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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.
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Carbon nanotube mechanics in scanning probe microscopy
NASA Astrophysics Data System (ADS)
Strus, Mark Christopher
Carbon nanotubes (CNTs) possess unique electrical, thermal, and mechanical properties which have led to the development of novel nanomechanical materials and devices. In this thesis, the mechanical properties of carbon nanotubes are studied with an Atomic Force Microscope (AFM) and, conversely, the use of CNTs to enhance conventional AFM probes is also investigated. First, the performance of AFM probes with multiwalled CNT tips are evaluated during attractive regime AFM imaging of high aspect ratio structures. The presented experimental results show two distinct imaging artifacts, the divot and large ringing artifacts, which are inherent to such CNT AFM probes. Through the adjustment of operating parameters, the connection of these artifacts to CNT bending, adhesion, and stiction is described qualitatively and explained. Next, the adhesion and peeling of CNTs on different substrates is quantitatively investigated with theoretical models and a new AFM mode for nanomechanical peeling. The theoretical model uncovers the rich physics of peeling of CNTs from surfaces, including sudden transitions between different geometric configurations of the nanotube with vastly different interfacial energies. The experimental peeling of CNTs is shown to be capable of resolving differences in CNT peeling energies at attoJoule levels on different materials. AFM peeling force spectroscopy is further studied on a variety of materials, including several polymers, to demonstrate the capability of direct measurement of interfacial energy between an individual nanotube or nanofiber and a given material surface. Theoretical investigations demonstrate that interfacial and flexural energies can be decoupled so that the work of the applied peeling force can be used to estimate the CNT-substrate interfacial fracture energy and nanotube's flexural stiffness. Hundreds of peeling force experiments on graphite, epoxy, and polyimide demonstrate that the peeling force spectroscopy offers a convenient experimental framework to quickly screen different combinations of polymers and functionalized nanotubes for optimal interfacial strength. Finally, multiple CNT AFM probe oscillation states in tapping mode AFM as the cantilever is brought closer to a sample are fully investigated, including two kinds of permanent contact and two types of intermittent contact. Large deformation continuum elastica models of MWCNTs with different end boundary conditions are used to identify whether the CNT remains anchored to the sample in line-contact or in point-contact in the permanent contact regime. Energy dissipation spectroscopy and phase contrast are demonstrated as a way to predict the state of CNT-substrate boundary condition in the intermittent tapping regime on different substrates and to highlight the implications of these different imaging regimes for critical dimension AFM, biological sensing, and nanolithography. Together, this work studies the effect of CNT mechanical interactions in AFM, including artifact-avoidance optimization of and new compositional mapping using CNT AFM probes as well as novel techniques that will potentially enhance the future development of CNT-based nanodevices and materials.
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Noncontact Atomic Force Microscopy: An Emerging Tool for Fundamental Catalysis Research.
PubMed
Altman, Eric I; Baykara, Mehmet Z; Schwarz, Udo D
2015-09-15
Although atomic force microscopy (AFM) was rapidly adopted as a routine surface imaging apparatus after its introduction in 1986, it has not been widely used in catalysis research. The reason is that common AFM operating modes do not provide the atomic resolution required to follow catalytic processes; rather the more complex noncontact (NC) mode is needed. Thus, scanning tunneling microscopy has been the principal tool for atomic scale catalysis research. In this Account, recent developments in NC-AFM will be presented that offer significant advantages for gaining a complete atomic level view of catalysis. The main advantage of NC-AFM is that the image contrast is due to the very short-range chemical forces that are of interest in catalysis. This motivated our development of 3D-AFM, a method that yields quantitative atomic resolution images of the potential energy surfaces that govern how molecules approach, stick, diffuse, and rebound from surfaces. A variation of 3D-AFM allows the determination of forces required to push atoms and molecules on surfaces, from which diffusion barriers and variations in adsorption strength may be obtained. Pushing molecules towards each other provides access to intermolecular interaction between reaction partners. Following reaction, NC-AFM with CO-terminated tips yields textbook images of intramolecular structure that can be used to identify reaction intermediates and products. Because NC-AFM and STM contrast mechanisms are distinct, combining the two methods can produce unique insight. It is demonstrated for surface-oxidized Cu(100) that simultaneous 3D-AFM/STM yields resolution of both the Cu and O atoms. Moreover, atomic defects in the Cu sublattice lead to variations in the reactivity of the neighboring O atoms. It is shown that NC-AFM also allows a straightforward imaging of work function variations which has been used to identify defect charge states on catalytic surfaces and to map charge transfer within an individual molecule. These advances highlight the potential for NC-AFM-based methods to become the cornerstone upon which a quantitative atomic scale view of each step of a catalytic process may be gained. Realizing this potential will rely on two breakthroughs: (1) development of robust methods for tip functionalization and (2) simplification of NC-AFM instrumentation and control schemes. Quartz force sensors may offer paths forward in both cases. They allow any material with an atomic asperity to be used as a tip, opening the door to a wide range of surface functionalization chemistry. In addition, they do not suffer from the instabilities that motivated the initial adoption of complex control strategies that are still used today.
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Diagnosis of cervical cancer cell taken from scanning electron and atomic force microscope images of the same patients using discrete wavelet entropy energy and Jensen Shannon, Hellinger, Triangle Measure classifier.
PubMed
Aytac Korkmaz, Sevcan
2016-05-05
The aim of this article is to provide early detection of cervical cancer by using both Atomic Force Microscope (AFM) and Scanning Electron Microscope (SEM) images of same patient. When the studies in the literature are examined, it is seen that the AFM and SEM images of the same patient are not used together for early diagnosis of cervical cancer. AFM and SEM images can be limited when using only one of them for the early detection of cervical cancer. Therefore, multi-modality solutions which give more accuracy results than single solutions have been realized in this paper. Optimum feature space has been obtained by Discrete Wavelet Entropy Energy (DWEE) applying to the 3×180 AFM and SEM images. Then, optimum features of these images are classified with Jensen Shannon, Hellinger, and Triangle Measure (JHT) Classifier for early diagnosis of cervical cancer. However, between classifiers which are Jensen Shannon, Hellinger, and triangle distance have been validated the measures via relationships. Afterwards, accuracy diagnosis of normal, benign, and malign cervical cancer cell was found by combining mean success rates of Jensen Shannon, Hellinger, and Triangle Measure which are connected with each other. Averages of accuracy diagnosis for AFM and SEM images by averaging the results obtained from these 3 classifiers are found as 98.29% and 97.10%, respectively. It has been observed that AFM images for early diagnosis of cervical cancer have higher performance than SEM images. Also in this article, surface roughness of malign AFM images in the result of the analysis made for the AFM images, according to the normal and benign AFM images is observed as larger, If the volume of particles has found as smaller. Copyright © 2016 Elsevier B.V. All rights reserved.
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Simultaneous noncontact AFM and STM of Ag:Si(111)-(3×3)R30∘
NASA Astrophysics Data System (ADS)
Sweetman, Adam; Stannard, Andrew; Sugimoto, Yoshiaki; Abe, Masayuki; Morita, Seizo; Moriarty, Philip
2013-02-01
The Ag:Si(111)-(3×3)R30∘ surface structure has attracted considerable debate concerning interpretation of scanning tunneling microscope (STM) and noncontact atomic force microscope (NC-AFM) images. In particular, the accepted interpretation of atomic resolution images in NC-AFM has been questioned by theoretical and STM studies. In this paper, we use combined NC-AFM and STM to conclusively show that the inequivalent trimer (IET) configuration best describes the surface ground state. Thermal-averaging effects result in a honeycomb-chained-trimer (HCT) appearance at room temperature, in contrast to studies suggesting that the IET configuration remains stable at higher temperatures [Zhang, Gustafsson, and Johansson, Phys. Rev. BPRBMDO1098-012110.1103/PhysRevB.74.201304 74, 201304(R) (2006) and J. Phys.: Conf. Ser.1742-658810.1088/1742-6596/61/1/264 61, 1336 (2007)]. We also comment on results obtained at an intermediate temperature that suggest an intriguing difference between the imaging mechanisms of NC-AFM and STM on structurally fluctuating samples.
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Inverting dynamic force microscopy: From signals to time-resolved interaction forces
PubMed Central
Stark, Martin; Stark, Robert W.; Heckl, Wolfgang M.; Guckenberger, Reinhard
2002-01-01
Transient forces between nanoscale objects on surfaces govern friction, viscous flow, and plastic deformation, occur during manipulation of matter, or mediate the local wetting behavior of thin films. To resolve transient forces on the (sub) microsecond time and nanometer length scale, dynamic atomic force microscopy (AFM) offers largely unexploited potential. Full spectral analysis of the AFM signal completes dynamic AFM. Inverting the signal formation process, we measure the time course of the force effective at the sensing tip. This approach yields rich insight into processes at the tip and dispenses with a priori assumptions about the interaction, as it relies solely on measured data. Force measurements on silicon under ambient conditions demonstrate the distinct signature of the interaction and reveal that peak forces exceeding 200 nN are applied to the sample in a typical imaging situation. These forces are 2 orders of magnitude higher than those in covalent bonds. PMID:12070341
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A low-noise measurement system for scanning thermal microscopy resistive nanoprobes based on a transformer ratio-arm bridge
NASA Astrophysics Data System (ADS)
Świątkowski, Michał; Wojtuś, Arkadiusz; Wielgoszewski, Grzegorz; Rudek, Maciej; Piasecki, Tomasz; Jóźwiak, Grzegorz; Gotszalk, Teodor
2018-04-01
Atomic force microscopy (AFM) is a widely used technology for the investigation and characterization of nanomaterials. Its functionality can be easily expanded by applying dedicated extension modules, which can measure the electrical conductivity or temperature of a sample. In this paper, we introduce a transformer ratio-arm bridge setup dedicated to AFM-based thermal imaging. One of the key features of the thermal module is the use of a low-power driving signal that prevents undesirable tip heating during resistance measurement, while the other is the sensor location in a ratio-arm transformer bridge working in the audio frequency range and ensuring galvanic isolation of the tip, enabling contact-mode scanning of electronic circuits. The proposed expansion module is compact and it can be integrated onto the AFM head close to the cantilever. The calibration process and the resolution of 11 mK of the proposed setup are shown.
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An intelligent control scheme for precise tip-motion control in atomic force microscopy.
PubMed
Wang, Yanyan; Hu, Xiaodong; Xu, Linyan
2016-01-01
The paper proposes a new intelligent control method to precisely control the tip motion of the atomic force microscopy (AFM). The tip moves up and down at a high rate along the z direction during scanning, requiring the utilization of a rapid feedback controller. The standard proportional-integral (PI) feedback controller is commonly used in commercial AFMs to enable topography measurements. The controller's response performance is determined by the set of the proportional (P) parameter and the integral (I) parameter. However, the two parameters cannot be automatically altered simultaneously according to the scanning speed and the surface topography during continuors scanning, leading to an inaccurate measurement. Thus a new intelligent controller combining the fuzzy controller and the PI controller is put forward in the paper. The new controller automatically selects the most appropriate PI parameters to achieve a fast response rate on basis of the tracking errors. In the experimental setup, the new controller is realized with a digital signal process (DSP) system, implemented in a conventional AFM system. Experiments are carried out by comparing the new method with the standard PI controller. The results demonstrate that the new method is more robust and effective for the precise tip motion control, corresponding to the achievement of a highly qualified image by shortening the response time of the controller. © Wiley Periodicals, Inc.
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A universal fluid cell for the imaging of biological specimens in the atomic force microscope.
PubMed
Kasas, Sandor; Radotic, Ksenja; Longo, Giovanni; Saha, Bashkar; Alonso-Sarduy, Livan; Dietler, Giovanni; Roduit, Charles
2013-04-01
Recently, atomic force microscope (AFM) manufacturers have begun producing instruments specifically designed to image biological specimens. In most instances, they are integrated with an inverted optical microscope, which permits concurrent optical and AFM imaging. An important component of the set-up is the imaging chamber, whose design determines the nature of the experiments that can be conducted. Many different imaging chamber designs are available, usually designed to optimize a single parameter, such as the dimensions of the substrate or the volume of fluid that can be used throughout the experiment. In this report, we present a universal fluid cell, which simultaneously optimizes all of the parameters that are important for the imaging of biological specimens in the AFM. This novel imaging chamber has been successfully tested using mammalian, plant, and microbial cells. Copyright © 2013 Wiley Periodicals, Inc.
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AFM probing in aqueous environment of Staphylococcus epidermidis cells naturally immobilised on glass: physico-chemistry behind the successful immobilisation.
PubMed
Méndez-Vilas, A; Gallardo-Moreno, A M; Calzado-Montero, R; González-Martín, M L
2008-05-01
AFM probing of microbial cells in liquid environments usually requires them to be physically or chemically attached to a solid surface. The fixation mechanisms may influence the nanomechanical characterization done by force curve mapping using an AFM. To study the response of a microbial cell surface to this kind of local measurement this study attempts to overcome the problem associated to the uncertainties introduced by the different fixation treatments by analysing the surface of Staphylococcus epidermidis cells naturally (non-artificially mediated) immobilised on a glass support surface. The particularities of this natural bacterial fixation process for AFM surface analysis are discussed in terms of theoretical predictions of the XDLVO model applied to the systems bacteria/support substratum and bacteria/AFM tip immersed in water. In this sense, in the first part of this study the conditions for adequate natural fixation of three S. epidermidis strains have been analyzed by taking into account the geometries of the bacterium, substrate and tip. In the second part, bacteria are probed without the risk of any possible artefacts due to the mechanical or chemical fixation procedures. Forces measured over the successfully adhered cells have (directly) shown that the untreated bacterial surface suffers from a combination of both reversible and non-reversible deformations during acquisition of force curves all taken under the same operational conditions. This is revealed directly through high-resolution tapping-mode imaging of the bacterial surface immediately following force curve mapping. The results agree with the two different types of force curves that were repeatedly obtained. Interestingly, one type of these force curves suggests that the AFM tip is breaking (rather than pushing) the cell surface during acquisition of the force curve. In this case, adhesive peaks were always observed, suggesting a mechanical origin of the measured pull-off forces. The other type of force curves shows no adhesive peaks and exhibits juxtaposing of approaching and retraction curves, reflecting elastic deformations.
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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.
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Non-contact lateral force microscopy.
PubMed
Weymouth, A J
2017-08-16
The goal of atomic force microscopy (AFM) is to measure the short-range forces that act between the tip and the surface. The signal recorded, however, includes long-range forces that are often an unwanted background. Lateral force microscopy (LFM) is a branch of AFM in which a component of force perpendicular to the surface normal is measured. If we consider the interaction between tip and sample in terms of forces, which have both direction and magnitude, then we can make a very simple yet profound observation: over a flat surface, long-range forces that do not yield topographic contrast have no lateral component. Short-range interactions, on the other hand, do. Although contact-mode is the most common LFM technique, true non-contact AFM techniques can be applied to perform LFM without the tip depressing upon the sample. Non-contact lateral force microscopy (nc-LFM) is therefore ideal to study short-range forces of interest. One of the first applications of nc-LFM was the study of non-contact friction. A similar setup is used in magnetic resonance force microscopy to detect spin flipping. More recently, nc-LFM has been used as a true microscopy technique to systems unsuitable for normal force microscopy.
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Tip in–light on: Advantages, challenges, and applications of combining AFM and Raman microscopy on biological samples
PubMed Central
Gierlinger, Notburga
2016-01-01
Abstract Scanning probe microscopies and spectroscopies, especially AFM and Confocal Raman microscopy are powerful tools to characterize biological materials. They are both non‐destructive methods and reveal mechanical and chemical properties on the micro and nano‐scale. In the last years the interest for increasing the lateral resolution of optical and spectral images has driven the development of new technologies that overcome the diffraction limit of light. The combination of AFM and Raman reaches resolutions of about 50–150 nm in near‐field Raman and 1.7–50 nm in tip enhanced Raman spectroscopy (TERS) and both give a molecular information of the sample and the topography of the scanned surface. In this review, the mentioned approaches are introduced, the main advantages and problems for application on biological samples discussed and some examples for successful experiments given. Finally the potential of colocated AFM and Raman measurements is shown on a case study of cellulose‐lignin films: the topography structures revealed by AFM can be related to a certain chemistry by the colocated Raman scan and additionally the mechanical properties be revealed by using the digital pulsed force mode. Microsc. Res. Tech. 80:30–40, 2017. © 2016 Wiley Periodicals, Inc. PMID:27514318
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Direct, concurrent measurements of the forces and currents affecting DNA in a nanopore with comparable topography.
PubMed
Nelson, Edward M; Li, Hui; Timp, Gregory
2014-06-24
We report direct, concurrent measurements of the forces and currents associated with the translocation of a single-stranded DNA molecule tethered to the tip of an atomic force microscope (AFM) cantilever through synthetic pores with topagraphies comparable to the DNA. These measurements were performed to gauge the signal available for sequencing and the electric force required to impel a single molecule through synthetic nanopores ranging from 1.0 to 3.5 nm in diameter in silicon nitride membranes 6-10 nm thick. The measurements revealed that a molecule can slide relatively frictionlessly through a pore, but regular fluctuations are observed intermittently in the force (and the current) every 0.35-0.72 nm, which are attributed to individual nucleotides translating through the nanopore in a turnstile-like motion.
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A Student-Built Scanning Tunneling Microscope
ERIC Educational Resources Information Center
Ekkens, Tom
2015-01-01
Many introductory and nanotechnology textbooks discuss the operation of various microscopes including atomic force (AFM), scanning tunneling (STM), and scanning electron microscopes (SEM). In a nanotechnology laboratory class, students frequently utilize microscopes to obtain data without a thought about the detailed operation of the tool itself.…
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Atomic force microscopic study of the effects of ethanol on yeast cell surface morphology.
PubMed
Canetta, Elisabetta; Adya, Ashok K; Walker, Graeme M
2006-02-01
The detrimental effects of ethanol toxicity on the cell surface morphology of Saccharomyces cerevisiae (strain NCYC 1681) and Schizosaccharomyces pombe (strain DVPB 1354) were investigated using an atomic force microscope (AFM). In combination with culture viability and mean cell volume measurements AFM studies allowed us to relate the cell surface morphological changes, observed on nanometer lateral resolution, with the cellular stress physiology. Exposing yeasts to increasing stressful concentrations of ethanol led to decreased cell viabilities and mean cell volumes. Together with the roughness and bearing volume analyses of the AFM images, the results provided novel insight into the relative ethanol tolerance of S. cerevisiae and Sc. pombe.
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Imaging powders with the atomic force microscope: from biominerals to commercial materials.
PubMed
Friedbacher, G; Hansma, P K; Ramli, E; Stucky, G D
1991-09-13
Atomically resolved images of pressed powder samples have been obtained with the atomic force microscope (AFM). The technique was successful in resolving the particle, domain, and atomic structure of pismo clam (Tivela stultorum) and sea urchin (Strongylocentrotus purpuratus) shells and of commercially available calcium carbonate (CaCO(3)) and strontium carbonate (SrCO(3)) powders. Grinding and subsequent pressing of the shells did not destroy the microstructure of these materials. The atomic-resolution imaging capabilities of AFM can be applied to polycrystalline samples by means of pressing powders with a grain size as small as 50 micrometers. These results illustrate that the AFM is a promising tool for material science and the study of biomineralization.
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In-situ, time-lapse study of extracellular polymeric substance discharge in Streptococcus mutans biofilm.
PubMed
Liu, Bernard Haochih; Yu, Li-Chieh
2017-02-01
Streptococcus mutans is one of the main pathogens that cause tooth decay. By metabolizing carbohydrates, S. mutans emits extracellular polymeric substance (EPS) that adheres to the tooth surface and forms layers of biofilm. Periodontal disease occurs due to the low pH environment created by S. mutans biofilm, and such an acidic environment gradually erodes tooth enamel. Since the existence of EPS is essential in the formation of biofilm, the in-situ investigation of its generation and distribution in real time is the key to the control and suppression of S. mutans biofilm. Prior studies of the biofilm formation process by fluorescence microscope, scanning electron microscope, or spectroscope have roughly divided the mechanism into three stages: (1) initial attachment; (2) microcolonies; and (3) maturation. However, these analytical methods are incapable to observe real-time changes in different locations of the extracellular matrix, and to analyze mechanical properties for single bacteria in micro and nanoscale. Since atomic force microscopy (AFM) operates by precise control of tip-sample interaction forces in liquid and in air, living microorganisms can be analyzed under near-physiological conditions. Thus, analytical techniques based on AFM constitute powerful tools for the study of biological samples, both qualitatively and quantitatively. In this study, we used AFM to quantitatively track the changes of multiple nanomechanical properties of S. mutans, including dissipation energy, adhesion force, deformation, and elastic modulus at different metabolic stages. The data revealed that the bacterial extracellular matrix has a gradient distribution in stickiness, in which different stickiness indicates the variation of EPS compositions, freshness, and metabolic stages. In-situ, time-lapse AFM images showed the local generation and distribution of EPS at different times, in which the highest adhesion distributed along sides of the S. mutans cells. Through time-lapse analysis, we concluded that each contour layer is associated with a dynamic process of cell growth and nutrient consumption, and S. mutans is capable of controlling the priority of EPS secretion at specific locations. The live bacteria exhibited cyclic metabolic activities in the period of 23-34min at the maturation stage of biofilm formation. In addition, the discharge of EPS is responsive to the shear stress caused by the topographical change of biofilm to provide stronger mechanical support in the formation of 3D networked biofilm. Copyright © 2016 Elsevier B.V. All rights reserved.
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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
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Electrical characterization of FIB processed metal layers for reliable conductive-AFM on ZnO microstructures
NASA Astrophysics Data System (ADS)
Pea, M.; Maiolo, L.; Giovine, E.; Rinaldi, A.; Araneo, R.; Notargiacomo, A.
2016-05-01
We report on the conductive-atomic force microscopy (C-AFM) study of metallic layers in order to find the most suitable configuration for electrical characterization of individual ZnO micro-pillars fabricated by focused ion beam (FIB). The electrical resistance between the probe tip and both as deposited and FIB processed metal layers (namely, Cr, Ti, Au and Al) has been investigated. Both chromium and titanium evidenced a non homogenous and non ohmic behaviour, non negligible scanning probe induced anodic oxidation associated to electrical measurements, and after FIB milling they exhibited significantly higher tip-sample resistance. Aluminium had generally a more apparent non conductive behaviour. Conversely, gold films showed very good tip-sample conduction properties being less sensitive to FIB processing than the other investigated metals. We found that a reliable C-AFM electrical characterization of ZnO microstructures obtained by FIB machining is feasible by using a combination of metal films as top contact layer. An Au/Ti bilayer on top of ZnO was capable to sustain the FIB fabrication process and to form a suitable ohmic contact to the semiconductor, allowing for reliable C-AFM measurement. To validate the consistency of this approach, we measured the resistance of ZnO micropillars finding a linear dependence on the pillar height, as expected for an ohmic conductor, and evaluated the resistivity of the material. This procedure has the potential to be downscaled to nanometer size structures by a proper choice of metal films type and thickness.
