180 MHz range.

Nanometal Skin of Plasmonic Heterostructures for Highly Efficient Near-Field Scattering Probes

NASA Astrophysics Data System (ADS)

Zito, Gianluigi; Rusciano, Giulia; Vecchione, Antonio; Pesce, Giuseppe; di Girolamo, Rocco; Malafronte, Anna; Sasso, Antonio

2016-08-01

In this work, atomic force microscopy probes are functionalized by virtue of self-assembling monolayers of block copolymer (BCP) micelles loaded either with clusters of silver nanoparticles or bimetallic heterostructures consisting of mixed species of silver and gold nanoparticles. The resulting self-organized patterns allow coating the tips with a sort of nanometal skin made of geometrically confined nanoislands. This approach favors the reproducible engineering and tuning of the plasmonic properties of the resulting structured tip by varying the nanometal loading of the micelles. The newly conceived tips are applied for experiments of tip-enhanced Raman scattering (TERS) spectroscopy and scattering-type scanning near-field optical microscopy (s-SNOM). TERS and s-SNOM probe characterizations on several standard Raman analytes and patterned nanostructures demonstrate excellent enhancement factor with the possibility of fast scanning and spatial resolution <12 nm. In fact, each metal nanoisland consists of a multiscale heterostructure that favors large scattering and near-field amplification. Then, we verify the tips to allow challenging nongap-TER spectroscopy on thick biosamples. Our approach introduces a synergistic chemical functionalization of the tips for versatile inclusion and delivery of plasmonic nanoparticles at the tip apex, which may promote the tuning of the plasmonic properties, a large enhancement, and the possibility of adding new degrees of freedom for tip functionalization.

Single & Multiprobe Apertureless Thermal Imaging of Electromagnetic Excitation Over A Wide Range of Wavelengths

NASA Astrophysics Data System (ADS)

Dekhter, Rimma; Lewis, Aaron; Kokotov, Sophia; Hamra, Patricia; Fleischman, Boaz; Taha, Hesham

2013-03-01

Near-field optical effects have generally been detected using photodetectors. There are no reports on the use of the temperature changes caused by electromagnetic radiation using thermal sensing probes for scanned probe microscopy. In this paper we apply our development of such probes to monitor the effects of electromagnetic radiation at a number of different wavelengths using the heating caused in a sample by specific wavelengths and their propagation. The paper will catalogue effects over a wide spectrum of wavelengths from the near to mid infrared. The thermal sensing probes are based on glass nanopipettes that have metal wires that make a contact at the very tip of a tapered glass structure. These probes are cantilevered and use normal force tuning fork methodology to bring them either into contact or near-contact since this feedback method has no jump to contact instability associated with it. Data will be shown that defines the resolution of such thermal sensing to at least the 32 nm level. In addition the probes have the important attribute of having a highly exposed tip that allows for either optical sensing methodologies with a lens either from directly above or below or heat sensing with a single or additional probe in a multiprobe scanning probe system.

New Algorithm to Enable Construction and Display of 3D Structures from Scanning Probe Microscopy Images Acquired Layer-by-Layer.

PubMed

Deng, William Nanqiao; Wang, Shuo; Ventrici de Souza, Joao; Kuhl, Tonya L; Liu, Gang-Yu

2018-06-25

Scanning probe microscopy (SPM), such as atomic force microscopy (AFM), is widely known for high-resolution imaging of surface structures and nanolithography in two dimensions (2D), providing important physical insights into surface science and material science. This work reports a new algorithm to enable construction and display of layer-by-layer 3D structures from SPM images. The algorithm enables alignment of SPM images acquired during layer-by-layer deposition and removal of redundant features and faithfully constructs the deposited 3D structures. The display uses a "see-through" strategy to enable the structure of each layer to be visible. The results demonstrate high spatial accuracy as well as algorithm versatility; users can set parameters for reconstruction and display as per image quality and research needs. To the best of our knowledge, this method represents the first report to enable SPM technology for 3D imaging construction and display. The detailed algorithm is provided to facilitate usage of the same approach in any SPM software. These new capabilities support wide applications of SPM that require 3D image reconstruction and display, such as 3D nanoprinting and 3D additive and subtractive manufacturing and imaging.

Polarization Control via He-Ion Beam Induced Nanofabrication in Layered Ferroelectric Semiconductors

DOE PAGES

Belianinov, Alex; Iberi, Vighter; Tselev, Alexander; ...

2016-02-23

Rapid advanced in nanoscience rely on continuous improvements of matter manipulation at near atomic scales. Currently, well characterized, robust, resist-based lithography carries the brunt of the nanofabrication process. However, use of local electron, ion and physical probe methods is also expanding, driven largely by their ability to fabricate without the multi-step preparation processes that can result in contamination from resists and solvents. Furthermore, probe based methods extend beyond nanofabrication to nanomanipulation and imaging, vital ingredients to rapid transition to prototyping and testing of layered 2D heterostructured devices. In this work we demonstrate that helium ion interaction, in a Helium Ionmore » Microscope (HIM), with the surface of bulk copper indium thiophosphate CuM IIIP 2X 6 (M = Cr, In; X= S, Se), (CITP) results in the control of ferroelectric domains, and growth of cylindrical nanostructures with enhanced conductivity; with material volumes scaling with the dosage of the beam. The nanostructures are oxygen rich, sulfur poor, and with the copper concentration virtually unchanged as confirmed by Energy Dispersive X-ray (EDX). Scanning Electron Microscopy (SEM) imaging contrast as well as Scanning Microwave Microscopy (SMM) measurements suggest enhanced conductivity in the formed particle, whereas Atomic Force Microscopy (AFM) measurements indicate that the produced structures have lower dissipation and a lower Young s modulus.« less

Morphology and force probing of primary murine liver sinusoidal endothelial cells.

PubMed

Zapotoczny, B; Owczarczyk, K; Szafranska, K; Kus, E; Chlopicki, S; Szymonski, M

2017-07-01

Liver sinusoidal endothelial cells (LSECs) represent unique type of endothelial cells featured by their characteristic morphology, ie, lack of a basement membrane and presence of fenestrations-transmembrane pores acting as a dynamic filter between the vascular space and the liver parenchyma. Delicate structure of LSECs membrane combined with a submicron size of fenestrations hinders their visualization in live cells. In this work, we apply atomic force microscopy contact mode to characterize fenestrations in LSECs. We reveal the structure of fenestrations in live LSECs. Moreover, we show that the high-resolution imaging of fenestrations is possible for the glutaraldehyde-fixed LSECs. Finally, thorough information about the morphology of LSECs including great contrast in visualization of sieve plates and fenestrations is provided using Force Modulation mode. We show also the ability to precisely localize the cell nuclei in fixed LSECs. It can be helpful for more precise description of nanomechanical properties of cell nuclei using atomic force microscopy. Presented methodology combining high-quality imaging of fixed cells with an additional nanomechanical information of both live and fixed LSECs provides a unique approach to study LSECs morphology and nanomechanics that could foster understanding of the role of LSECs in maintaining liver homeostasis. Copyright © 2017 John Wiley & Sons, Ltd.

Detailed characterisation of focused ion beam induced lateral damage on silicon carbide samples by electrical scanning probe microscopy and transmission electron microscopy

NASA Astrophysics Data System (ADS)

Stumpf, F.; Abu Quba, A. A.; Singer, P.; Rumler, M.; Cherkashin, N.; Schamm-Chardon, S.; Cours, R.; Rommel, M.

2018-03-01

The lateral damage induced by focused ion beam on silicon carbide was characterized using electrical scanning probe microscopy (SPM), namely, scanning spreading resistance microscopy and conductive atomic force microscopy (c-AFM). It is shown that the damage exceeds the purposely irradiated circles with a radius of 0.5 μm by several micrometres, up to 8 μm for the maximum applied ion dose of 1018 cm-2. Obtained SPM results are critically compared with earlier findings on silicon. For doses above the amorphization threshold, in both cases, three different areas can be distinguished. The purposely irradiated area exhibits resistances smaller than the non-affected substrate. A second region with strongly increasing resistance and a maximum saturation value surrounds it. The third region shows the transition from maximum resistance to the base resistance of the unaffected substrate. It correlates to the transition from amorphized to defect-rich to pristine crystalline substrate. Additionally, conventional transmission electron microscopy (TEM) and annular dark-field STEM were used to complement and explain the SPM results and get a further understanding of the defect spreading underneath the surface. Those measurements also show three different regions that correlate well with the regions observed from electrical SPM. TEM results further allow to explain observed differences in the electrical results for silicon and silicon carbide which are most prominent for ion doses above 3 × 1016 cm-2. Furthermore, the conventional approach to perform current-voltage measurements by c-AFM was critically reviewed and several improvements for measurement and analysis process were suggested that result in more reliable and impactful c-AFM data.