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Sample records for afm nanoindentation experiments

  1. Development of a novel nanoindentation technique by utilizing a dual-probe AFM system

    PubMed Central

    Sahin, Ferat; Yablon, Dalia

    2015-01-01

    Summary A novel instrumentation approach to nanoindentation is described that exhibits improved resolution and depth sensing. The approach is based on a multi-probe scanning probe microscopy (SPM) tool that utilizes tuning-fork based probes for both indentation and depth sensing. Unlike nanoindentation experiments performed with conventional AFM systems using beam-bounce technology, this technique incorporates a second probe system with an ultra-high resolution for depth sensing. The additional second probe measures only the vertical movement of the straight indenter attached to a tuning-fork probe with a high spring constant and it can also be used for AFM scanning to obtain an accurate profiling. Nanoindentation results are demonstrated on silicon, fused silica, and Corning Eagle Glass. The results show that this new approach is viable in terms of accurately characterizing mechanical properties of materials through nanoindentation with high accuracy, and it opens doors to many other exciting applications in the field of nanomechanical characterization. PMID:26665072

  2. Size effect study of thin film hardness using AFM nano-indentation

    NASA Astrophysics Data System (ADS)

    Xu, Linyan; Qian, Shuangbei; Li, Juan; Liu, Congcong; Guo, Shijia; Huang, Di; Wu, Sen; Hu, Xiaodong

    2015-10-01

    With nano-level spatial and force resolution, atomic force microscope (AFM) becomes an indispensable nanoindentation measurement instrument for thin films and soft films. To do the research of size effect of the hardness property of thin films, indentation experiments have been done on a gold film with 200 nm thickness and a silicon nitride film with 110 nm thickness. It is possible to change the maximum load forces to get discrete residual depths on the film samples. The contact depths of the gold film are 15.91 nm and 26.67 nm respectively, while the contact depths of the silicon nitride film are 7.82 nm and 10.25 nm respectively. A group of nanoindentation force curves are recorded for the transformation into force-depth curves. Subsequently, a 3D image of the residual indentation can be obtained by in-situ scanning immediately after nanoindentation. The topography data is imported into a Matlab program to estimate the contact area of the indentation. For the gold film, the hardness parameters of 3.31 GPa and 2.57 GPa are calculated under the above two contact depths. And for silicon nitride film, the corresponding results are 6.51GPa and 3.58 GPa. The experimental results illustrate a strong size effect for thin film hardness. The correction of the residual indentation image of the gold film is also done as an initial study. Blind tip reconstruction (BTR) algorithm is introduced to calibrate the tip shape, and more reliable hardness values of 1.15 GPa and 0.94 GPa are estimated.

  3. Mechanical properties of in situ demineralised human enamel measured by AFM nanoindentation

    NASA Astrophysics Data System (ADS)

    Finke, Manuela; Hughes, Julie A.; Parker, David M.; Jandt, Klaus D.

    2001-10-01

    Diet-induced demineralisation is one of the key factors in surface changes of tooth enamel, with soft drinks being a significant etiological agent. The first step in this dissolution process is characterised by a change in the mechanical properties of the enamel and a roughening of the surface. The objective of this pilot study was to measure early stages of in situ induced hardness changes of polished human enamel surfaces with high accuracy using a nanoindenter attached to an atomic force microscope (AFM). Human unerupted third molars were cleaned, sterilised with sodium hypochlorite, sectioned and embedded in epoxy resin. The outer enamel surface was polished and the samples partly covered with a tape, allowing a 2-mm-wide zone to be exposed to the oral environment. Samples were fitted in an intra-oral appliance, which was worn from 9 a.m. to 5 p.m. for one day. During this time the volunteer sipped 250 ml of a drink over 10 min periods at 9.00, 11.00, 13.00 and 15.00 h. Three different drinks, mineral water, orange juice and the prototype of a blackcurrant drink with low demineralisation potential were used in this study. At the end of the experiment the samples were detached from the appliance, the tape removed and the surfaces chemically cleaned. The surface hardness and reduced Young's modulus of the exposed and unexposed areas of each sample were determined. In addition, high resolution topographical AFM images were obtained. This study shows that by determining the hardness and reduced Young's modulus, the difference in demineralisation caused by the drinks can be detected and quantified before statistically significant changes in surface topography could be observed with the AFM. The maximum decrease in surface hardness and Young's modulus occurred in the samples exposed to orange juice, followed by those exposed to the blackcurrant drink, while exposure to water led to the same values as unexposed areas. A one-way ANOVA showed a statistically significant

  4. Nanomechanical characterization of nanostructured bainitic steel: Peak Force Microscopy and Nanoindentation with AFM

    NASA Astrophysics Data System (ADS)

    Morales-Rivas, Lucia; González-Orive, Alejandro; Garcia-Mateo, Carlos; Hernández-Creus, Alberto; Caballero, Francisca G.; Vázquez, Luis

    2015-11-01

    The full understanding of the deformation mechanisms in nanostructured bainite requires the local characterization of its mechanical properties, which are expected to change from one phase, bainitic ferrite, to another, austenite. This study becomes a challenging process due to the bainitic nanostructured nature and high Young’s modulus. In this work, we have carried out such study by means of the combination of AFM-based techniques, such as nanoindentation and Peak Force Quantitative Nanomechanical Mapping (PF-QNM) measurements. We have addressed critically the limits and advantages of these techniques and been able to measure some elastoplastic parameters of both phases. Specifically, we have analyzed by PF-QNM two nanostructured bainitic steels, with a finer and a coarser structure, and found that both phases have a similar Young’s modulus.

  5. Nanomechanical characterization of nanostructured bainitic steel: Peak Force Microscopy and Nanoindentation with AFM

    PubMed Central

    Morales-Rivas, Lucia; González-Orive, Alejandro; Garcia-Mateo, Carlos; Hernández-Creus, Alberto; Caballero, Francisca G.; Vázquez, Luis

    2015-01-01

    The full understanding of the deformation mechanisms in nanostructured bainite requires the local characterization of its mechanical properties, which are expected to change from one phase, bainitic ferrite, to another, austenite. This study becomes a challenging process due to the bainitic nanostructured nature and high Young’s modulus. In this work, we have carried out such study by means of the combination of AFM-based techniques, such as nanoindentation and Peak Force Quantitative Nanomechanical Mapping (PF-QNM) measurements. We have addressed critically the limits and advantages of these techniques and been able to measure some elastoplastic parameters of both phases. Specifically, we have analyzed by PF-QNM two nanostructured bainitic steels, with a finer and a coarser structure, and found that both phases have a similar Young’s modulus. PMID:26602631

  6. Nanomechanical characterization of nanostructured bainitic steel: Peak Force Microscopy and Nanoindentation with AFM.

    PubMed

    Morales-Rivas, Lucia; González-Orive, Alejandro; Garcia-Mateo, Carlos; Hernández-Creus, Alberto; Caballero, Francisca G; Vázquez, Luis

    2015-01-01

    The full understanding of the deformation mechanisms in nanostructured bainite requires the local characterization of its mechanical properties, which are expected to change from one phase, bainitic ferrite, to another, austenite. This study becomes a challenging process due to the bainitic nanostructured nature and high Young's modulus. In this work, we have carried out such study by means of the combination of AFM-based techniques, such as nanoindentation and Peak Force Quantitative Nanomechanical Mapping (PF-QNM) measurements. We have addressed critically the limits and advantages of these techniques and been able to measure some elastoplastic parameters of both phases. Specifically, we have analyzed by PF-QNM two nanostructured bainitic steels, with a finer and a coarser structure, and found that both phases have a similar Young's modulus. PMID:26602631

  7. Biomechanical properties of murine meniscus surface via AFM-based nanoindentation.

    PubMed

    Li, Qing; Doyran, Basak; Gamer, Laura W; Lu, X Lucas; Qin, Ling; Ortiz, Christine; Grodzinsky, Alan J; Rosen, Vicki; Han, Lin

    2015-06-01

    This study aimed to quantify the biomechanical properties of murine meniscus surface. Atomic force microscopy (AFM)-based nanoindentation was performed on the central region, proximal side of menisci from 6- to 24-week old male C57BL/6 mice using microspherical tips (Rtip≈5µm) in PBS. A unique, linear correlation between indentation depth, D, and response force, F, was found on menisci from all age groups. This non-Hertzian behavior is likely due to the dominance of tensile resistance by the collagen fibril bundles on meniscus surface that are mostly aligned along the circumferential direction. The indentation resistance was calculated as both the effective modulus, Eind, via the isotropic Hertz model, and the effective stiffness, Sind = dF/dD. Values of Sind and Eind were found to depend on indentation rate, suggesting the existence of poro-viscoelasticity. These values do not significantly vary with anatomical sites, lateral versus medial compartments, or mouse age. In addition, Eind of meniscus surface (e.g., 6.1±0.8MPa for 12 weeks of age, mean±SEM, n=13) was found to be significantly higher than those of meniscus surfaces in other species, and of murine articular cartilage surface (1.4±0.1MPa, n=6). In summary, these results provided the first direct mechanical knowledge of murine knee meniscus tissues. We expect this understanding to serve as a mechanics-based benchmark for further probing the developmental biology and osteoarthritis symptoms of meniscus in various murine models. PMID:25817332

  8. Biomechanical Properties of Murine Meniscus Surface via AFM-based Nanoindentation

    PubMed Central

    Li, Qing; Doyran, Basak; Gamer, Laura W.; Lu, X. Lucas; Qin, Ling; Ortiz, Christine; Grodzinsky, Alan J.; Rosen, Vicki; Han, Lin

    2015-01-01

    This study aimed to quantify the biomechanical properties of murine meniscus surface. Atomic force microscopy (AFM)-based nanoindentation was performed on the central region, proximal side of menisci from 6- to 24-week old male C57BL/6 mice using microspherical tips (Rtip ≈ 5 μm) in PBS. A unique, linear correlation between indentation depth, D, and response force, F, was found on menisci from all age groups. This non-Hertzian behavior is likely due to the dominance of tensile resistance by the collagen fibril bundles on meniscus surface that are mostly aligned along the circumferential direction observed on 12-week old menisci. The indentation resistance was calculated as both the effective stiffness, Sind = dF/dD, and the effective modulus, Eind, via the isotropic Hertz model. Values of Sind and Eind were found to depend on indentation rate, suggesting the existence of poro-viscoelasticity. These values do not significantly vary with anatomical sites, lateral versus medial compartments, or mouse age. In addition, Eind of meniscus surface (e.g., 6.1 ± 0.8 MPa for 12 weeks of age, mean ± SEM, n = 13) was found to be significantly higher than those of meniscus surfaces in other species, and of murine articular cartilage surface (1.4 ± 0.1 MPa, n = 6). In summary, these results provided the first direct mechanical knowledge of murine knee meniscus tissues. We expect this understanding to serve as a mechanics-based benchmark for further probing the developmental biology and osteoarthritis symptoms of meniscus in various murine models. PMID:25817332

  9. Nano-indentation experiments: from viruses to cells

    NASA Astrophysics Data System (ADS)

    Roos, Wouter; Vorselen, Daan; van Loon, Jack; Wuite, Gijs

    2012-02-01

    Over the last years AFM imaging and nanoindentation have become an indispensable tool for biophysical studies in liquid at the nano- and micro-scale. We look at both these length scales, at the cellular as well as the sub-cellular level. In particular, we perform combined imaging and force spectroscopy experiments on viral particles to elucidate their structure and mechanics [1]. These studies revealed that Noro virus has found an intriguing way to increase its mechanical strength. These self-assembling, natural nanoparticles incorporate a pre-stress during assembly, consolidating the structure of its protein shell that protects the genome [2]. Next, we studied whole cells. Mechanical loading is increasingly recognized as an important stimulus to cells. Establishing the local viscoelastic properties within a cell is vital to the understanding of the underlying mechanisms of cytoskeletal changes in response to these stimuli. We study the mechanical response of mammalian bone forming (osteoblast-like) cells on a substrate of physiological stiffness using spherical, μm-sized probes and we compare these results to the properties of bone forming cells originating from fish (teleosts).[4pt] [1] Roos et al. Nature Physics (2010), 6:733[0pt] [2] Baclayon et al. Nano Letters (2011), 11:4865

  10. Dislocation dynamical approach to force fluctuations in nanoindentation experiments

    NASA Astrophysics Data System (ADS)

    Ananthakrishna, G.; Katti, Rohit; K, Srikanth

    2014-09-01

    We develop an approach that combines the power of nonlinear dynamics with the evolution equations for the mobile and immobile dislocation densities and force to explain force fluctuations in nanoindentation experiments. The model includes nucleation, multiplication, and propagation thresholds for mobile dislocations, and other well known dislocation transformation mechanisms. The model predicts all the generic features of nanoindentation such as the Hertzian elastic branch followed by several force drops of decreasing magnitudes, and residual plasticity after unloading. The stress corresponding to the elastic force maximum is close to the yield stress of an ideal solid. The predicted values for all the quantities are close to those reported by experiments. Our model allows us to address the indentation-size effect including the ambiguity in defining the hardness in the force drop dominated regime. At large indentation depths, the hardness remains nearly constant with a marginal decreasing trend.

  11. Piezoelectric Nanoindentation

    SciTech Connect

    Rar, Andrei; Pharr, George Mathews; Oliver, Warren C.; Karapetian, Edgar; Kalinin, Sergei V

    2006-01-01

    Piezoelectric nanoindentation (PNI) has been developed to quantitatively address electromechanical coupling and pressure-induced dynamic phenomena in ferroelectric materials on the nanoscale. In PNI, an oscillating voltage is applied between the back side of the sample and the indenter tip, and the first harmonic of bias-induced surface displacement at the area of indenter contact is detected. PNI is implemented using a standard nanoindentation system equipped with a continuous stiffness measurement system. The piezoresponse of polycrystalline lead zirconate titanate (PZT) and BaTiO{sub 3} piezoceramics was studied during a standard nanoindentation experiment. For PZT, the response was found to be load independent, in agreement with theoretical predictions. In polycrystalline barium titanate, a load dependence of the piezoresponse was observed. The potential of piezoelectric nanoindentation for studies of phase transitions and local structure-property relations in piezoelectric materials is discussed.

  12. Nanoindentation of soft films on hard substrates: Experiments and finite element simulations

    SciTech Connect

    Pharr, G.M.; Tsui, T.Y.; Bolshakov, A.; Hay, J.C.

    1997-12-31

    Experiments and finite element simulations have been performed to examine error measurement of hardness and elastic modulus caused by pile-up when soft films deposited on hard substrates are tested by nanoindentation methods. Pile-up is exacerbated in soft-film/hard-substrate systems by the constraint imposed on plastic deformation in the film by the relatively non-deformable substrate. To experimentally examine pile-up effects, soft aluminum films with thicknesses of 240, 650, and 1700 nm were deposited on hard soda-lime glass substrates and tested by nanoindentation techniques. This system is attractive because the elastic modulus of the film and the substrate are approximately the same, but the substrate is harder than the film by a factor of about ten. Consequently, substrate influences on the indentation load-displacement behavior are manifested primarily by differences in the plastic flow characteristics alone. The elastic modulus of the film/substrate system, as measured by nanoindentation techniques, exhibits an increase with indenter penetration depth which peaks at a value approximately 30% greater than the true film modulus at a penetration depth close to the film thickness. Finite element simulation shows that this unusual behavior is caused by substrate-induced enhancement of pile-up. Finite element simulation also shows that the amount of pile-up increases with increasing penetration depth, and that the pile-up geometry depends on the work-hardening characteristics of the film. Because of these effects, nanoindentation techniques overestimate the true film hardness and elastic modulus by as much as 68% and 35%, respectively, depending on the work-hardening behavior of the film and the indenter penetration depth. The largest errors occur in non-work-hardening materials at penetration depths close to the film thickness, for which substrate-induced enhancement of pile-up is greatest.

  13. Liquid contact resonance AFM: analytical models, experiments, and limitations

    NASA Astrophysics Data System (ADS)

    Parlak, Zehra; Tu, Qing; Zauscher, Stefan

    2014-11-01

    Contact resonance AFM (CR-AFM) is a scanning probe microscopy technique that utilizes the contact resonances of the AFM cantilever for concurrent imaging of topography and surface stiffness. The technique has not been used in liquid until recently due to analytical and experimental difficulties, associated with viscous damping of cantilever vibrations and fluid loading effects. To address these difficulties, (i) an analytical approach for contact resonances in liquid is developed, and (ii) direct excitation of the contact resonances is demonstrated by actuating the cantilever directly in a magnetic field. By implementing the analytical approach and the direct actuation through magnetic particles, quantitative stiffness imaging on surfaces with a wide range of stiffness can be achieved in liquid with soft cantilevers and low contact forces.

  14. Nanoindentation experiments for single-layer rectangular graphene films: a molecular dynamics study

    PubMed Central

    2014-01-01

    A molecular dynamics study on nanoindentation experiments is carried out for some single-layer rectangular graphene films with four edges clamped. Typical load–displacement curves are obtained, and the effects of various factors including indenter radii, loading speeds, and aspect ratios of the graphene film on the simulation results are discussed. A formula describing the relationship between the load and indentation depth is obtained according to the molecular dynamics simulation results. Young’s modulus and the strength of the single-layer graphene film are measured as about 1.0 TPa and 200 GPa, respectively. It is found that the graphene film ruptured in the central point at a critical indentation depth. The deformation mechanisms and dislocation activities are discussed in detail during the loading-unloading-reloading process. It is observed from the simulation results that once the loading speed is larger than the critical loading speed, the maximum force exerted on the graphene film increases and the critical indentation depth decreases with the increase of the loading speed. PMID:24447765

  15. Simulation of nanoindentation experiment on RF magnetron sputtered nanocolumnar V2O5 film using finite element method

    NASA Astrophysics Data System (ADS)

    Porwal, Deeksha; Gupta, A. K.; Pillai, Anju M.; Sharma, Anand Kumar; Mukhopadhyay, Anoop Kumar; Khan, Kallol; Dey, Arjun

    2016-07-01

    The present work reports the nanomechanical behavior of a pulsed radio frequency (RF) magnetron sputtered vanadium pentoxide (V2O5) film deposited on silicon (Si) substrate using a combination of nanoindentation experiments and a finite element model (FEM). Deposited V2O5 film is characterized by x-ray diffraction (XRD), nanoprofilometry, field emission scanning electron microscopy (FESEM), nanoindentation and FEM. The phase pure 6.16 μm V2O5 film shows a nanocolumnar structure. The film exhibits nanohardness (H) of 0.16 ± 0.013 GPa and Young’s modulus (E) of about 12.05 ± 1.41 GPa. The FEM reproduces experimentally obtained load versus depth (P–h) plot and subsequently give yield stress and strain hardening component data of V2O5 film on Si substrate. Stress–strain behavior and von-Mises stress distribution of the V2O5 film with Si substrate system are also simulated. The FE model confirms the local maximum equivalent stress active underneath the nanoindenters to be nearly twice as high as the yield stress and thereby explains the plastic deformation observed in the V2O5 film.

  16. Strain-rate stiffening of cortical bone: observations and implications from nanoindentation experiments

    NASA Astrophysics Data System (ADS)

    Maruyama, Noriko; Shibata, Yo; Wurihan, Affb; Swain, Michael V.; Kataoka, Yu; Takiguchi, Yuichi; Yamada, Atsushi; Maki, Koutaro; Miyazaki, Takashi

    2014-11-01

    While bone mineralization is considered to be responsible for its stiffness, bone durability partially associated with the time-dependent viscoelasticity of matrix proteins is still poorly elucidated. Here we demonstrate a novel mechanism of highly mineralized bone durability almost independent of inherent viscoelastic behaviour along with a protocol for measuring the mechanical properties of mineralized tissues. Strain-rate nanoindentation tests showed substantial stiffening of the highly mineralized calvarial bone, whereas large creep or stress relaxation was observed during constant load or displacement tests, respectively. Based on the lower viscoelasticity of the highly mineralized structure, such large time-dependent response appears to be associated with nanoscale dimensional recovery, rather than viscoelastic behaviour, implying the inverse namely strain-rate dependent dilatant behaviour. This dilatant expansion increased the indenter penetration resistance into the surface, enhancing instantaneous stiffness. The associated stiffening and higher effective elastic modulus were highly strain-rate dependent and more readily observed in more highly mineralized tissues such as the calvarial bone. Such strain-rate stiffening and consequent dimensional recovery may be vital responses of bone tissues against excessive deformation to maintain tissue integrity.While bone mineralization is considered to be responsible for its stiffness, bone durability partially associated with the time-dependent viscoelasticity of matrix proteins is still poorly elucidated. Here we demonstrate a novel mechanism of highly mineralized bone durability almost independent of inherent viscoelastic behaviour along with a protocol for measuring the mechanical properties of mineralized tissues. Strain-rate nanoindentation tests showed substantial stiffening of the highly mineralized calvarial bone, whereas large creep or stress relaxation was observed during constant load or displacement

  17. An innovative method and experiment for fabricating bulgy shape nanochannel using AFM

    NASA Astrophysics Data System (ADS)

    Lin, Zone-Ching; Jheng, Hao-Yuan; Ding, Hao-Yang

    2015-08-01

    The paper proposes using atomic force microscopy (AFM) and the concept of specific down force energy (SDFE) to establish an innovative offset cycle cutting method for fabricating a bulgy shape nanochannel on a single-crystal silicon substrate. In the offset cycle cutting method, cutting is performed at a constant down force in all cutting passes. After the first cutting pass, the AFM probe is offset rightward for the second pass and subsequently offset leftward to the middle (i.e., between the positions of the first two cutting passes) for the third cutting pass. Applying a step-by-step method to modify the offset distance and approach the defined SDFE value, this study determined the depth of the middle cutting pass and smaller values of upward bulginess and downward indentation at the bottom of the nanochannel. The nanochannel width can be increased by increasing the number of offset cycle cutting passes. In addition, by applying the proposed method, this study involved a simulation and experiment concerning the cutting path plan of bulgy shape nanochannels. Furthermore, using a small down force along the burr path is proposed for reducing burr height. The results of the simulation and experiment were compared to verify the feasibility of the method.

  18. Hydrodynamics in nanoscale confinement: SFA and colloid probe AFM liquid drainage experiments

    NASA Astrophysics Data System (ADS)

    Krasowska, M.; Popescu, M. N.; Ralston, J.

    2012-12-01

    Flow and drainage of very thin liquid films play an important role in mineral recovery, drop coalescence and emulsion stability, as well as lubrication of micromechanical devices. Studies of liquid flow under strong confinement (i.e., film thickness below a few hundred of nanometers and down to a few nanometers) can reveal the limits of applicability of a classical hydrodynamics description, but are very challenging. The Surface Force Apparatus (SFA) technique has enabled studies of drainage at nanoscale separation between atomically smooth mica sheets. The development of the colloid probe Atomic Force Microscope (AFM) as an alternative technique has allowed a significantly wider variety of confining solid surfaces to be studied. Both the SFA and the colloid probe AFM have been adapted to permit the surfaces confining the film to be soft, e.g., the surface of a drop or bubble, and therefore deformable. We present a succinct review of the experimental and theoretical modeling challenges for such studies and critically discuss the outcomes of recent experiments.

  19. Nanopuller-open data acquisition platform for AFM force spectroscopy experiments.

    PubMed

    Pawlak, Konrad; Strzelecki, Janusz

    2016-05-01

    Atomic Force Microscope (AFM) is a widely used tool in force spectroscopy studies. Presently, this instrument is accessible from numerous vendors, albeit commercial solutions are expensive and almost always hardware and software closed. Approaches for open setups were published, as with modern low cost and readily available piezoelectric actuators, data acquisition interfaces and optoelectronic components building such force spectroscopy AFM is relatively easy. However, suitable software to control such laboratory made instrument was not released. Developing it in the lab requires significant time and effort. Our Nanopuller software described in this paper is intended to eliminate this obstacle. With only minimum adjustments this program can be used to control and acquire data with any suitable National Instruments universal digital/analog interface and piezoelectric actuator analog controller, giving significant freedom and flexibility in designing force spectroscopy experiment. Since the full code, written in a graphical LabVIEW environment is available, our Nanopuller can be easily customized. In this paper we describe the program and test its performance in controlling different setups. Successful and accurate force curve acquisition for standard samples (single molecules of I27O reference titin polyprotein and DNA as well as red blood cells) is shown. PMID:26994468

  20. A study of the micro- and nanoscale deformation behavior of individual austenitic dendrites in a FeCrMoVC cast alloy using micro- and nanoindentation experiments

    NASA Astrophysics Data System (ADS)

    Zeisig, J.; Hufenbach, J.; Wendrock, H.; Gemming, T.; Eckert, J.; Kühn, U.

    2016-04-01

    Micro- and nanoindentation experiments were conducted to investigate the deformation mechanisms in a Fe79.4Cr13Mo5V1C1.6 (wt. %) cast alloy. This alloy consists of an as cast microstructure mainly composed of austenite, martensite, and a complex carbide network. During microhardness testing, metastable austenite transforms partially into martensite confirmed by electron backscatter diffraction. For nanoindentation tests, two different indenter geometries were applied (Berkovich and cube corner type). Load-displacement curves of nanoindentation in austenitic dendrites depicted pop-ins after transition into plastic deformation for both nanoindenters. Characterizations of the region beneath a nanoindent by transmission electron microscopy revealed a martensitic transformation as an activated deformation mechanism and suggest a correlation with the pop-in phenomena of the load-displacement curves. Furthermore, due to an inhomogeneous chemical composition within the austenitic dendrites, more stabilized regions deform by mechanical twinning. This additional deformation mechanism was only observed for the cube corner indenter with the sharper geometry since higher shear stresses are induced beneath the contact area.

  1. Understanding pop-ins in spherical nanoindentation

    SciTech Connect

    Pathak, Siddhartha; Riesterer, Jessica L.; Kalidindi, Surya R.; Michler, Johann

    2014-10-24

    In this study, pop-ins, or sudden displacement-bursts at constant load in a nanoindentation test, are typically attributed to the difficulty of setting up potent dislocation sources in the very small indentation zones in these experiments. Such displacement (and strain) bursts would intuitively indicate a sharp drop in stress during the pop-in event itself. However, spherical indentation stress-strain curves routinely exhibit a high and stable indentation stress value during the pop-in, and the indentation stresses decrease only after a further finite amount of additional indentation displacement has been applied. In order to understand this discrepancy, we utilize a combination of interrupted spherical indentation tests along with depth profiling of the residual indentation surfaces using in-situ atomic force microscopy (AFM) to study pop-ins. The AFM surface profile maps show that there is an asymmetric profile change over a limited region around the indentation contact area for a single pop-in; the asymmetry disappears upon further loading beyond the pop-in. A plausible sequence of physical processes (related to metal plasticity) occurring underneath the indenter during and immediately after the occurrence of the pop-in is proposed to explain these observations.

  2. Understanding pop-ins in spherical nanoindentation

    DOE PAGESBeta

    Pathak, Siddhartha; Riesterer, Jessica L.; Kalidindi, Surya R.; Michler, Johann

    2014-10-24

    In this study, pop-ins, or sudden displacement-bursts at constant load in a nanoindentation test, are typically attributed to the difficulty of setting up potent dislocation sources in the very small indentation zones in these experiments. Such displacement (and strain) bursts would intuitively indicate a sharp drop in stress during the pop-in event itself. However, spherical indentation stress-strain curves routinely exhibit a high and stable indentation stress value during the pop-in, and the indentation stresses decrease only after a further finite amount of additional indentation displacement has been applied. In order to understand this discrepancy, we utilize a combination of interruptedmore » spherical indentation tests along with depth profiling of the residual indentation surfaces using in-situ atomic force microscopy (AFM) to study pop-ins. The AFM surface profile maps show that there is an asymmetric profile change over a limited region around the indentation contact area for a single pop-in; the asymmetry disappears upon further loading beyond the pop-in. A plausible sequence of physical processes (related to metal plasticity) occurring underneath the indenter during and immediately after the occurrence of the pop-in is proposed to explain these observations.« less

  3. Understanding pop-ins in spherical nanoindentation

    SciTech Connect

    Pathak, Siddhartha E-mail: siddharthapathak@gmail.com; Riesterer, Jessica L.; Michler, Johann; Kalidindi, Surya R.

    2014-10-20

    Pop-ins, or sudden displacement-bursts at constant load in a nanoindentation test, are typically attributed to the difficulty of setting up potent dislocation sources in the very small indentation zones in these experiments. Such displacement (and strain) bursts would intuitively indicate a sharp drop in stress during the pop-in event itself. However, spherical indentation stress-strain curves routinely exhibit a high and stable indentation stress value during the pop-in, and the indentation stresses decrease only after a further finite amount of additional indentation displacement has been applied. In order to understand this discrepancy, we utilize a combination of interrupted spherical indentation tests along with depth profiling of the residual indentation surfaces using in-situ atomic force microscopy (AFM) to study pop-ins. The AFM surface profile maps show that there is an asymmetric profile change over a limited region around the indentation contact area for a single pop-in; the asymmetry disappears upon further loading beyond the pop-in. A plausible sequence of physical processes (related to metal plasticity) occurring underneath the indenter during and immediately after the occurrence of the pop-in is proposed to explain these observations.

  4. Assembly of live micro-organisms on microstructured PDMS stamps by convective/capillary deposition for AFM bio-experiments

    NASA Astrophysics Data System (ADS)

    Dague, E.; Jauvert, E.; Laplatine, L.; Viallet, B.; Thibault, C.; Ressier, L.

    2011-09-01

    Immobilization of live micro-organisms on solid substrates is an important prerequisite for atomic force microscopy (AFM) bio-experiments. The method employed must immobilize the cells firmly enough to enable them to withstand the lateral friction forces exerted by the tip during scanning but without denaturing the cell interface. In this work, a generic method for the assembly of living cells on specific areas of substrates is proposed. It consists in assembling the living cells within the patterns of microstructured, functionalized poly-dimethylsiloxane (PDMS) stamps using convective/capillary deposition. This versatile approach is validated by applying it to two systems of foremost importance in biotechnology and medicine: Saccharomyces cerevisiae yeasts and Aspergillus fumigatus fungal spores. We show that this method allows multiplexing AFM nanomechanical measurements by force spectroscopy on S. cerevisiae yeasts and high-resolution AFM imaging of germinated Aspergillus conidia in buffer medium. These two examples clearly demonstrate the immense potential of micro-organism assembly on functionalized, microstructured PDMS stamps by convective/capillary deposition for performing rigorous AFM bio-experiments on living cells.

  5. Dynamic force microscopy simulator (dForce): A tool for planning and understanding tapping and bimodal AFM experiments.

    PubMed

    Guzman, Horacio V; Garcia, Pablo D; Garcia, Ricardo

    2015-01-01

    We present a simulation environment, dForce, which can be used for a better understanding of dynamic force microscopy experiments. The simulator presents the cantilever-tip dynamics for two dynamic AFM methods, tapping mode AFM and bimodal AFM. It can be applied for a wide variety of experimental situations in air or liquid. The code provides all the variables and parameters relevant in those modes, for example, the instantaneous deflection and tip-surface force, velocity, virial, dissipated energy, sample deformation and peak force as a function of time or distance. The simulator includes a variety of interactions and contact mechanics models to describe AFM experiments including: van der Waals, Hertz, DMT, JKR, bottom effect cone correction, linear viscoelastic forces or the standard linear solid viscoelastic model. We have compared two numerical integration methods to select the one that offers optimal accuracy and speed. The graphical user interface has been designed to facilitate the navigation of non-experts in simulations. Finally, the accuracy of dForce has been tested against numerical simulations performed during the last 18 years. PMID:25821676

  6. Dynamic force microscopy simulator (dForce): A tool for planning and understanding tapping and bimodal AFM experiments

    PubMed Central

    Guzman, Horacio V; Garcia, Pablo D

    2015-01-01

    Summary We present a simulation environment, dForce, which can be used for a better understanding of dynamic force microscopy experiments. The simulator presents the cantilever–tip dynamics for two dynamic AFM methods, tapping mode AFM and bimodal AFM. It can be applied for a wide variety of experimental situations in air or liquid. The code provides all the variables and parameters relevant in those modes, for example, the instantaneous deflection and tip–surface force, velocity, virial, dissipated energy, sample deformation and peak force as a function of time or distance. The simulator includes a variety of interactions and contact mechanics models to describe AFM experiments including: van der Waals, Hertz, DMT, JKR, bottom effect cone correction, linear viscoelastic forces or the standard linear solid viscoelastic model. We have compared two numerical integration methods to select the one that offers optimal accuracy and speed. The graphical user interface has been designed to facilitate the navigation of non-experts in simulations. Finally, the accuracy of dForce has been tested against numerical simulations performed during the last 18 years. PMID:25821676

  7. The use of nanoindentation for determining internal lengths and the constitutive response of monument materials: models and experiments

    NASA Astrophysics Data System (ADS)

    Konstantinidis, Avraam A.; Frantziskonis, George; Askes, Harm; Aifantis, Elias C.

    2016-04-01

    An alternative interpretation of nanoindentation experimental data and the associated phenomenon of indentation size effect (ISE) is proposed on the basis of a simple gradient elasticity equation, used to account for the development of elastic gradients generated by the geometry characterizing the indenter-specimen system. An application is considered for marble, i.e. a construction/restoration material.

  8. Effect of AFM probe geometry on visco-hyperelastic characterization of soft materials.

    PubMed

    Boccaccio, Antonio; Lamberti, Luciano; Papi, Massimiliano; De Spirito, Marco; Pappalettere, Carmine

    2015-08-14

    Atomic force microscopy (AFM) nanoindentation is very suited for nano- and microscale mechanical characterization of soft materials. Although the structural response of polymeric networks that form soft matter depends on viscous effects caused by the relative slippage of polymeric chains, the usual assumption made in the AFM-based characterization is that the specimen behaves as a purely elastic material and viscous forces are negligible. However, for each geometric configuration of the AFM tip, there will be a limit indentation rate above which viscous effects must be taken into account to correctly determine mechanical properties. A parametric finite element study conducted on 12 geometric configurations of a blunt cone AFM tip (overall, the study included about 200 finite element analyses) allowed us to determine the limit indentation rate for each configuration. The selected tip dimensions cover commercially available products and account for changes in tip geometry caused by serial measurements. Nanoindentation rates cover typical experimental conditions set in AFM bio-measurements on soft matter. Viscous effects appear to be more significant in the case of sharper tips. This implies that, if quantitative data on sample viscosity are not available, using a rounded indenter and carrying out experiments below the limit indentation rate will allow errors in the determination of mechanical properties to be minimized. PMID:26201503

  9. Nonlinear finite-element analysis of nanoindentation of viral capsids

    NASA Astrophysics Data System (ADS)

    Gibbons, Melissa M.; Klug, William S.

    2007-03-01

    Recent atomic force microscope (AFM) nanoindentation experiments measuring mechanical response of the protein shells of viruses have provided a quantitative description of their strength and elasticity. To better understand and interpret these measurements, and to elucidate the underlying mechanisms, this paper adopts a course-grained modeling approach within the framework of three-dimensional nonlinear continuum elasticity. Homogeneous, isotropic, elastic, thick-shell models are proposed for two capsids: the spherical cowpea chlorotic mottle virus (CCMV), and the ellipsocylindrical bacteriophage ϕ29 . As analyzed by the finite-element method, these models enable parametric characterization of the effects of AFM tip geometry, capsid dimensions, and capsid constitutive descriptions. The generally nonlinear force response of capsids to indentation is shown to be insensitive to constitutive particulars, and greatly influenced by geometric and kinematic details. Nonlinear stiffening and softening of the force response is dependent on the AFM tip dimensions and shell thickness. Fits of the models capture the roughly linear behavior observed in experimental measurements and result in estimates of Young’s moduli of ≈280-360MPa for CCMV and ≈4.5GPa for ϕ29 .

  10. Adsorption mechanisms for fatty acids on DLC and steel studied by AFM and tribological experiments

    NASA Astrophysics Data System (ADS)

    Simič, R.; Kalin, M.

    2013-10-01

    Fatty acids are known to affect the friction and wear of steel contacts via adsorption onto the surface, which is one of the fundamental boundary-lubrication mechanisms. The understanding of the lubrication mechanisms of polar molecules on diamond-like carbon (DLC) is, however, still insufficient. In this work we aimed to find out whether such molecules have a similar effect on DLC coatings as they do on steel. The adsorption of hexadecanoic acid in various concentrations (2-20 mmol/l) on DLC was studied under static conditions using an atomic force microscope (AFM). The amount of surface coverage of the adsorbed fatty-acid molecules was analysed. In addition, tribological tests were performed to correlate the wear and friction behaviours in tribological contacts with the adsorption of molecules on the surface under static conditions. A good correlation between the AFM results and the tribological behaviour was observed. We confirmed that fatty acids can adsorb onto the DLC surfaces and are, therefore, potential boundary-lubrication agents for DLC coatings. The adsorption of the fatty acid onto the DLC surfaces reduces the wear of the coatings, but it is less effective in reducing the friction. Tentative adsorption mechanisms that include an environmental species effect, a temperature effect and a tribochemical effect are proposed for DLC and steel surfaces based on our results and few potential mechanisms found in literature.

  11. Structural investigations on native collagen type I fibrils using AFM

    SciTech Connect

    Strasser, Stefan; Zink, Albert; Janko, Marek; Heckl, Wolfgang M.; Thalhammer, Stefan . E-mail: stefan.thalhammer@gsf.de

    2007-03-02

    This study was carried out to determine the elastic properties of single collagen type I fibrils with the use of atomic force microscopy (AFM). Native collagen fibrils were formed by self-assembly in vitro characterized with the AFM. To confirm the inner assembly of the collagen fibrils, the AFM was used as a microdissection tool. Native collagen type I fibrils were dissected and the inner core uncovered. To determine the elastic properties of collagen fibrils the tip of the AFM was used as a nanoindentor by recording force-displacement curves. Measurements were done on the outer shell and in the core of the fibril. The structural investigations revealed the banding of the shell also in the core of native collagen fibrils. Nanoindentation experiments showed the same Young's modulus on the shell as well as in the core of the investigated native collagen fibrils. In addition, the measurements indicate a higher adhesion in the core of the collagen fibrils compared to the shell.

  12. Nanoindentation of Carbon Nanostructures.

    PubMed

    Kumar, Dinesh; Singh, Karamjit; Verma, Veena; Bhatti, H S

    2016-06-01

    In the present research paper carbon nanostructures viz. single walled carbon nanotubes, multi-walled carbon nanotubes, single walled carbon nanohorns and graphene nanoplatelets have been synthesized by CVD technique, hydrothermal method, DC arc discharge method in liquid nitrogen and microwave technique respectively. After synthesis 5 mm thick pallets of given nanomaterial are prepared by making a paste in isopropyl alcohol and using polyvinylidene difluoride as a binder and then these pallets were used for nanoindentation measurements. Hardness, reduced modulus, stiffness, contact height and contact area have been measured using nanoindenter. PMID:27427726

  13. Modeling and simulation of the mechanical response from nanoindentation test of DNA-filled viral capsids.

    PubMed

    Ahadi, Aylin; Johansson, Dan; Evilevitch, Alex

    2013-03-01

    Viruses can be described as biological objects composed mainly of two parts: a stiff protein shell called a capsid, and a core inside the capsid containing the nucleic acid and liquid. In many double-stranded DNA bacterial viruses (aka phage), the volume ratio between the liquid and the encapsidated DNA is approximately 1:1. Due to the dominant DNA hydration force, water strongly mediates the interaction between the packaged DNA strands. Therefore, water that hydrates the DNA plays an important role in nanoindentation experiments of DNA-filled viral capsids. Nanoindentation measurements allow us to gain further insight into the nature of the hydration and electrostatic interactions between the DNA strands. With this motivation, a continuum-based numerical model for simulating the nanoindentation response of DNA-filled viral capsids is proposed here. The viral capsid is modeled as large- strain isotropic hyper-elastic material, whereas porous elasticity is adopted to capture the mechanical response of the filled viral capsid. The voids inside the viral capsid are assumed to be filled with liquid, which is modeled as a homogenous incompressible fluid. The motion of a fluid flowing through the porous medium upon capsid indentation is modeled using Darcy's law, describing the flow of fluid through a porous medium. The nanoindentation response is simulated using three-dimensional finite element analysis and the simulations are performed using the finite element code Abaqus. Force-indentation curves for empty, partially and completely DNA-filled capsids are directly compared to the experimental data for bacteriophage λ. Material parameters such as Young's modulus, shear modulus, and bulk modulus are determined by comparing computed force-indentation curves to the data from the atomic force microscopy (AFM) experiments. Predictions are made for pressure distribution inside the capsid, as well as the fluid volume ratio variation during the indentation test. PMID:23860868

  14. Influence of Hydroxyapatite Nano-particles on the Mechanical and Tribological Properties of Orthopedic Cement-Based Nano-composites Measured by Nano-indentation and Nano-scratch Experiments

    NASA Astrophysics Data System (ADS)

    Asgharzadeh Shirazi, H.; Ayatollahi, M. R.; Naimi-Jamal, M. R.

    2015-09-01

    The aim of this study was to examine the mechanical and tribological properties of a commercially available bone cement by incorporating nano-sized hydroxyapatite using nano-indentation and nano-scratch experiments. In order to achieve this goal, the nano-composite cement samples with different amounts of commercial nano-hydroxyapatite (HAc), as a bone compatible nano-filler, were prepared via vacuum mixing method. The results indicated that nano-indentation and nano-scratch experiments are acceptable methods for measuring the mechanical and tribological properties of orthopedic cement-based nano-composites. Moreover, it was found that the nano-composite of 10 wt.% HAc exhibits the optimum performance compared to the other nano-composite samples in terms of mechanical and tribological properties. These findings can play an important role in achieving the goal of clinical and biomechanical function optimization of bone cement, especially in the field of orthopedic surgery.

  15. Note: A method for minimizing oxide formation during elevated temperature nanoindentation

    SciTech Connect

    Cheng, I. C.; Hodge, A. M.; Garcia-Sanchez, E.

    2014-09-15

    A standardized method to protect metallic samples and minimize oxide formation during elevated-temperature nanoindentation was adapted to a commercial instrument. Nanoindentation was performed on Al (100), Cu (100), and W (100) single crystals submerged in vacuum oil at 200 °C, while the surface morphology and oxidation was carefully monitored using atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS). The results were compared to room temperature and 200 °C nanoindentation tests performed without oil, in order to evaluate the feasibility of using the oil as a protective medium. Extensive surface characterization demonstrated that this methodology is effective for nanoscale testing.

  16. Stability of Norwalk Virus Capsid Protein Interfaces Evaluated by in Silico Nanoindentation

    PubMed Central

    Boyd, Kevin J.; Bansal, Prakhar; Feng, Jun; May, Eric R.

    2015-01-01

    Norwalk virus causes severe gastroenteritis for which there is currently no specific anti-viral therapy. A stage of the infection process is uncoating of the protein capsid to expose the viral genome and allow for viral replication. A mechanical characterization of the Norwalk virus may provide important information relating to the mechanism of uncoating. The mechanical strength of the Norwalk virus has previously been investigated using atomic force microscopy (AFM) nanoindentation experiments. Those experiments cannot resolve specific molecular interactions, and therefore, we have employed a molecular modeling approach to gain insights into the potential uncoating mechanism of the Norwalk capsid. In this study, we perform simulated nanoindentation using a coarse-grained structure-based model, which provides an estimate of the spring constant in good agreement with the experimentally determined value. We further analyze the fracture mechanisms and determine weak interfaces in the capsid structure, which are potential sites to inhibit uncoating by stabilization of these weak interfaces. We conclude by identifying potential target sites at the junction of a weak protein–protein interface. PMID:26284238

  17. Interfacial diffusion aided deformation during nanoindentation

    NASA Astrophysics Data System (ADS)

    Samanta, Amit; E, Weinan

    2016-07-01

    Nanoindentation is commonly used to quantify the mechanical response of material surfaces. Despite its widespread use, a detailed understanding of the deformation mechanisms responsible for plasticity during these experiments has remained elusive. Nanoindentation measurements often show stress values close to a material's ideal strength which suggests that dislocation nucleation and subsequent dislocation activity dominates the deformation. However, low strain-rate exponents and small activation volumes have also been reported which indicates high temperature sensitivity of the deformation processes. Using an order parameter aided temperature accelerated sampling technique called adiabatic free energy dynamics [J. B. Abrams and M. E. Tuckerman, J. Phys. Chem. B, 112, 15742 (2008)], and molecular dynamics we have probed the diffusive mode of deformation during nanoindentation. Localized processes such as surface vacancy and ad-atom pair formation, vacancy diffusion are found to play an important role during indentation. Our analysis suggests a change in the dominant deformation mode from dislocation mediated plasticity to diffusional flow at high temperatures, slow indentation rates and small indenter tip radii.

  18. Nanoindentation on ion irradiated steels

    NASA Astrophysics Data System (ADS)

    Hosemann, P.; Vieh, C.; Greco, R. R.; Kabra, S.; Valdez, J. A.; Cappiello, M. J.; Maloy, S. A.

    2009-06-01

    Radiation induced mechanical property changes can cause major difficulties in designing systems operating in a radiation environment. Investigating these mechanical property changes in an irradiation environment is a costly and time consuming activity. Ion beam accelerator experiments have the advantage of allowing relatively fast and inexpensive materials irradiations without activating the sample but do in general not allow large beam penetration depth into the sample. In this study, the ferritic/martensitic steel HT-9 was processed and heat treated to produce one specimen with a large grained ferritic microstructure and further heat treated to form a second specimen with a fine tempered martensitic lath structure and exposed to an ion beam and tested after irradiation using nanoindentation to investigate the irradiation induced changes in mechanical properties. It is shown that the HT-9 in the ferritic heat treatment is more susceptible to irradiation hardening than HT-9 after the tempered martensitic heat treatment. Also at an irradiation temperature above 550 °C no detectable hardness increase due to irradiation was detected. The results are also compared to data from the literature gained from the fast flux test facility.

  19. Nanoindentation of Pseudomonas aeruginosa bacterial biofilm using atomic force microscopy

    NASA Astrophysics Data System (ADS)

    Baniasadi, Mahmoud; Xu, Zhe; Gandee, Leah; Du, Yingjie; Lu, Hongbing; Zimmern, Philippe; Minary-Jolandan, Majid

    2014-12-01

    Bacterial biofilms are a source of many chronic infections. Biofilms and their inherent resistance to antibiotics are attributable to a range of health issues including affecting prosthetic implants, hospital-acquired infections, and wound infection. Mechanical properties of biofilm, in particular, at micro- and nano-scales, are governed by microstructures and porosity of the biofilm, which in turn may contribute to their inherent antibiotic resistance. We utilize atomic force microscopy (AFM)-based nanoindentation and finite element simulation to investigate the nanoscale mechanical properties of Pseudomonas aeruginosa bacterial biofilm. This biofilm was derived from human samples and represents a medically relevant model.

  20. Nanoindentation of gold nanorods with an atomic force microscope

    NASA Astrophysics Data System (ADS)

    Reischl, B.; Kuronen, A.; Nordlund, K.

    2014-12-01

    The atomic force microscope (AFM) can be used to measure mechanical properties of nanoscale objects, which are too small to be studied using a conventional nanoindenter. The contact mechanics at such small scales, in proximity of free surfaces, deviate substantially from simple continuum models. We present results from atomistic computer simulations of the indentation of gold nanorods using a diamond AFM tip and give insight in the atomic scale processes, involving creation and migration of dislocations, leading to the plastic deformation of the sample under load, and explain the force-distance curves observed for different tip apex radii of curvature, as well as different crystallographic structure and orientation of the gold nanorod samples.

  1. Nanoindentation studies on silver nanoparticles

    NASA Astrophysics Data System (ADS)

    Saha, Dhriti Ranjan; Mandal, Amrita; Mitra, Sreemanta; Mada, Mykanth Reddy; Boughton, Philip; Bandyopadhyay, Sri; Chakravorty, Dipankar

    2013-06-01

    Nanodimensional metallic silver was grown by electrodeposion technique in a semi solid polymer matrix of polyacrylamide. The whole structure looks like dendronic. The average particle diameter of the as grown metallic silver is 13 nm. Nanoindentation study of these nanoparticles shows modulus and hardness value as 103.93 GPa and 3.12 GPa respectively.

  2. Nanoindentation of Chitosan Doped with Silver Nanoparticles

    NASA Astrophysics Data System (ADS)

    Palumbo, Matthew; Teklu, Alem; Kuthirummal, Narayanan; Levi-Polyachenko, Nicole; Department of Physics; Astronomy, College of Charleston Collaboration; Department of Plastic; Reconstructive Surgery, Wake Forest University Health Sciences Collaboration

    Imaging and spectroscopic analysis via nanoindentation was performed with the Nanosurf EasyScan2 AFM on the pure and silver doped chitosan samples allowing for a more localized determination of their stiffness, hardness, and reduced Young's modulus. The pure chitosan sample was tested to have a stiffness of 0.367 N/m, a hardness of 1.12 GPa, and a reduced Young's modulus of 30.5 MPa. The film with 5mg Ag nanoparticle per gram of chitosan was tested on the boundaries between the chitosan and Ag nanoparticles to show an increase in stiffness of about 4.6% at 0.384 N/m, an increase in hardness of about 5.4% at 1.18 GPa, and an increase in the reduced Young's modulus of about 5.0% at 3.2 MPa in comparison to the pure chitosan sample. On the other hand, upon increasing the doping to 10mg Ag nanoparticle per gram of chitosan showed a decrease in stiffness of about 6.3% at 0.344 N/m, a decrease in hardness of about 27.0% at 0.820 GPa, and a decrease in the reduced Young's modulus of about 6.0% at 28.7 MPa in comparison to the pure chitosan sample. Obviously, films doped with 5mg Ag nanoparicle per gram of chitosan provided the composites with improved mechanical strength compared to chitosan alone.

  3. Size Effects and Stochastic Behavior of Nanoindentation Pop In

    SciTech Connect

    Morris, James R; Bei, Hongbin; Pharr, George M; George, Easo P

    2011-01-01

    One reason for the much higher strengths of small volumes of materials compared to their bulk counterparts is the absence of defects in the probed volumes. The present work demonstrates that the defect density gives rise to a natural length scale to the mechanical behavior. Experimentally, a nanoindentation size effect is demonstrated in single-crystal Mo, showing behavior ranging from theoretical strength to near-bulk behavior with a well-defined yielding at much lower stresses. A statistical model captures the change in nanoindentation behavior, including the wide variability of an intermediate regime between the theoretical defect free limit and the bulk behavior where large numbers of defects are present. A predicted scaling behavior is verified by nanoindentation experiments, using indenter radii that vary by over an order of magnitude in size.

  4. Nanoindentation and nanoscratching of hard coating materials for magnetic disks

    SciTech Connect

    Tsui, T.Y.; Pharr, G.M.; Oliver, W.C.; Chung, Y.W.; Cutiongco, E.C.; Bhatia, C.S.; White, R.L.; Rhodes, R.L.; Gorbatkin, S.M.

    1994-12-31

    Nanoindentation and nanoscratching experiments have been performed to assess the mechanical and tribological behavior of three thin film materials with potential application as wear resistant coatings for magnetic disk storage: (1) hydrogenated-carbon (CHx); (2) nitrogenated-carbon (CNx); and (3) boron suboxide (BOx). The hardness and elastic modulus were measured using nanoindentation. Ultra-low load nanoscratching tests were performed to assess the relative scratch resistance of the films and measure their friction coefficients. The mechanical and tribological performance of the three materials are discussed and compared.

  5. Force spectroscopy 101: how to design, perform, and analyze an AFM-based single molecule force spectroscopy experiment.

    PubMed

    Noy, Aleksandr

    2011-10-01

    Single molecule force spectroscopy presents a deceptively simple approach to probing interaction between molecules and molecular assemblies on the nanoscale by measuring forces that it takes to pull the molecules apart. Yet, a more detailed analysis reveals a wealth of different behaviors and interesting physics. This article aims to explore basic physical concepts behind these experiments from a strictly practical point of using these data to extract meaningful information about the interactions. It also focuses on different loading regimes in these experiments, different kinetics that they cause, and different data interpretation that is required for measurements in those regimes. PMID:21862386

  6. Qplus AFM driven nanostencil.

    PubMed

    Grévin, B; Fakir, M; Hayton, J; Brun, M; Demadrille, R; Faure-Vincent, J

    2011-06-01

    We describe the development of a novel setup, in which large stencils with suspended silicon nitride membranes are combined with atomic force microscopy (AFM) regulation by using tuning forks. This system offers the possibility to perform separate AFM and nanostencil operations, as well as combined modes when using stencil chips with integrated tips. The flexibility and performances are demonstrated through a series of examples, including wide AFM scans in closed loop mode, probe positioning repeatability of a few tens of nanometer, simultaneous evaporation of large (several hundred of micron square) and nanoscopic metals and fullerene patterns in static, multistep, and dynamic modes. This approach paves the way for further developments, as it fully combines the advantages of conventional stenciling with the ones of an AFM driven shadow mask. PMID:21721701

  7. Influence of the degree of order of InGaP on its hardness determined using nanoindentation

    NASA Astrophysics Data System (ADS)

    Zakaria, A.; Fetzer, C. M.; Goorsky, M. S.

    2010-10-01

    Spontaneous atomic ordering takes place during metal-organic vapor phase epitaxy when certain semiconductors alloys start forming long-range arrangements different from their standard lattice unit cells. In the case of InGaP, a zincblende semiconductor, the ordered CuPt(B) structure consists of alternating Ga and In rich (1¯11) and (11¯1) planes. In this investigation, InGaP was deposited on (001) Ge wafers with a 6° miscut toward the [111] direction in two consecutive experiments. A surfactant was used in experiment A while depositing InGaP to induce a lower degree of order. high resolution x-ray diffraction was used to calculate composition and strain of the InGaP epilayers. The symmetric (004) as well as the asymmetric (224) glancing exit reflections were used. The results enabled the extraction of a theoretical band gap energy Eg corrected for strain effects. Photoluminescence was used to measure the actual Eg. By comparing the two, the degree of order η was determined to be 0.12-0.15 for wafers from experiment A and 0.43-0.44 for wafers from experiment B. Atomic force microscopy AFM demonstrated that all experimental wafers had a surface rms roughness of 6.1-7.4 Å. Extensive nanoindentation measurements were performed on samples from both experiments. It was determined that the degree of order has no effect on the nanoindentation hardness of InGaP. Using 1/2 (115) superlattice reflection scans, the InGaP ordered domains size was estimated to be 28.5 nm for sample B1. No superlattice peak was detected in sample A1. The large ordered domain size in B1 explains why no order-hardening behavior was observed in InGaP.

  8. Nanoindentation and thermal characterization of poly (vinylidenefluoride)/MWCNT nanocomposites

    SciTech Connect

    Eggedi, Obulapathi; Valiyaneerilakkal, Uvais; Varghese, Soney; Darla, M. R.

    2014-04-15

    We report the preparation, thermal and micro/nanomechanical behavior of poly (vinylidine diflouride) (PVDF)/multiwalled carbon nanotube (MWCNT) nanocomposites. It has been found that the addition of MWCNT considerably enhances the β-phase formation, thermal and mechanical properties of PVDF. Atomic force microscope (AFM) studies have been performed on the composites under stress conditions to measure the mechanical properties. The nanoscale mechanical properties of the composites like Young's modulus and hardness of the nanocomposites were investigated by nanoindentation technique. Morphological studies of the nanocomposites were also studied, observations show a uniform distribution of MWCNT in the matrix and interfacial adhesion between PVDF and MWCNT was achieved, which was responsible for enhancement in the hardness and Young's modulus. Differential scanning calorimetry (DSC) studies indicate that the melting temperature of the composites have been slightly increased while the heat of fusion markedly decreased with increasing MWCNT content.

  9. Berkovich Nanoindentation on AlN Thin Films

    PubMed Central

    2010-01-01

    Berkovich nanoindentation-induced mechanical deformation mechanisms of AlN thin films have been investigated by using atomic force microscopy (AFM) and cross-sectional transmission electron microscopy (XTEM) techniques. AlN thin films are deposited on the metal-organic chemical-vapor deposition (MOCVD) derived Si-doped (2 × 1017 cm−3) GaN template by using the helicon sputtering system. The XTEM samples were prepared by means of focused ion beam (FIB) milling to accurately position the cross-section of the nanoindented area. The hardness and Young’s modulus of AlN thin films were measured by a Berkovich nanoindenter operated with the continuous contact stiffness measurements (CSM) option. The obtained values of the hardness and Young’s modulus are 22 and 332 GPa, respectively. The XTEM images taken in the vicinity regions just underneath the indenter tip revealed that the multiple “pop-ins” observed in the load–displacement curve during loading are due primarily to the activities of dislocation nucleation and propagation. The absence of discontinuities in the unloading segments of load–displacement curve suggests that no pressure-induced phase transition was involved. Results obtained in this study may also have technological implications for estimating possible mechanical damages induced by the fabrication processes of making the AlN-based devices. PMID:20672096

  10. Nanoindentation on porous bioceramic scaffolds for bone tissue engineering.

    PubMed

    Chowdhury, S; Thomas, Vinoy; Dean, Derrick; Catledge, Shane A; Vohra, Yogesh K

    2005-11-01

    We report nanoindentation mechanical properties measurements on porous ceramic scaffolds made for tissue engineering applications. The scaffolds have been made from tricalcium phosphate (TCP), hydroxyapatite (HA) nanopowder and mixed powders of HA (50 wt%) and TCP (50 wt%) using the polyurethane sponge method, which produces open porous ceramic scaffolds through replication of a porous polymer template. The scaffolds prepared by this method have a controllable pore size and interconnected pore structure. The crystal structures and morphology of porous scaffolds were determined by X-ray diffraction (XRD) and atomic force microscopy (AFM) respectively. Nanoindentation measurements to a depth of 600 nm showed a Young's modulus value of 10.3 GPa for HA+TCP composite scaffolds and 1.5 GPa for TCP scaffolds. The hardness values were 240 MPa for HA+TCP composites and 21 MPa for TCP sample respectively. The results showed that the mechanical properties of the biodegradable scaffolds can be considerably enhanced with the addition of HA while maintaining the interconnected open pores and pore geometry desirable for bone tissue engineering. PMID:16433415

  11. AFM-based mechanical characterization of single nanofibres.

    PubMed

    Neugirg, Benedikt R; Koebley, Sean R; Schniepp, Hannes C; Fery, Andreas

    2016-04-28

    Nanofibres are found in a broad variety of hierarchical biological systems as fundamental structural units, and nanofibrillar components are playing an increasing role in the development of advanced functional materials. Accurate determination of the mechanical properties of single nanofibres is thus of great interest, yet measurement of these properties is challenging due to the intricate specimen handling and the exceptional force and deformation resolution that is required. The atomic force microscope (AFM) has emerged as an effective, reliable tool in the investigation of nanofibrillar mechanics, with the three most popular approaches-AFM-based tensile testing, three-point deformation testing, and nanoindentation-proving preferable to conventional tensile testing in many (but not all) cases. Here, we review the capabilities and limitations of each of these methods and give a comprehensive overview of the recent advances in this field. PMID:27055900

  12. AFM-based mechanical characterization of single nanofibres

    NASA Astrophysics Data System (ADS)

    Neugirg, Benedikt R.; Koebley, Sean R.; Schniepp, Hannes C.; Fery, Andreas

    2016-04-01

    Nanofibres are found in a broad variety of hierarchical biological systems as fundamental structural units, and nanofibrillar components are playing an increasing role in the development of advanced functional materials. Accurate determination of the mechanical properties of single nanofibres is thus of great interest, yet measurement of these properties is challenging due to the intricate specimen handling and the exceptional force and deformation resolution that is required. The atomic force microscope (AFM) has emerged as an effective, reliable tool in the investigation of nanofibrillar mechanics, with the three most popular approaches--AFM-based tensile testing, three-point deformation testing, and nanoindentation--proving preferable to conventional tensile testing in many (but not all) cases. Here, we review the capabilities and limitations of each of these methods and give a comprehensive overview of the recent advances in this field.

  13. Nanoindentation of osteonal bone lamellae.

    PubMed

    Faingold, Anna; Cohen, Sidney R; Wagner, H Daniel

    2012-05-01

    Variations in Young's modulus of individual lamellae around a single bone osteon have been measured in three orthogonal planes by nanoindentation. The objective of these measurements was to establish a correlation between the mechanical properties and the microstructure of the osteonal lamellae. When indentation was performed in a plane perpendicular to the osteon axis (OA), the modulus of the lamella closest to the canal appears to be higher than the modulus of all other lamellae. No such difference was observed in planes parallel to the OA. However, in the parallel planes, an unexpected asymmetry in modulus was detected on opposing sides of the canal, potentially supporting the validity of the rotated plywood structure model of bone lamellae. Finally, based on the experimentally measured Young's modulus values, most osteonal lamellae appear to exhibit structural anisotropy. PMID:22498296

  14. Local Mechanical Properties by Atomic Force Microscopy Nanoindentations

    NASA Astrophysics Data System (ADS)

    Tranchida, Davide; Piccarolo, Stefano

    The analysis of mechanical properties on a nanometer scale is a useful tool for combining information concerning texture organization obtained by microscopy with the properties of individual components. Moreover, this technique promotes the understanding of the hierarchical arrangement in complex natural materials as well in the case of simpler morphologies arising from industrial processes. Atomic Force Microscopy (AFM) can bridge morphological information, obtained with outstanding resolution, to local mechanical properties. When performing an AFM nanoindentation, the rough force curve, i.e., the plot of the voltage output from the photodiode vs. the voltage applied to the piezo-scanner, can be translated into a curve of the applied load vs. the penetration depth after a series of preliminary determinations and calibrations. However, the analysis of the unloading portion of the force curves collected for polymers does not lead to a correct evaluation of Young's modulus. The high slope of the unloading curves is not linked to an elastic behavior, as would be expected, but rather to a viscoelastic effect. This can be argued on the basis that the unloading curves are superimposed on the loading curves in the case of an ideal elastic behavior, as for rubbers, or generally in the case of materials with very short relaxation times. In contrast, when the relaxation time of the sample is close to or even much larger than the indentation time scale, very high slopes are recorded.

  15. Spherical nanoindentation stress–strain curves

    DOE PAGESBeta

    Pathak, Siddhartha; Kalidindi, Surya R.

    2015-03-24

    Although indentation experiments have long been used to measure the hardness and Young's modulus, the utility of this technique in analyzing the complete elastic–plastic response of materials under contact loading has only been realized in the past few years – mostly due to recent advances in testing equipment and analysis protocols. This paper provides a timely review of the recent progress made in this respect in extracting meaningful indentation stress–strain curves from the raw datasets measured in instrumented spherical nanoindentation experiments. These indentation stress–strain curves have produced highly reliable estimates of the indentation modulus and the indentation yield strength inmore » the sample, as well as certain aspects of their post-yield behavior, and have been critically validated through numerical simulations using finite element models as well as direct in situ scanning electron microscopy (SEM) measurements on micro-pillars. Much of this recent progress was made possible through the introduction of a new measure of indentation strain and the development of new protocols to locate the effective zero-point of initial contact between the indenter and the sample in the measured datasets. As a result, this has led to an important key advance in this field where it is now possible to reliably identify and analyze the initial loading segment in the indentation experiments.« less

  16. Spherical nanoindentation stress–strain curves

    SciTech Connect

    Pathak, Siddhartha; Kalidindi, Surya R.

    2015-03-24

    Although indentation experiments have long been used to measure the hardness and Young's modulus, the utility of this technique in analyzing the complete elastic–plastic response of materials under contact loading has only been realized in the past few years – mostly due to recent advances in testing equipment and analysis protocols. This paper provides a timely review of the recent progress made in this respect in extracting meaningful indentation stress–strain curves from the raw datasets measured in instrumented spherical nanoindentation experiments. These indentation stress–strain curves have produced highly reliable estimates of the indentation modulus and the indentation yield strength in the sample, as well as certain aspects of their post-yield behavior, and have been critically validated through numerical simulations using finite element models as well as direct in situ scanning electron microscopy (SEM) measurements on micro-pillars. Much of this recent progress was made possible through the introduction of a new measure of indentation strain and the development of new protocols to locate the effective zero-point of initial contact between the indenter and the sample in the measured datasets. As a result, this has led to an important key advance in this field where it is now possible to reliably identify and analyze the initial loading segment in the indentation experiments.

  17. Measuring the constitutive behavior of viscoelastic solids in the time and frequency domain using flat punch nanoindentation

    SciTech Connect

    Herbert, E. G.; Oliver, W. C.; Lumsdaine, A.; Pharr, George Mathews

    2009-01-01

    The purpose of this work is to further develop experimental methodologies using flat punch nanoindentation to measure the constitutive behavior of viscoelastic solids in the frequency and time domain. The reference material used in this investigation is highly plasticized polyvinylchloride (PVC) with a glass transition temperature of -17 C. The nanoindentation experiments were conducted using a 983-{micro}m-diameter flat punch. For comparative purposes, the storage and loss modulus obtained by nanoindentation with a 103-{micro}m-diameter flat punch and dynamic mechanical analysis are also presented. Over the frequency range of 0.01-50 Hz, the storage and loss modulus measured using nanoindentation and uniaxial compression is shown to be in excellent agreement. The creep compliance function measured using a constant stress test performed in uniaxial compression and flat punch nanoindentation is also shown to correlate well over nearly 4 decades in time. In addition, the creep compliance function predicted from nanoindentation data acquired in the frequency domain is shown to correlate strongly with the creep compliance function measured in the time domain. Time-temperature superposition of nanoindentation data taken at 5, 10, 15, and 22 C shows the sample is not thermorheologically simple, and thus the technique cannot be used to expand the mechanical characterization of this material. Collectively, these results clearly demonstrate the ability of flat punch nanoindentation to accurately and precisely determine the constitutive behavior of viscoelastic solids in the time and frequency domain.

  18. TEM-nanoindentation studies of semiconducting structures.

    PubMed

    Le Bourhis, E; Patriarche, G

    2007-01-01

    This paper reviews the application of nanoindentation coupled with transmission electron microscopy (TEM) to investigations of the plastic behaviour of semiconducting structures and its implication for device design. Instrumented nanoindentation has been developed to extract the mechanical behaviour of small volumes scaled to those encountered in semiconductor heterostructures. We illustrate that TEM is a powerful complementary tool for the study of local plasticity induced by nanoindentation. TEM-nanoindentation allows for detailed understanding of the plastic deformation in semiconducting structures and opens practical routes for improvement of devices. Performances of heterostructures are deteriously affected by dislocations that relax the lattice mismatched layers. Different ways to obtain compliant substructures are being developed in order to concentrate the plastic relaxation underneath the heterostructure. Such approaches allow for mechanical design of micro- and opto-electronic devices to be considered throughout the fabrication process. PMID:16901706

  19. Is the second harmonic method applicable for thin films mechanical properties characterization by nanoindentation?

    NASA Astrophysics Data System (ADS)

    Guillonneau, G.; Kermouche, G.; Teisseire, J.; Barthel, E.; Bec, S.; Loubet, J.-L.

    2015-06-01

    The second harmonic method is a dynamic indentation technique independent of the direct indentation depth measurement. It can be used to determine near-surface mechanical properties of bulk materials more precisely than classical dynamic nanoindentation. In this paper, the second harmonic method is extended to the measurement of the mechanical properties of thin poly(methyl methacrylate) (PMMA) layers deposited onto silicon wafers. It is shown that this new technique gives precise results at small depths (less than 100 nm), even for films with a thickness lower than 500 nm, which was not possible to achieve with the classical continuous stiffness measurement method. However, experimental and numerical results obtained both with classical nanoindentation and second harmonic methods differ at high indentation depth. Using finite element (FE) simulations and AFM measurements, it is shown that the contact depth calculation with classical models can explain this difference.

  20. Nanoindentation of Zr by molecular dynamics simulation

    NASA Astrophysics Data System (ADS)

    Lu (芦子哲), Zizhe; Chernatynskiy, Aleksandr; Noordhoek, Mark J.; Sinnott, Susan B.; Phillpot, Simon R.

    2015-12-01

    Molecular dynamics simulations of nanoindentation are used to study the deformation behaviors of single crystal Zr for four different surface orientations. The comparison of results for two different potentials, an embedded atom method potential and a charged optimized many body potential, reveals the influence of stable and unstable stacking fault energy on dislocation behaviors under nanoindentation. The load-displacement curve, hardness and deformation behaviors of the various surface orientations Zr are compared and the elastic and plastic deformation behaviors are analyzed.

  1. Ceramic Coating Inspection Using Laser-Based Ultrasonics and Nanoindentation

    SciTech Connect

    Steen, T. L.; Murray, T. W.; Basu, S. N.; Sarin, V. K.

    2007-03-21

    A combination of laser-based ultrasonic (LBU) inspection and nanoindentation testing is used to evaluate the thickness uniformity and through-thickness mechanical property distributions in 5-20 {mu}m thick CVD environmental barrier coatings. Mullite (3Al2O3{center_dot}2SiO2) coatings grown on silicon carbide substrates are studied in order to provide feedback on the growth process under a range of operating conditions. Nanoindentation tests are performed on polished coating cross sections, and the depth dependence of the elastic modulus of each coating is found. In the LBU experiments, a modulated continuous wave (CW) source is used for surface wave generation. The source is held at a fixed temporal frequency as it is scanned over the surface of the coating. At each temporal frequency of interest, the spatial frequencies of the acoustic modes are found, allowing for phase velocities to be determined. The mean values of elastic moduli found using the LBU approach compare well with the nanoindentation results.

  2. Atomistic processes of dislocation generation and plastic deformation during nanoindentation

    SciTech Connect

    Begau, C.; Hartmaier, A.; George, Easo P; Pharr, George M

    2011-01-01

    To enable plastic deformation during nanoindentation of an initially defect-free crystal, it is necessary first to produce dislocations. While it is now widely accepted that the nucleation of the first dislocations occurs at the start of the pop-in event frequently observed in experiments, it is unclear how these initial dislocations multiply during the early stages of plastic deformation and produce pop-in displacements that are typically much larger than the magnitude of the Burgers vector. This uncertainty about the complex interplay between dislocation multiplication and strain hardening during nanoindentation makes a direct correlation between force-displacement curves and macroscopic material properties difficult. In this paper, we study the early phase of plastic deformation during nanoindentation with the help of large-scale molecular dynamics simulations. A skeletonization method to simplify defect structures in atomistic simulations enables the direct observation and quantitative analysis of dislocation nucleation and multiplication processes occurring in the bulk as well as at the surface.

  3. In-situ nanoindentation specimen holder for a high-voltage transmission electron microscope

    SciTech Connect

    Dahmen; U; Wall, M A

    1998-09-17

    This report describes the design, construction, and testing of a nanoindentation specimen holder used for dynamic observation of subsurface microstructure evolution under an indenter tip, while viewing in cross-section in a high-voltage transmission electron microscope (TEM). It also discusses the initial experimental results from in-situ indentation of Si samples in the TEM to demonstrate the capability of this new nanoindentation specimen holder, which uses three-axis position control of a diamond indenter in combination with micromachined specimens. Additionally, the sample design techniques developed for these procedures may eliminate the need for TEM specimen preparation in future ex-situ nanoindentation experiments and for sample preparation for characterizing these experiments in the electron microscope.

  4. Low Temperature Plasticity of Olivine Determined by Nano-indentation

    NASA Astrophysics Data System (ADS)

    Skemer, P. A.; Kranjc, K.; Rouse, Z.; Flores, K.

    2015-12-01

    Earth's upper mantle is thought to deform mainly by dislocation creep, during which strain-rate and stress are related by a simple power law equation. However at much higher stresses there is a break-down in the power law relationship and strain-rate depends exponentially on stress. This phenomenon, known as low temperature plasticity, may be important in the shallow ductile or semi-brittle regions of the lithosphere, at the tips of cracks, or during high-stress laboratory experiments. Several studies have attempted to constrain the low-temperature rheology of olivine using micro-indentation or high pressure experiments. In this study we provide the first measurements of olivine rheology at low temperature using instrumented nano-indention. Although nano-indentation has been widely used in the materials sciences, its application in the Earth sciences has been very limited. Nano-indentation methods provide rheological measurements that are significantly more precise than other mechanical tests at high pressure and temperature. Moreover, experiments are rapid and largely non-destructive, so many tests can be conducted in a short amount of time. In this study, olivine single crystal and polycrystalline samples were tested using a Hysitron TI950 TriboIndenter. Temperature was varied using a cooling/heating stage from 0-175°C. Experiments were conducted under quasi-static and constant strain-rate conditions. Indentation hardness measurements were converted to uniaxial rheological properties to facilitate direct comparison with previous studies. Yield strengths for olivine range from 4.19 GPa at 175°C to 4.60 GPa at 0°C. Using various models for obstacles to dislocation motion, data are extrapolated to 0 Kelvin to extract a Peierls stress for olivine (5.32-6.45 GPa), which is at the lower end of the range of values determined in previous studies. This study demonstrates the efficacy of the nano-indentation method for the study of mineral rheology, and opens a

  5. Dislocation luminescence in GaN single crystals under nanoindentation

    NASA Astrophysics Data System (ADS)

    Huang, Jun; Xu, Ke; Fan, Ying Min; Wang, Jian Feng; Zhang, Ji Cai; Ren, Guo Qiang

    2014-12-01

    This work presents an experimental study on the dislocation luminescence in GaN by nanoindentation, cathodoluminescence, and Raman. The dislocation luminescence peaking at 3.12 eV exhibits a series of special properties in the cathodoluminescence measurements, and it completely disappears after annealing at 500°C. Raman spectroscopy shows evidence for existence of vacancies in the indented region. A comprehensive investigation encompassing cathodoluminescence, Raman, and annealing experiments allow the assignment of dislocation luminescence to conduction-band-acceptor transition involving Ga vacancies. The nanoscale plasticity of GaN can be better understood by considering the dislocation luminescence mechanism.

  6. Structure-property-glass transition relationships in non-isocyanate polyurethanes investigated by dynamic nanoindentation

    NASA Astrophysics Data System (ADS)

    Weyand, Stephan; Blattmann, Hannes; Schimpf, Vitalij; Mülhaupt, Rolf; Schwaiger, Ruth

    2016-07-01

    Newly developed green-chemistry approaches towards the synthesis of non-isocyanate polyurethane (NIPU) systems represent a promising alternative to polyurethanes (PU) eliminating the need for harmful ingredients. A series of NIPU systems were studied using different nanoindentation techniques in order to understand the influence of molecular parameters on the mechanical behavior. Nanoindentation revealed a unique characteristic feature of those materials, i.e. stiffening with increasing deformation. It is argued that the origin of this observed stiffening is a consequence of the thermodynamic state of the polymer network, the molecular characteristics of the chemical building blocks and resulting anisotropic elastic response of the network structure. Flat-punch nanoindentation was applied in order to characterize the constitutive viscoelastic nature of the materials. The complex modulus shows distinct changes as a function of the NIPU network topology illustrating the influence of the chemical building blocks. The reproducibility of the data indicates that the materials are homogeneous over the volumes sampled by nanoindentation. Our study demonstrates that nanoindentation is very well-suited to investigate the molecular characteristics of NIPU materials that cannot be quantified in conventional experiments. Moreover, the technique provides insight into the functional significance of complex molecular architectures thereby supporting the development of NIPU materials with tailored properties.

  7. Dynamic nanoindentation by instrumented nanoindentation and force microscopy: a comparative review

    PubMed Central

    Kalfon-Cohen, Estelle

    2013-01-01

    Summary Viscoelasticity is a complex yet important phenomenon that drives material response at different scales of time and space. Burgeoning interest in nanoscale dynamic material mechanics has driven, and been driven by two key techniques: instrumented nanoindentation and atomic force microscopy. This review provides an overview of fundamental principles in nanoindentation, and compares and contrasts these two techniques as they are used for characterization of viscoelastic processes at the nanoscale. PMID:24367751

  8. Probing the mechanical properties of dental porcelain through nanoindentation

    NASA Astrophysics Data System (ADS)

    Manda, Marianthi; Moschakis, Nikolaos; Konstantinidis, Avraam; Christophilos, Demetrios; Papadopoulou, Lambrini; Koidis, Petros; Aifantis, Elias

    2012-11-01

    The purpose of this short communication is to report on some micro/nanoscale aspects of the mechanical behavior of dental porcelain. Specimens were characterized by micro-Raman spectroscopy and scanning electron microscopy (SEM) coupled with energy dispersive spectroscopy (EDS). Massive nanoindentation experiments on the surface of the specimens were performed, and typical load-displacement or load-depth (P-h) curves were obtained, which in turn were used to determine the Young modulus (E) and nanoindentation hardness (n-H), based on the Oliver-Pharr method [1]. Statistical analyses were carried out to determine the Spearman’s rank correlation coefficient (Spearman’s ρ), along with non-parametric linear regression analysis by employing Kolmogorov-Smirnov and Two-Step Cluster tests. Densification due to grain boundary diffusion and open-pore elimination was revealed by SEM. EDS analysis indicated a leucite-dispersed silicate glass matrix, as well as its contamination by traces of other minerals. Raman spectroscopy supported the EDS assignments. The P-h curves suggested that inelastic deformation and material flow increases at larger depths. Spearman’s ρ value showed strong dependence of E and n-H on h, indicating the occurrence of a size effect. The logarithmic data of E and n-H as functions of h were fitted by using linear regression analysis. The data did not obey a normal distribution (as the Kolmogorov-Smirnov test showed) due to the chemical heterogeneity involved. The Two-Step Cluster analysis indicated clustering in four groups associated with the chemical heterogeneity of the surface. Similar works using nanoindentation to determine the mechanical properties of dental materials can be found, for example, in [2, 3]. Corresponding methods for extracting the values of E and n-H from P-h experimental curves can be found, for example, in [4-6].

  9. Low-temperature plastic rheology of olivine determined by nanoindentation

    NASA Astrophysics Data System (ADS)

    Kranjc, Kelly; Rouse, Zachary; Flores, Katharine M.; Skemer, Philip

    2016-01-01

    Low-temperature plasticity is a deformation mechanism that occurs mainly at high stress and low temperatures and may be important in the shallow lithosphere, at the tips of cracks, and in laboratory experiments. Previous studies investigating the low-temperature plasticity of the mineral olivine have exhibited wide variability in their extrapolations to the athermal flow strength or Peierls stress. To better constrain the rheology of olivine, nanoindentation tests were performed on samples in the temperature range of 0-175°C. The indentation properties were converted to uniaxial properties using a finite element-based method. The data were fit to a standard flow law for low-temperature plasticity, and Peierls stresses between 5.32 and 6.45 GPa were obtained. These results provide increased confidence in the extrapolation of high-pressure and high-temperature laboratory experiments to low-temperature conditions and illustrate the applicability of nanoindentation methods to the study of mineral rheology.

  10. Experimental Analysis of the Elastic Plastic Transition During Nanoindentation of Single Crystal a-Silicon Nitride

    SciTech Connect

    Jang, Jae-il; Bei, Hongbin; Becher, Paul F; Pharr, George M

    2012-01-01

    The elastic-to-plastic transition in single crystal a-silicon nitride was experimentally characterized through a series of nanoindentation experiments using a spherical indenter. The experimental results provide a quantitative description of the critical shear strengths for the transition, as well as estimates of the shear modulus and nanohardness of the material.

  11. Nanoindentation and nanoscratching of hard carbon coatings for magnetic disks

    SciTech Connect

    Tsui, T.Y.; Pharr, G.M.; Oliver, W.C.; Bhatia, C.S.; White, R.L.; Anders, S.; Anders, A.; Brown, I.G.

    1995-06-01

    Nanoindentation and nanoscratching experiments have been performed to assess the mechanical properties of several carbon thin films with potential application as wear resistant coatings for magnetic disks. These include three hydrogenated-carbon films prepared by sputter deposition in a H{sub 2}/Ar gas mixture (hydrogen contents of 20, 34, and 40 atomic %) and a pure carbon film prepared by cathodic-arc plasma techniques. Each film was deposited on a silicon substrate to thickness of about 300 run. The hardness and elastic modulus were measured using nanoindentation methods, and ultra-low load scratch tests were used to assess the scratch resistance of the films and measure friction coefficients. Results show that the hardness, elastic modulus, and scratch resistance of the 20 and 34% hydrogenated films are significantly greater than the 40% film, thereby showing that there is a limit to the amount of hydrogen producing beneficial effects. The cathodic-arc film, with a hardness of greater than 59 GPa, is considerably harder than any of the hydrogenated films and has a superior scratch resistance.

  12. The Conductance of Nanotubes Deformed by the AFM Tip

    NASA Technical Reports Server (NTRS)

    Svizhenko, Alexei; Maiti, Amitesh; Anantram, M. P.

    2003-01-01

    The conductance drop under AFM-tip deformation can be explained by stretching of the tube length. NT sensors can be built utilizing uniform stretching. Single sp3 bond cross section cannot block electrons, because another conducting path may exist. AFM tip which forms sp3 bonds with the tube will decrease conductance. In the "table experiment" a conductance drop of 2 orders of magnitude happened only after some bonds were broken.

  13. PREFACE: Non-contact AFM Non-contact AFM

    NASA Astrophysics Data System (ADS)

    Giessibl, Franz J.; Morita, Seizo

    2012-02-01

    This special issue is focussed on high resolution non-contact atomic force microscopy (AFM). Non-contact atomic force microscopy was established approximately 15 years ago as a tool to image conducting and insulating surfaces with atomic resolution. Since 1998, an annual international conference has taken place, and although the proceedings of these conferences are a useful source of information, several key developments warrant devoting a special issue to this subject. In the theoretic field, the possibility of supplementing established techniques such as scanning tunneling microscopy (STM) and Kelvin probe microscopy with atomically resolved force micrsoscopy poses many challenges in the calculation of contrast and contrast reversal. The surface science of insulators, self-assembled monolayers and adsorbates on insulators is a fruitful field for the application of non-contact AFM: several articles in this issue are devoted to these subjects. Atomic imaging and manipulation have been pioneered using STM, but because AFM allows the measurement of forces, AFM has had a profound impact in this field as well. Three-dimensional force spectroscopy has allowed many important insights into surface science. In this issue a combined 3D tunneling and force microscopy is introduced. Non-contact AFM typically uses frequency modulation to measure force gradients and was initially used mainly in a vacuum. As can be seen in this issue, frequency modulation is now also used in ambient conditions, allowing better spatial and force resolution. We thank all of the contributors for their time and efforts in making this special issue possible. We are also very grateful to the staff of IOP Publishing for handling the administrative aspects and for steering the refereeing process. Non-contact AFM contents Relation between the chemical force and the tunnelling current in atomic point contacts: a simple model Pavel Jelínek, Martin Ondrácek and Fernando Flores Theoretical simulation of

  14. Deformation Mechanisms of Gum Metals Under Nanoindentation

    NASA Astrophysics Data System (ADS)

    Sankaran, Rohini Priya

    defect structures to applied loading, we perform ex-situ nanoindentation. Nanoindentation is a convenient method as the plastic deformation is localized and probes a nominally defect free volume of the material. We subsequently characterize the defect structures in these alloys with both conventional TEM and advanced techniques such as HAADF HRSTEM and nanoprobe diffraction. These advanced techniques allow for a more thorough understanding of the observed deformation features. The main findings from this investigation are as follows. As expected we observe that a non-equilibrium phase, o, is present in the leaner beta-stabilized alloy, ST Ref-1. We do not find any direct evidence of secondary phases in STGM, and we find the beta phase in CWGM, along with lath microstructure with subgrain structure consisting of dislocation cell networks. Upon nanoindentation, we find twinning accompanied by beta nucleation on the twin boundary in ST Ref-1 samples. This result is consistent with previous findings and is reasonable considering the alloy is unstable with respect to beta transformation. We find deformation nanotwinning in cold worked gum metals under nanoindentation, which is initially surprising. We argue that when viewed as a nanocrystalline material, such a deformation mechanism is consistent with previous work, and furthermore, a deformation nanotwinned structure does not preclude an ideal shear mechanism from operating in the alloy. Lastly, we observe continuous lattice rotations in STGM under nanoindentation via nanoprobe diffraction. With this technique, for the first time we can demonstrate that the lattice rotations are truly continuous at the nanoscale. We can quantify this lattice rotation, and find that even though the rotation is large, it may be mediated by a reasonable geometrically necessary dislocation density, and note that similar rotations are typically observed in other materials under nanoindentation. HRSTEM and conventional TEM data confirm the

  15. Nanoindentation on the doubler plane of KDP single crystal

    NASA Astrophysics Data System (ADS)

    Xiaoguang, Guo; Xiaoji, Zhang; Xianzhao, Tang; Dongming, Guo; Hang, Gao; Xiaoji, Teng

    2013-03-01

    The nanohardness is from 1.44 to 2.61 GPa, the Vickers hardness is from 127 to 252 Vickers, and elastic modulus is from 52 to 123 GPa by the nanoindentation experiments on the doubler plane of KDP crystal. An indentation size effect is observed on the doubler plane in the test as the nanohardness and elastic modulus decreases with the increase of the maximum load. Slippage is identified as the major mode of plastic deformation, and pop-in events are attributed to the initiation of slippage. And the variation of unloading curve end is the result of stick effects between the indenter and the contact surface. The depth of the elastic deformation, which is between 40 and 75 nm, is responsible for the elastic deformation. The doubler plane of KDP crystal has anisotropy, and the relative anisotropy of nanohardness is 8.2% and the relative anisotropy of elastic modulus is 8.0%.

  16. Initial Stages of Yield in Nanoindentation

    SciTech Connect

    Houston, J.E.; Jarausch, K.F.; Kiely, J.D.; Russell, P.E.

    1998-11-24

    We have used the Interracial Force Microscope" to perform nanoindentations on Au single- crystal surfaces. We have observed two distinct regimes of plastic deformation which are distinguished by the magnitude of discontinuities in load relaxation. At lower stresses, relaxation occurs in small deviations from elastic behavior, while at the higher stresses they take the form of large load drops often resulting in complete relaxation of the applied load. These major events create a relatively wide plastic zone that subsequently deepens more rapidly than it widens. We discuss these findings in terms of contrasting models of dislocation processes in the two regimes.

  17. Nanoindentation-induced amorphization in silicon carbide

    NASA Astrophysics Data System (ADS)

    Szlufarska, Izabela; Kalia, Rajiv K.; Nakano, Aiichiro; Vashishta, Priya

    2004-07-01

    The nanoindentation-induced amorphization in SiC is studied using molecular dynamics simulations. The load-displacement response shows an elastic shoulder followed by a plastic regime consisting of a series of load drops. Analyses of bond angles, local pressure, and shear stress, and shortest-path rings show that these drops are related to dislocation activities under the indenter. We show that amorphization is driven by coalescence of dislocation loops and that there is a strong correlation between load-displacement response and ring distribution.

  18. Modeling the Interaction between AFM Tips and Pinned Surface Nanobubbles.

    PubMed

    Guo, Zhenjiang; Liu, Yawei; Xiao, Qianxiang; Schönherr, Holger; Zhang, Xianren

    2016-01-26

    Although the morphology of surface nanobubbles has been studied widely with different AFM modes, AFM images may not reflect the real shapes of the nanobubbles due to AFM tip-nanobubble interactions. In addition, the interplay between surface nanobubble deformation and induced capillary force has not been well understood in this context. In our work we used constraint lattice density functional theory to investigate the interaction between AFM tips and pinned surface nanobubbles systematically, especially concentrating on the effects of tip hydrophilicity and shape. For a hydrophilic tip contacting a nanobubble, its hydrophilic nature facilitates its departure from the bubble surface, displaying a weak and intermediate-range attraction. However, when the tip squeezes the nanobubble during the approach process, the nanobubble shows an elastic effect that prevents the tip from penetrating the bubble, leading to a strong nanobubble deformation and repulsive interactions. On the contrary, a hydrophobic tip can easily pierce the vapor-liquid interface of the nanobubble during the approach process, leading to the disappearance of the repulsive force. In the retraction process, however, the adhesion between the tip and the nanobubble leads to a much stronger lengthening effect on nanobubble deformation and a strong long-range attractive force. The trends of force evolution from our simulations agree qualitatively well with recent experimental AFM observations. This favorable agreement demonstrates that our model catches the main intergradient of tip-nanobubble interactions for pinned surface nanobubbles and may therefore provide important insight into how to design minimally invasive AFM experiments. PMID:26751634

  19. Characterization of the interaction between AFM tips and surface nanobubbles.

    PubMed

    Walczyk, Wiktoria; Schönherr, Holger

    2014-06-24

    While the presence of gaseous enclosures observed at various solid-water interfaces, the so-called "surface nanobubles", has been confirmed by many groups in recent years, their formation, properties, and stability have not been convincingly and exhaustively explained. Here we report on an atomic force microscopy (AFM) study of argon nanobubbles on highly oriented pyrolitic graphite (HOPG) in water to elucidate the properties of nanobubble surfaces and the mechanism of AFM tip-nanobubble interaction. In particular, the deformation of the nanobubble-water interface by the AFM tip and the question whether the AFM tip penetrates the nanobubble during scanning were addressed by this combined intermittent contact (tapping) mode and force volume AFM study. We found that the stiffness of nanobubbles was smaller than the cantilever spring constant and comparable with the surface tension of water. The interaction with the AFM tip resulted in severe quasi-linear deformation of the bubbles; however, in the case of tip-bubble attraction, the interface deformed toward the tip. We tested two models of tip-bubble interaction, namely, the capillary force and the dynamic interaction model, and found, depending on the tip properties, good agreement with experimental data. The results showed that the tip-bubble interaction strength and the magnitude of the bubble deformation depend strongly on tip and bubble geometry and on tip and substrate material, and are very sensitive to the presence of contaminations that alter the interfacial tension. In particular, nanobubbles interacted differently with hydrophilic and hydrophobic AFM tips, which resulted in qualitatively and quantitatively different force curves measured on the bubbles in the experiments. To minimize bubble deformation and obtain reliable AFM results, nanobubbles must be measured with a sharp hydrophilic tip and with a cantilever having a very low spring constant in a contamination-free system. PMID:24856074

  20. Endodontic instruments after torsional failure: nanoindentation test.

    PubMed

    Jamleh, Ahmed; Sadr, Alireza; Nomura, Naoyuki; Ebihara, Arata; Yahata, Yoshio; Hanawa, Takao; Tagami, Junji; Suda, Hideaki

    2014-01-01

    This study aimed to evaluate effects of torsional loading on the mechanical properties of endodontic instruments using the nanoindentation technique. ProFile (PF; size 30, taper 04; Dentsply Maillefer, Switzerland) and stainless steel (SS; size 30, taper 02; Mani, Japan) instruments were subjected to torsional test. Nanoindentation was then performed adjacent to the edge of fracture (edge) and at the cutting part beside the shank (shank). Hardness and elastic modulus were measured under 100-mN force on 100 locations at each region, and compared to those obtained from the same regions on new instruments. It showed that PF and SS instruments failed at 559 ± 67 and 596 ± 73 rotation degrees and mean maximum torque of 0.90 ± 0.07 and 0.99 ± 0.05 N-cm, respectively. Hardness and elastic modulus ranged 4.8-6.7 and 118-339 GPa in SS, and 2.7-3.2 and 52-81 GPa in PF. Significant differences between torsion-fractured and new instruments in hardness and elastic modulus were detected in the SS system used. While in PF system, the edge region after torsional fracture had significantly lower hardness and elastic modulus compared to new instruments. The local hardness and modulus of elasticity of endodontic instruments adjacent to the fracture edge are significantly reduced by torsional loading. PMID:24610598

  1. Deformation Mechanisms of Gum Metals Under Nanoindentation

    NASA Astrophysics Data System (ADS)

    Sankaran, Rohini Priya

    defect structures to applied loading, we perform ex-situ nanoindentation. Nanoindentation is a convenient method as the plastic deformation is localized and probes a nominally defect free volume of the material. We subsequently characterize the defect structures in these alloys with both conventional TEM and advanced techniques such as HAADF HRSTEM and nanoprobe diffraction. These advanced techniques allow for a more thorough understanding of the observed deformation features. The main findings from this investigation are as follows. As expected we observe that a non-equilibrium phase, o, is present in the leaner beta-stabilized alloy, ST Ref-1. We do not find any direct evidence of secondary phases in STGM, and we find the beta phase in CWGM, along with lath microstructure with subgrain structure consisting of dislocation cell networks. Upon nanoindentation, we find twinning accompanied by beta nucleation on the twin boundary in ST Ref-1 samples. This result is consistent with previous findings and is reasonable considering the alloy is unstable with respect to beta transformation. We find deformation nanotwinning in cold worked gum metals under nanoindentation, which is initially surprising. We argue that when viewed as a nanocrystalline material, such a deformation mechanism is consistent with previous work, and furthermore, a deformation nanotwinned structure does not preclude an ideal shear mechanism from operating in the alloy. Lastly, we observe continuous lattice rotations in STGM under nanoindentation via nanoprobe diffraction. With this technique, for the first time we can demonstrate that the lattice rotations are truly continuous at the nanoscale. We can quantify this lattice rotation, and find that even though the rotation is large, it may be mediated by a reasonable geometrically necessary dislocation density, and note that similar rotations are typically observed in other materials under nanoindentation. HRSTEM and conventional TEM data confirm the

  2. Thermodynamic work of adhesion measurements of polymer bonded explosive constituents via the Wilhelmy plate technique and their application to AFM pull-off experiments

    NASA Astrophysics Data System (ADS)

    Williamson, D. M.; Hamilton, N. R.; Palmer, S. J. P.; Jardine, A. P.; Leppard, C.

    2014-05-01

    A major strength limiting factor for polymer bonded explosives above their glass-transition conditions is the magnitude of adhesion that exists between the polymeric matrix binder-system and the filler particles. Experimental measurements of the components of the free surface energy of the binder KEL-F8OO have been made using the Wilhelmy Plate technique. These data can be combined with equivalent data on the filler particles to calculate the so-called Thermodynamic Work of Adhesion. This under-pinning quantity can be used to predict the levels of load (stress) required to cause debonding in different geometries. A simple geometry of interest is a spherical-cap of polymer debonding from a flat substrate. Experiments using this geometry have been performed with an Atomic Force Microscope pulloff technique to measure the critical loads (stresses) required for debonding. There is excellent agreement between the predicted values based on the Wilhelmy Plate data and the measured values from the Atomic Force Microscope. Experimental data and understanding are required for the development and validation of microstructural models of mechanical behaviour.

  3. Nanoindentation techniques for the cell walls of wood

    NASA Astrophysics Data System (ADS)

    Jakes, Joseph Eugene

    There is a recognized need in forest products research to better understand how the mechanical properties of wood derive from the basic polymer components that make up the wood. For development of new engineered wood products there is the need to understand how chemical additives and adhesives interact with wood polymers and influence properties at the cellular level. To meet these needs I have developed nanoindentation techniques for probing the mechanical properties of the cell walls in wood. There are two, key results of this research. The first is a newly invented structural compliance method for isolating the properties of local regions within materials and excluding artifacts brought about by neighboring edges including free edges and interfaces between dissimilar cell wall layers. The second consists of methods to obtain viscoplastic and viscoelastic data over as wide a range of deformation rate as possible. The broadband nanoindentation creep (BNC) technique assesses the viscoplastic properties over 5 orders of magnitude in deformation rate (-10-4 to 10 s-1). Viscoelastic measurements can be made with unloading times ranging from 0.01 to 100 s, resulting in viscoelastic data that span four orders of magnitude in frequency or inverse time (˜10-3 to 10 s-1). To demonstrate the efficacy of these techniques, experiments are performed on a range of materials including fused silica, silicon, molybdenum, siliconon-insulator layered specimen, poly (methylmetacrylate), polycarbonate, polystyrene, wood cells in loblolly pine (Pinus taeda ), and a polypropylene-wood composite. Finally, the structural compliance method and BNC are combined to explore polymeric methylene diphenyl diisocyanate (pMDI)-wood interactions. The data suggest that pMDI polymerizes in situ to create an interpenetrating polymer network.

  4. Nanomechanical probing of soft matter through hydrophobic AFM tips fabricated by two-photon polymerization

    NASA Astrophysics Data System (ADS)

    Suriano, Raffaella; Zandrini, Tommaso; De Marco, Carmela; Osellame, Roberto; Turri, Stefano; Bragheri, Francesca

    2016-04-01

    Atomic force microscopy (AFM) nanoindentation of soft materials is a powerful tool for probing mechanical properties of biomaterials. Though many results have been reported in this field over the last decade, adhesion forces between the tip and the sample hinder the elastic modulus measurement when hydrophilic soft samples are investigated. Here, two-photon polymerization (2PP) technology was used to fabricate hydrophobic perfluoropolyether-based AFM tips. The hydrophobic 2PP tips allowed us to overcome the limitations of commercial and functionalized tips as well as to successfully measure the elastic modulus of medically relevant soft materials in air. Our results obtained in the characterization of poly(dimethyl siloxane) and polyethylene glycol hydrogels showed lower adhesion forces over a larger measurement range when compared to measurements performed with commercial tips. The elastic moduli measured by means of hydrophobic 2PP AFM tips were also found to be comparable to those obtained using conventional techniques for macroscopic samples. We successfully showed that the hydrophobic AFM tips developed by this highly versatile technology enable the study of mechanical properties of soft matter, benefiting from reduced sample-tip interactions, and a custom-made shape and dimension of the tips.

  5. Nanomechanical probing of soft matter through hydrophobic AFM tips fabricated by two-photon polymerization.

    PubMed

    Suriano, Raffaella; Zandrini, Tommaso; De Marco, Carmela; Osellame, Roberto; Turri, Stefano; Bragheri, Francesca

    2016-04-15

    Atomic force microscopy (AFM) nanoindentation of soft materials is a powerful tool for probing mechanical properties of biomaterials. Though many results have been reported in this field over the last decade, adhesion forces between the tip and the sample hinder the elastic modulus measurement when hydrophilic soft samples are investigated. Here, two-photon polymerization (2PP) technology was used to fabricate hydrophobic perfluoropolyether-based AFM tips. The hydrophobic 2PP tips allowed us to overcome the limitations of commercial and functionalized tips as well as to successfully measure the elastic modulus of medically relevant soft materials in air. Our results obtained in the characterization of poly(dimethyl siloxane) and polyethylene glycol hydrogels showed lower adhesion forces over a larger measurement range when compared to measurements performed with commercial tips. The elastic moduli measured by means of hydrophobic 2PP AFM tips were also found to be comparable to those obtained using conventional techniques for macroscopic samples. We successfully showed that the hydrophobic AFM tips developed by this highly versatile technology enable the study of mechanical properties of soft matter, benefiting from reduced sample-tip interactions, and a custom-made shape and dimension of the tips. PMID:26926558

  6. Nanomechanical properties of α-synuclein amyloid fibrils: a comparative study by nanoindentation, harmonic force microscopy, and Peakforce QNM

    NASA Astrophysics Data System (ADS)

    Sweers, Kim; van der Werf, Kees; Bennink, Martin; Subramaniam, Vinod

    2011-12-01

    We report on the use of three different atomic force spectroscopy modalities to determine the nanomechanical properties of amyloid fibrils of the human α-synuclein protein. α-Synuclein forms fibrillar nanostructures of approximately 10 nm diameter and lengths ranging from 100 nm to several microns, which have been associated with Parkinson's disease. Atomic force microscopy (AFM) has been used to image the morphology of these protein fibrils deposited on a flat surface. For nanomechanical measurements, we used single-point nanoindentation, in which the AFM tip as the indenter is moved vertically to the fibril surface and back while the force is being recorded. We also used two recently developed AFM surface property mapping techniques: Harmonic force microscopy (HarmoniX) and Peakforce QNM. These modalities allow extraction of mechanical parameters of the surface with a lateral resolution and speed comparable to tapping-mode AFM imaging. Based on this phenomenological study, the elastic moduli of the α-synuclein fibrils determined using these three different modalities are within the range 1.3-2.1 GPa. We discuss the relative merits of these three methods for the determination of the elastic properties of protein fibrils, particularly considering the differences and difficulties of each method.

  7. Direct comparison of nanoindentation and macroscopic measurements of bone viscoelasticity

    PubMed Central

    Shepherd, Tara N.; Zhang, Jingzhou; Ovaert, Timothy C.; Roeder, Ryan K.; Niebur, Glen L.

    2011-01-01

    Nanoindentation has become a standard method for measuring mechanical properties of bone, especially within microstructural units such as individual osteons or trabeculae. The use of nanoindentation to measure elastic properties has been thoroughly studied and validated. However, it is also possible to assess time dependent properties of bone by nanoindentation. The goal of this study was to compare time dependent mechanical properties of bone measured at the macroscopic level with those measured by nanoindentation. Twelve samples were prepared from the posterior distal femoral cortex of young cows. Initially, dogbone samples were prepared and subjected to torsional stress relaxation in a saline bath at 37 C. A 5 mm thick disk was subsequently sectioned from the gage length, and subjected to nanoindentation. Nanoindentation was performed on hydrated samples using a standard protocol with 20 indents performed in 20 different osteons in each sample. Creep and stress relaxation data were fit to a Burgers four parameter rheological model, a five parameter generalized Maxwell model, and a three parameter standard linear solid. For Burgers viscoelastic model, the time constants measured by nanoindentation and torsion were weakly negatively correlated, while for the other two models the time constants were uncorrelated. The results support the notion that the viscoelastic behavior of bone at the macroscopic scale is primarily due to microstructural features, interfaces, or fluid flow, rather than viscous behavior of the bone tissue. As viscoelasticity affects the fatigue behavior of materials, the microscale properties may provide a measure of bone quality associated with initial damage formation. PMID:22098905

  8. Finite-element modeling of nanoindentation

    SciTech Connect

    Knapp, J.A.; Follstaedt, D.M.; Myers, S.M.; Barbour, J.C.; Friedmann, T.A.

    1999-02-01

    Procedures have been developed based on finite-element modeling of nanoindentation data to obtain the mechanical properties of thin films and ion-beam-modified layers independently of the properties of the underlying substrates. These procedures accurately deduce the yield strength, Young{close_quote}s elastic modulus, and layer hardness from indentations as deep as 50{percent} of the layer thickness or more. We have used these procedures to evaluate materials ranging from ion implanted metals to deposited, diamond-like carbon layers. The technique increases the applicability of indentation testing to very thin layers, composite layers, and modulated compositions. This article presents an overview of the procedures involved and illustrates them with selected examples. {copyright} {ital 1999 American Institute of Physics.}

  9. Quantitative in situ nanoindentation in an electron microscope

    SciTech Connect

    Minor, A. M.; Morris, J. W.; Stach, E. A.

    2001-09-10

    We report the development of a method for quantitative, in situ nanoindentation in an electron microscope and its application to study the onset of deformation during the nanoindentation of aluminum films. The force--displacement curve developed shows the characteristic ''staircase'' instability at the onset of plastic deformation. This instability corresponds to the first appearance of dislocations in a previously defect-free grain. Plastic deformation proceeds through the formation and propagation of prismatic loops punched into the material, and half loops that emanate from the sample surface. These results represent the first real time observations of the discrete microstructural events that occur during nanoindentation.

  10. [Estimations of mechanical properties of bones using nanoindentation].

    PubMed

    Sakamoto, Makoto

    2016-01-01

    Nanoindentation has been applied in recent years to measure the mechanical properties of bone tissues at a microscopic scale, overcoming the limitations of traditional mechanical testing techniques for small samples. This method is precise and accurate and appears well suited for measuring mechanical properties in bone. Dynamic nanoindentation is also a promising method of measuring the viscoelastic properties of bone tissues at smaller length and load scales than allowed by other testing methods, thus allowing individual constituents and local regions of inhomogeneous tissues to be characterized individually. This article describes our nanoindentation studies of bone tissues with recent studies. PMID:26728534

  11. Characterization of Viscoelastic Properties of Polymeric Materials Through Nanoindentation

    NASA Technical Reports Server (NTRS)

    Odegard, G. M.; Bandorawalla, T.; Herring, H. M.; Gates, T. S.

    2003-01-01

    Nanoindentation is used to determine the dynamic viscoelastic properties of six polymer materials. It is shown that varying the harmonic frequency of the nanoindentation does not have any significant effect on the measured storage and loss moduli of the polymers. Agreement is found between these results and data from DMA testing of the same materials. Varying the harmonic amplitude of the nanoindentation does not have a significant effect on the measured properties of the high performance resins, however, the storage modulus of the polyethylene decreases as the harmonic amplitude increases. Measured storage and loss moduli are also shown to depend on the density of the polyethylene.

  12. Microstructural properties of superalloys investigated by nanoindentations in an atomic force microscope

    SciTech Connect

    Goeken, M.; Kempf, M.

    1999-02-05

    The microstructure of nickel-base superalloys with differently shaped {gamma}{prime} precipitates determines their excellent high-temperature behavior. A reliable quantitative determination of volume fraction and particle size distribution (PSD) of these precipitates is difficult, since the size of the precipitates is often below 100 nm. With an atomic force microscope (AFM), sections through specimens are analyzed with a resolution in the nanometer range, which allows a quantitative determination of the {gamma}{prime} volume content and PSD for different superalloys. Thus, determined volume fractions for the {gamma}{prime} phase in the superalloys CMSX-6 and Waspaloy amount to 56% and 27%, respectively. A combination of an AFM with a nanoindentation system also allows the measurement of local mechanical properties such as hardness and elasticity. These quantities are determined for the first time directly on the superalloys CMSX-6 and Waspaloy for the {gamma}{prime} and matrix phases, separately. The {gamma}{prime} phase in both alloys shows a significantly higher but different hardness than the matrix phase, whereas the moduli of elasticity are similar. A depth dependence of the hardness was found for very small indentations.

  13. Homogeneity, Modulus and Viscoelasticity of Polyelectrolyte Multilayers by Nano-Indentation: Refining the Buildup Mechanism

    PubMed Central

    Lehaf, Ali M.; Hariri, Haifa H.; Schlenoff, Joseph B.

    2012-01-01

    Atomic force microscopy, AFM, and nanoindentation of polyelectrolyte multilayers, PEMUs, made from poly(diallyldimethylammonium), PDADMA, and poly(styrene sulfonate), PSS, provided new insight into their surface morphology and growth mechanism. A strong odd/even alternation of surface modulus revealed greater extrinsic (counterion-balanced) charge compensation for fully hydrated multilayers ending in the polycation, PDADMA. These swings in modulus indicate a much more asymmetric layer-by-layer growth mechanism than previously proposed. Viscoelastic properties of the PEMU, which may contribute to cell response, were highlighted by variable indentation rates and minimized by extrapolating to zero indentation rate, at which point the surface and bulk equilibrium moduli were comparable. Variations in surface composition were probed at high resolution using force mapping and the surface was found to be uniform, with no evidence of phase separation. AFM comparison of wet and dry films terminated with PSS and PDADMA revealed much greater swelling of the PDADMA-terminated PEMU by water, with collapse of surface roughness features in dry conditions. Dynamic and static contact angle measurements suggested less rearrangement for the glassy PSS surface. PMID:22480307

  14. Evaluation and analysis of polished fused silica subsurface quality by the nanoindenter technique

    SciTech Connect

    Ma Bin; Shen Zhengxiang; He Pengfei; Sha Fei; Wang Chunliang; Wang Bin; Ji Yiqin; Liu Huasong; Li Weihao; Wang Zhanshan

    2011-03-20

    We evaluate the subsurface quality of polished fused silica samples using the nanoindenter technique. Two kinds of samples, consisting of hundreds of nanometers and micrometers of subsurface damage layers, are fabricated by controlling the grinding and polishing processes, and the subsurface quality has been verified by the chemical etching method. Then several nanoindentation experiments are performed using the Berkovich tip to investigate the subsurface quality. Some differences are found by relative measurements in terms of the relationship between the total penetration and the peak load on the surfaces, the modulus calculated over the defined depths and from unload, and the indented morphology at a constant load near the surface collapse threshold. Finally, the capabilities of such a mechanical method for detecting subsurface flaws are discussed and analyzed.

  15. AFM investigation of Martian soil simulants on micromachined Si substrates.

    PubMed

    Vijendran, S; Sykulska, H; Pike, W T

    2007-09-01

    The micro and nanostructures of Martian soil simulants with particles in the micrometre-size range have been studied using a combination of optical and atomic force microscopy (AFM) in preparation for the 2007 NASA Phoenix Mars Lander mission. The operation of an atomic force microscope on samples of micrometre-sized soil particles is a poorly investigated area where the unwanted interaction between the scanning tip and loose particles results in poor image quality and tip contamination by the sample. In order to mitigate these effects, etched silicon substrates with a variety of features have been used to facilitate the sorting and gripping of particles. From these experiments, a number of patterns were identified that were particularly good at isolating and immobilizing particles for AFM imaging. This data was used to guide the design of micromachined substrates for the Phoenix AFM. Both individual particles as well as aggregates were successfully imaged, and information on sizes, shapes and surface morphologies were obtained. This study highlights both the strengths and weaknesses of AFM for the potential in situ investigation of Martian soil and dust. Also presented are more general findings of the limiting operational constraints that exist when attempting the AFM of high aspect ratio particles with current technology. The performance of the final designs of the substrates incorporated on Phoenix will be described in a later paper. PMID:17760618

  16. The strength characterization of Al/Si interfaces with a hybrid nanoindentation/FEM method

    NASA Astrophysics Data System (ADS)

    Xia, Shuman; Qi, Yue; Perry, Thomas A.; Kim, Kyung-Suk

    2008-03-01

    The mechanical property characterization of the reinforcement/matrix interface in a metal matrix composite (MMC) is entailed for tailoring the interface in the microstructure design of the composite. In this work we developed a hybrid method to characterize the interface strength of an MMC, combining a nanoindentation experiment and a finite element analysis. The nanoindentation experiment was carried out by indenting individual reinforcement particles on a free surface with a nanoindenter. The dependence of indentation response on the interface properties was systematically studied through the finite element analysis with cohesive zone modeling of the interface failure. The interface strength could then be extracted from the comparison between the experimental and FEM results. With this method, the shear strength of an Al/Si interface was measured approximately 240MPa which compares well with the lower bound of an atomistic simulation with a modified EAM potential. The intrinsic fracture toughness of the interface crack tip surrounded by densely populated dislocations was measured 0.25 J/m2. We also studied the effect of the strontium modification on the interface strength with this hybrid method.

  17. A new view of the onset of plasticity during the nanoindentation of aluminium.

    PubMed

    Minor, Andrew M; Asif, S A Syed; Shan, Zhiwei; Stach, Eric A; Cyrankowski, Edward; Wyrobek, Thomas J; Warren, Oden L

    2006-09-01

    In nanoscale contact experiments, it is generally believed that the shear stress at the onset of plasticity can approach the theoretical shear strength of an ideal, defect-free lattice, a trend also observed in idealized molecular dynamics simulations. Here we report direct evidence that plasticity in a dislocation-free volume of polycrystalline aluminium can begin at very small forces, remarkably, even before the first sustained rise in repulsive force. However, the shear stresses associated with these very small forces do approach the theoretical shear strength of aluminium (approximately 2.2 GPa). Our observations entail correlating quantitative load-displacement measurements with individual video frames acquired during in situ nanoindentation experiments in a transmission electron microscope. We also report direct evidence that a submicrometre grain of aluminium plastically deformed by nanoindentation to a dislocation density of approximately 10(14) m(-2) is also capable of supporting shear stresses close to the theoretical shear strength. This result is contrary to earlier assumptions that a dislocation-free volume is necessary to achieve shear stresses near the theoretical shear strength of the material. Moreover, our results in entirety are at odds with the prevalent notion that the first obvious displacement excursion in a nanoindentation test is indicative of the onset of plastic deformation. PMID:16906139

  18. Charging C60 islands with the AFM tip.

    PubMed

    Hoff, Brice; Henry, Claude R; Barth, Clemens

    2016-01-01

    We show that electrons can be transferred on demand from an AFM tip into single bulk-like C60 islands, which are supported on the insulating NaCl(001) surface. We exemplify this by controlled charge-manipulation experiments conducted in ultrahigh vacuum by noncontact AFM (nc-AFM), electrostatic force microscopy (EFM) and Kelvin probe force microscopy (KPFM). KPFM shows a homogeneous contrast at the islands, which is a signature for an equal distribution of the electrons in the T1u band. The charge dissipates during half a day due to an interaction of the charged C60 islands with defects in the near surface region of NaCl. Our results open the perspective in photo-voltaics to study charge attachment, stability and charge exchange with the environment of any C60 bulk-like system. PMID:26617348

  19. Charging C60 islands with the AFM tip

    NASA Astrophysics Data System (ADS)

    Hoff, Brice; Henry, Claude R.; Barth, Clemens

    2015-12-01

    We show that electrons can be transferred on demand from an AFM tip into single bulk-like C60 islands, which are supported on the insulating NaCl(001) surface. We exemplify this by controlled charge-manipulation experiments conducted in ultrahigh vacuum by noncontact AFM (nc-AFM), electrostatic force microscopy (EFM) and Kelvin probe force microscopy (KPFM). KPFM shows a homogeneous contrast at the islands, which is a signature for an equal distribution of the electrons in the T1u band. The charge dissipates during half a day due to an interaction of the charged C60 islands with defects in the near surface region of NaCl. Our results open the perspective in photo-voltaics to study charge attachment, stability and charge exchange with the environment of any C60 bulk-like system.We show that electrons can be transferred on demand from an AFM tip into single bulk-like C60 islands, which are supported on the insulating NaCl(001) surface. We exemplify this by controlled charge-manipulation experiments conducted in ultrahigh vacuum by noncontact AFM (nc-AFM), electrostatic force microscopy (EFM) and Kelvin probe force microscopy (KPFM). KPFM shows a homogeneous contrast at the islands, which is a signature for an equal distribution of the electrons in the T1u band. The charge dissipates during half a day due to an interaction of the charged C60 islands with defects in the near surface region of NaCl. Our results open the perspective in photo-voltaics to study charge attachment, stability and charge exchange with the environment of any C60 bulk-like system. Electronic supplementary information (ESI) available. See DOI: 10.1039/C5NR04541J

  20. Poroelastic response of articular cartilage by nanoindentation creep tests at different characteristic lengths.

    PubMed

    Taffetani, M; Gottardi, R; Gastaldi, D; Raiteri, R; Vena, P

    2014-07-01

    Nanoindentation is an experimental technique which is attracting increasing interests for the mechanical characterization of articular cartilage. In particular, time dependent mechanical responses due to fluid flow through the porous matrix can be quantitatively investigated by nanoindentation experiments at different penetration depths and/or by using different probe sizes. The aim of this paper is to provide a framework for the quantitative interpretation of the poroelastic response of articular cartilage subjected to creep nanoindentation tests. To this purpose, multiload creep tests using spherical indenters have been carried out on saturated samples of mature bovine articular cartilage achieving two main quantitative results. First, the dependence of indentation modulus in the drained state (at equilibrium) on the tip radius: a value of 500 kPa has been found using the large tip (400 μm radius) and of 1.7 MPa using the smaller one (25 μm). Secon, the permeability at microscopic scale was estimated at values ranging from 4.5×10(-16) m(4)/N s to 0.1×10(-16) m(4)/N s, from low to high equivalent deformation. Consistently with a poroelastic behavior, the size-dependent response of the indenter displacement disappears when characteristic size and permeability are accounted for. For comparison purposes, the same protocol was applied to intrinsically viscoelastic homogeneous samples of polydimethylsiloxane (PDMS): both indentation modulus and time response have been found size-independent. PMID:24814573

  1. Novel Polymer Linkers for Single Molecule AFM Force Spectroscopy

    PubMed Central

    Tong, Zenghan; Mikheikin, Andrey; Krasnoslobodtsev, Alexey; Lv, Zhengjian; Lyubchenko, Yuri L.

    2013-01-01

    Flexible polymer linkers play an important role in various imaging and probing techniques that require surface immobilization, including atomic force microscopy (AFM). In AFM force spectroscopy, polymer linkers are necessary for the covalent attachment of molecules of interest to the AFM tip and the surface. The polymer linkers tether the molecules and provide their proper orientation in probing experiments. Additionally, the linkers separate specific interactions from nonspecific short-range adhesion and serve as a reference point for the quantitative analysis of single molecule probing events. In this report, we present our results on the synthesis and testing of a novel polymer linker and the identification of a number of potential applications for its use in AFM force spectroscopy experiments. The synthesis of the linker is based on the well-developed phosphoramidate (PA) chemistry that allows the routine synthesis of linkers with predetermined lengths and PA composition. These linkers are homogeneous in length and can be terminated with various functional groups. PA linkers with different functional groups were synthesized and tested in experimental systems utilizing different immobilization chemistries. We probed interactions between complementary DNA oligonucleotides; DNA and protein complexes formed by the site-specific binding protein SfiI; and interactions between amyloid peptide (Aβ42). The results of the AFM force spectroscopy experiments validated the feasibility of the proposed approach for the linker design and synthesis. Furthermore, the properties of the tether (length, functional groups) can be adjusted to meet the specific requirements for different force spectroscopy experiments and system characteristics, suggesting that it could be used for a large number of various applications. PMID:23624104

  2. Mechanical characterization of Lipon films using nanoindentation

    SciTech Connect

    Herbert, Erik; Tenhaeff, Wyatt E; Dudney, Nancy J; Pharr, V, George M

    2011-01-01

    Nanoindentation has been used to characterize the elastic modulus and hardness of LiPON films ranging in thickness from 1 to 10 m. Four fully dense, amorphous films were deposited on glass and sapphire substrates with one film annealed at 200 C for 20 min. The modulus of LiPON is found to be approximately 77 GPa, and argued to be independent of the substrate type, film thickness, and annealing. Based on the numerical analysis of Monroe and Newman, this value may be sufficiently high to mechanically suppress dendrite formation at the lithium/LiPON interface in thin film batteries [1]. Using Sneddon's stiffness equation and assuming the modulus is 77 GPa, the hardness is found to be approximately 3.9 GPa for all but the annealed film. The hardness of the annealed film is approximately 5% higher, at 4.1 GPa. Atomic force microscopy images of the residual hardness impressions confirm the unexpected increase in hardness of the annealed film. Surprisingly, the indentation data also reveal time-dependent behavior in all four films. This indicates that creep may also play a significant role in determining how LiPON responds to complex loading conditions and could be important in relieving stresses as they develop during service.

  3. Conductive supports for combined AFM SECM on biological membranes

    NASA Astrophysics Data System (ADS)

    Frederix, Patrick L. T. M.; Bosshart, Patrick D.; Akiyama, Terunobu; Chami, Mohamed; Gullo, Maurizio R.; Blackstock, Jason J.; Dooleweerdt, Karin; de Rooij, Nico F.; Staufer, Urs; Engel, Andreas

    2008-09-01

    Four different conductive supports are analysed regarding their suitability for combined atomic force and scanning electrochemical microscopy (AFM-SECM) on biological membranes. Highly oriented pyrolytic graphite (HOPG), MoS2, template stripped gold, and template stripped platinum are compared as supports for high resolution imaging of reconstituted membrane proteins or native membranes, and as electrodes for transferring electrons from or to a redox molecule. We demonstrate that high resolution topographs of the bacterial outer membrane protein F can be recorded by contact mode AFM on all four supports. Electrochemical feedback experiments with conductive cantilevers that feature nanometre-scale electrodes showed fast re-oxidation of the redox couple Ru(NH3)63+/2+ with the two metal supports after prolonged immersion in electrolyte. In contrast, the re-oxidation rates decayed quickly to unpractical levels with HOPG or MoS2 under physiological conditions. On HOPG we observed heterogeneity in the re-oxidation rate of the redox molecules with higher feedback currents at step edges. The latter results demonstrate the capability of conductive cantilevers with small electrodes to measure minor variations in an SECM signal and to relate them to nanometre-scale features in a simultaneously recorded AFM topography. Rapid decay of re-oxidation rate and surface heterogeneity make HOPG or MoS2 less attractive for combined AFM-SECM experiments on biological membranes than template stripped gold or platinum supports.

  4. Eliminating adhesion errors in nanoindentation of compliant polymers and hydrogels.

    PubMed

    Kohn, Julie C; Ebenstein, Donna M

    2013-04-01

    Nanoindentation is a valuable tool for characterization of biomaterials due to its ability to measure local properties in heterogeneous, small or irregularly shaped samples. However, applying nanoindentation to compliant, hydrated biomaterials leads to many challenges including adhesion between the nanoindenter tip and the sample. Although adhesion leads to overestimation of the modulus of compliant samples when analyzing nanoindentation data using traditional analysis techniques, most studies of biomaterials have ignored its effects. This paper demonstrates two methods for managing adhesion in nanoindentation analysis, the nano-JKR force curve method and the surfactant method, through application to two biomedically-relevant compliant materials, poly(dimethyl siloxane) (PDMS) elastomers and poly(ethylene glycol) (PEG) hydrogels. The nano-JKR force curve method accounts for adhesion during data analysis using equations based on the Johnson-Kendall-Roberts (JKR) adhesion model, while the surfactant method eliminates adhesion during data collection, allowing data analysis using traditional techniques. In this study, indents performed in air or water resulted in adhesion between the tip and the sample, while testing the same materials submerged in Optifree Express(®) contact lens solution eliminated tip-sample adhesion in most samples. Modulus values from the two methods were within 7% of each other, despite different hydration conditions and evidence of adhesion. Using surfactant also did not significantly alter the properties of the tested material, allowed accurate modulus measurements using commercial software, and facilitated nanoindentation testing in fluids. This technique shows promise for more accurate and faster determination of modulus values from nanoindentation of compliant, hydrated biological samples. PMID:23517775

  5. Single ricin detection by AFM chemomechanical mapping

    Technology Transfer Automated Retrieval System (TEKTRAN)

    This research reports a method of detecting ricin molecules immobilized on chemically modified gold (Au;111) surface by chemomechanically mapping the molecular interactions with a chemically modified Atomic Force Microscope (AFM) tip. AFM images resolved the different fold-up conformations of single...

  6. Nanoindentation of virus capsids in a molecular model

    NASA Astrophysics Data System (ADS)

    Cieplak, Marek; Robbins, Mark O.

    2010-01-01

    A molecular-level model is used to study the mechanical response of empty cowpea chlorotic mottle virus (CCMV) and cowpea mosaic virus (CPMV) capsids. The model is based on the native structure of the proteins that constitute the capsids and is described in terms of the Cα atoms. Nanoindentation by a large tip is modeled as compression between parallel plates. Plots of the compressive force versus plate separation for CCMV are qualitatively consistent with continuum models and experiments, showing an elastic region followed by an irreversible drop in force. The mechanical response of CPMV has not been studied, but the molecular model predicts an order of magnitude higher stiffness and a much shorter elastic region than for CCMV. These large changes result from small structural changes that increase the number of bonds by only 30% and would be difficult to capture in continuum models. Direct comparison of local deformations in continuum and molecular models of CCMV shows that the molecular model undergoes a gradual symmetry breaking rotation and accommodates more strain near the walls than the continuum model. The irreversible drop in force at small separations is associated with rupturing nearly all of the bonds between capsid proteins in the molecular model, while a buckling transition is observed in continuum models.

  7. Nanoindentation mapping of a wood-adhesive bond

    NASA Astrophysics Data System (ADS)

    Konnerth, J.; Valla, A.; Gindl, W.

    2007-08-01

    A mapping experiment of a wood phenol-resorcinol-formaldehyde adhesive bond was performed by means of grid nanoindentation. The variability of the modulus of elasticity and the hardness was evaluated for an area of 17 μm by 90 μm. Overall, the modulus of elasticity of the adhesive was clearly lower than the modulus of wood cell walls, whereas the hardness of the adhesive was slightly higher compared to cell walls. A very slight trend of decreasing modulus of elasticity was found with increasing distance from the immediate bond line. However, the trend was superimposed by a high variability of the modulus of elasticity in dependence on the position in the wood cell wall. The unexpectedly high variation of the modulus between 12 and 24 GPa may be explained by the interaction between the helical orientation of the cellulose microfibrils in the S2 layer of the wood cell wall and the geometry of the three-sided Berkovich type indenter pyramid used. Corresponding to the very slight decrease in modulus with increasing distance from the bond line, a similar but clearer trend was found for hardness. Both trends of changing mechanical properties of wood cell walls with varying distance from the bond line are attributed to effects of adhesive penetration into the wood cell wall.

  8. Nanoindentation of virus capsids in a molecular model.

    PubMed

    Cieplak, Marek; Robbins, Mark O

    2010-01-01

    A molecular-level model is used to study the mechanical response of empty cowpea chlorotic mottle virus (CCMV) and cowpea mosaic virus (CPMV) capsids. The model is based on the native structure of the proteins that constitute the capsids and is described in terms of the C(alpha) atoms. Nanoindentation by a large tip is modeled as compression between parallel plates. Plots of the compressive force versus plate separation for CCMV are qualitatively consistent with continuum models and experiments, showing an elastic region followed by an irreversible drop in force. The mechanical response of CPMV has not been studied, but the molecular model predicts an order of magnitude higher stiffness and a much shorter elastic region than for CCMV. These large changes result from small structural changes that increase the number of bonds by only 30% and would be difficult to capture in continuum models. Direct comparison of local deformations in continuum and molecular models of CCMV shows that the molecular model undergoes a gradual symmetry breaking rotation and accommodates more strain near the walls than the continuum model. The irreversible drop in force at small separations is associated with rupturing nearly all of the bonds between capsid proteins in the molecular model, while a buckling transition is observed in continuum models. PMID:20078182

  9. Hydrodynamic effects in fast AFM single-molecule force measurements.

    PubMed

    Janovjak, Harald; Struckmeier, Jens; Müller, Daniel J

    2005-02-01

    Atomic force microscopy (AFM) allows the critical forces that unfold single proteins and rupture individual receptor-ligand bonds to be measured. To derive the shape of the energy landscape, the dynamic strength of the system is probed at different force loading rates. This is usually achieved by varying the pulling speed between a few nm/s and a few microm/s, although for a more complete investigation of the kinetic properties higher speeds are desirable. Above 10 microm/s, the hydrodynamic drag force acting on the AFM cantilever reaches the same order of magnitude as the molecular forces. This has limited the maximum pulling speed in AFM single-molecule force spectroscopy experiments. Here, we present an approach for considering these hydrodynamic effects, thereby allowing a correct evaluation of AFM force measurements recorded over an extended range of pulling speeds (and thus loading rates). To support and illustrate our theoretical considerations, we experimentally evaluated the mechanical unfolding of a multi-domain protein recorded at 30 microm/s pulling speed. PMID:15257425

  10. Investigation of Oxidation Profile in PMR-15 Polyimide using Atomic Microscope (AFM)

    NASA Technical Reports Server (NTRS)

    Meador, Mary Ann B.; Johnson, Lili L.; Eby, R. K.

    2002-01-01

    Nanoindentation measurements are made on thermosetting materials using cantiever deflection vs. piezoelectric scanner position behavior determined by AFM. The spring model is used to determine mechanical properties of materials. The generalized Sneddon's equation is utilized to calculate Young's moduli for thermosetting materials at ambient conditions. Our investigations show that the force-penetration depth curves during unloading in these materials can be described accurately by a power law relationship. The results show that the accuracy of the measurements can be controlled within 7%. The above method is used to study oxidation profiles in Pl\\1R-15 polyimide. The thermo-mechanical profiles ofPNIR-15 indicate that the elastic modulus at the surface portion of the specimen is different from that at the interior of the material. It is also shown that there are two zones within the oxidized portion of the samples. Results confirm that the surface layer and the core material have substantially different properties.

  11. ezAFM: A low cost Atomic Force Microscope(AFM)

    NASA Astrophysics Data System (ADS)

    Celik, Umit; Celik, Kubra; Aslan, Husnu; Kehribar, Ihsan; Dede, Munir; Ozgur Ozer, H.; Oral, Ahmet

    2012-02-01

    A low cost AFM, ezAFM is developed for educational purposes as well as research. Optical beam deflection method is used to measure the deflection of cantilever. ezAFM scanner is built using voice coil motors (VCM) with ˜50x50x6 μm scan area. The microscope uses alignment free cantilevers, which minimizes setup times. FPGA based AFM feedback Control electronics is developed. FPGA technology allows us to drive all peripherals in parallel. ezAFM Controller is connected to PC by USB 2.0 interface as well as Wi-Fi. We have achieved <5nm lateral and ˜0.01nm vertical resolution. ezAFM can image single atomic steps in HOPG and mica. An optical microscope with <3 μm resolution is also integrated into the system. ezAFM supports different AFM operation modes such as dynamic mode, contact mode, lateral force microscopy. Advanced modes like magnetic force microscopy and electric force microscopy will be implemented later on. The new ezAFM system provides, short learning times for student labs, quick setup and easy to transport for portable applications with the best price/performance ratio. The cost of the system starts from 15,000, with system performance comparable with the traditional AFM systems.

  12. Strengthening and softening of nanocrystalline nickel during multistep nanoindentation

    SciTech Connect

    Nieh, Tai-Gang; Pan, D; Chen, Ming-Wei

    2006-04-01

    Multistep load-unload nanoindentation was employed to address the effect of deformation-induced microstructural evolution on mechanical behavior of nanocrystalline Ni. Deformation discontinuity was deliberately introduced by unloading-reloading during nanoindentation testing, which allows us to examine the influence of microstructural evolution on the successive deformation. Strain strengthening/softening of nanocrystalline nickel, associated with the transition of deformation behavior from dislocation activity at high loading rates to a grain-boundary-mediated process at low loading rates, was uncovered by means of this experimental methodology.

  13. MOS-based nanocapacitor using C-AFM

    NASA Astrophysics Data System (ADS)

    Hill, Daniel; Sadewasser, Sascha; Aymerich, Xavier

    2003-04-01

    This report details the attempts made to realise nanocapacitors for nanoscale MOS based integrated circuits by AFM anodic oxidation, and therefore isolation, of nano-sized squares of poly-silicon, titanium and aluminium on Si/SiO2. Conductive AFM (C-AFM) was used to perform topographical and electrical characterisation. The experiments were performed with contact mode C-AFM, in ambient air, using Pt-Ir, Co-Cr and Ti coated (20nm) n-type silicon cantilevers. Each sample consisted of a 3-5nm thick conductor deposited on 6nm of SiO2, which was thermally grown on Phosphorus doped (1019 cm-3) n-type Si(100) substrates. Standard cleaning and passivation processes were used. Poly-silicon was immediately found to be too rough to oxidise. Initial current-voltage measurements inside of the titanium-oxide squares suggest initial isolation followed by degradation through Fowler-Nordheim tunnelling. Measurement inconsistencies seen suggest charge storage on the surface or tip with the barrier height of the native titanium oxide thought to be responsible. Al has a thicker natural oxide. To overcome this we designed a series of structures consisting of a Ti finger on SiO2, that is connected to a Ti bond pad, allowing direct probing by a semiconductor parameter analyser. AFM anodic oxidation was performed upon these Ti fingers to reduce their in-plane dimensions towards the nanoscale. To confirm the existence of a nanocapacitor topographical and electrical measurements were then done on and around them.

  14. Nano Mechanical Machining Using AFM Probe

    NASA Astrophysics Data System (ADS)

    Mostofa, Md. Golam

    Complex miniaturized components with high form accuracy will play key roles in the future development of many products, as they provide portability, disposability, lower material consumption in production, low power consumption during operation, lower sample requirements for testing, and higher heat transfer due to their very high surface-to-volume ratio. Given the high market demand for such micro and nano featured components, different manufacturing methods have been developed for their fabrication. Some of the common technologies in micro/nano fabrication are photolithography, electron beam lithography, X-ray lithography and other semiconductor processing techniques. Although these methods are capable of fabricating micro/nano structures with a resolution of less than a few nanometers, some of the shortcomings associated with these methods, such as high production costs for customized products, limited material choices, necessitate the development of other fabricating techniques. Micro/nano mechanical machining, such an atomic force microscope (AFM) probe based nano fabrication, has, therefore, been used to overcome some the major restrictions of the traditional processes. This technique removes material from the workpiece by engaging micro/nano size cutting tool (i.e. AFM probe) and is applicable on a wider range of materials compared to the photolithographic process. In spite of the unique benefits of nano mechanical machining, there are also some challenges with this technique, since the scale is reduced, such as size effects, burr formations, chip adhesions, fragility of tools and tool wear. Moreover, AFM based machining does not have any rotational movement, which makes fabrication of 3D features more difficult. Thus, vibration-assisted machining is introduced into AFM probe based nano mechanical machining to overcome the limitations associated with the conventional AFM probe based scratching method. Vibration-assisted machining reduced the cutting forces

  15. Analytical model for nanoscale viscoelastic properties characterization using dynamic nanoindentation

    NASA Astrophysics Data System (ADS)

    Yuya, Philip A.; Patel, Nimitt G.

    2014-08-01

    In the last few decades, nanoindentation has gained widespread acceptance as a technique for materials properties characterization at micron and submicron length scales. Accurate and precise characterization of material properties with a nanoindenter is critically dependent on the ability to correctly model the response of the test equipment in contact with the material. In dynamic nanoindention analysis, a simple Kelvin-Voigt model is commonly used to capture the viscoelastic response. However, this model oversimplifies the response of real viscoelastic materials such as polymers. A model is developed that captures the dynamic nanoindentation response of a viscoelastic material. Indenter tip-sample contact forces are modelled using a generalized Maxwell model. The results on a silicon elastomer were analysed using conventional two element Kelvin-Voigt model and contrasted to analysis done using the Maxwell model. The results show that conventional Kelvin-Voigt model overestimates the storage modulus of the silicone elastomer by ~30%. Maxwell model represents a significant improvement in capturing the viscoelastic material behaviour over the Voigt model.

  16. In situ nanoindentation in a transmission electron microscope

    SciTech Connect

    Minor, Andrew M.

    2002-12-02

    This dissertation presents the development of the novel mechanical testing technique of in situ nanoindentation in a transmission electron microscope (TEM). This technique makes it possible to simultaneously observe and quantify the mechanical behavior of nano-scale volumes of solids.

  17. New topics on nanoindentation of polymers and composite materials

    NASA Astrophysics Data System (ADS)

    Martinez Hernandez, Ricardo

    In this study, nanoindentation was used to determine Young's modulus of homogeneous plastic materials as well as inhomogeneous epoxy woven fabric composites using various indenters. In the first part, homogeneous PMMA and polycarbonate were characterized using conical and spherical indenters. The conventional approach of the inverse analysis was modified in order to account for effects obtained during spherical nanoindentation. The experimental results were verified using FEA analysis in ABAQUS. It was found that viscous effects were present in conical nanoindentations which led to an overestimation of contact stiffness. The second part, the response of carbon and glass fiber woven fabric epoxy composites was investigated using Berkovich and spherical indenters. Localized nanoindentation was performed using the Berkovich probe in both materials which led to determination of glass fibers and matrix stiffnesses. The anisotropic nature of the response was treated modifying the classical approach to calculate transverse modulus of a unidirectional composite. Finally, fiber volume ratios were calculated according to type of composite and indenter used.

  18. Modulated Nanoindentation (MoNI) - a novel characterization tool of two-dimensional materials and nanotubes

    NASA Astrophysics Data System (ADS)

    Gao, Yang; Kim, Suenne; Zhou, Si; Chiu, Hsiang-Chih; Nelias, Daniel; Berger, Claire; de Heer, Walt; Polloni, Laura; Sordan, Roman; Klinke, Christian; Bongiorno, Angelo; Riedo, Elisa

    We report on a novel Atomic Force Microscopy (AFM) based technique with sub-angstrom vertical resolution - Modulated Nanoindentation (MoNI). MoNI has been applied to measure the radial elasticity of multi-walled nanotubes. Recently the interlayer coupling of two-dimensional materials (such as graphene and MoS2) characterized by strong in-plane bonds and weak interlayer interactions has been studied by MoNI combined with semi-analytical methods (SAM) and DFT calculations. The out-of-plane stiffness of varied 2D materials and its dependence on number of layers and intercalated water has been investigated in different environmental conditions. This non-destructive technique provides a new path to study the interlayer elastic coupling and the Van der Waals forces in few-layer-thick 2D materials, offering the possibility to understand how interlayer coupling is related to the electronic, phononic, and thermal properties of 2D materials. Y. Gao et al ., Nature Materials 14 , 714-720 (2015).

  19. Nanoindentation of 35 Virus Capsids in a Molecular Model: Relating Mechanical Properties to Structure

    PubMed Central

    2013-01-01

    A coarse-grained model is used to study the mechanical response of 35 virus capsids of symmetries T = 1, T = 2, T = 3, pseudo T = 3, T = 4, and T = 7. The model is based on the native structure of the proteins that constitute the capsids and is described in terms of the C atoms associated with each amino acid. The number of these atoms ranges between 8 460 (for SPMV – satellite panicum mosaic virus) and 135 780 (for NBV – nudaureli virus). Nanoindentation by a broad AFM tip is modeled as compression between two planes: either both flat or one flat and one curved. Plots of the compressive force versus plate separation show a variety of behaviors, but in each case there is an elastic region which extends to a characteristic force . Crossing results in a drop in the force and irreversible damage. Across the 35 capsids studied, both and the elastic stiffness are observed to vary by a factor of 20. The changes in mechanical properties do not correlate simply with virus size or symmetry. There is a strong connection to the mean coordination number , defined as the mean number of interactions to neighboring amino acids. The Young's modulus for thin shell capsids rises roughly quadratically with , where 6 is the minimum coordination for elastic stability in three dimensions. PMID:23785395

  20. Nanoindentation of 35 virus capsids in a molecular model: relating mechanical properties to structure.

    PubMed

    Cieplak, Marek; Robbins, Mark O

    2013-01-01

    A coarse-grained model is used to study the mechanical response of 35 virus capsids of symmetries T = 1, T = 2, T = 3, pseudo T = 3, T = 4, and T = 7. The model is based on the native structure of the proteins that constitute the capsids and is described in terms of the C[Formula: see text] atoms associated with each amino acid. The number of these atoms ranges between 8 460 (for SPMV - satellite panicum mosaic virus) and 135 780 (for NBV - nudaureli virus). Nanoindentation by a broad AFM tip is modeled as compression between two planes: either both flat or one flat and one curved. Plots of the compressive force versus plate separation show a variety of behaviors, but in each case there is an elastic region which extends to a characteristic force [Formula: see text]. Crossing [Formula: see text] results in a drop in the force and irreversible damage. Across the 35 capsids studied, both [Formula: see text] and the elastic stiffness are observed to vary by a factor of 20. The changes in mechanical properties do not correlate simply with virus size or symmetry. There is a strong connection to the mean coordination number [Formula: see text], defined as the mean number of interactions to neighboring amino acids. The Young's modulus for thin shell capsids rises roughly quadratically with [Formula: see text], where 6 is the minimum coordination for elastic stability in three dimensions. PMID:23785395

  1. Investigation of the Mechanoelectrical Transduction at Single Stereocilia by Afm

    NASA Astrophysics Data System (ADS)

    Langer, M. G.; Fink, S.; Löffler, K.; Koitschev, A.; Zenner, H.-P.

    2003-02-01

    The transduction of sound into an electrical signal in the inner ear is closely related to the mechanical properties of the hair bundles cytoskeleton and cross-linkage. In this study the effect of lateral cross-links on hair bundle mechanics and the transduction current response is demonstrated on the level of individual stereocilia. For experiments stereocilia of outer hair cells of postnatal rats (P3 - P8) were scanned with a sharp AFM tip at nanometerscale. Transduction currents were simultaneously recorded in the whole-cell-recording mode with patch clamp. AFM was used as a nanotool for local mechanical stimulation and force measurement at stereocilia whereas patch clamp serves as a detector for the electrical response of the cell. In a first experiment force transmission between adjacent stereocilia of the V- and W- shaped hair bundles of outer hair cells was investigated. Results showed that a force exerted to a single stereocilium declined to 36 % at the nearest adjacent stereocilium of the same row. This result supposes AFM to be convenient for local displacement of single stereocilia. For control, the local response of transduction channels was measured at single stereocilia of the same hair bundle. Measured transduction current amplitudes ranged from 9 to 49 pA supposing an opening of one to five transduction channels. Both, weak force transmission by lateral cross-links and small transduction current amplitudes indicate a weak mechanical interaction between individual stereocilia of the tallest row of stereocilia of outer hair cells from postnatal rats.

  2. Nano-Bio-Mechanics of Neuroblastoma Cells Using AFM

    NASA Astrophysics Data System (ADS)

    Bastatas, Lyndon; Matthews, James; Kang, Min; Park, Soyeun

    2011-10-01

    We have conducted an in vitro study to determine the elastic moduli of neurobalstoma cell lines using atomic force microscopy. Using a panel of cell lines established from neuroblastoma patients at different stages of disease progress and treatment, we have investigated the differences in elastic moduli during a course of cancer progression and chemotherapy. The cells were grown on the hard substrates that are chemically functionalized to enhance adhesion. We have performed the AFM indentation experiments with different applied forces from the AFM probe. For the purpose of the comparison between cell lines, the indentations were performed only on cell centers. The obtained force-distance curves were analyzed using the Hertz model in order to extract the elastic moduli. We have found that the elastic moduli of human neuroblastoma cells significantly varied during the disease progression. We postulate that the observed difference might be affected by the treatment and chemotherapy.

  3. Hydration states of AFm cement phases

    SciTech Connect

    Baquerizo, Luis G.; Matschei, Thomas; Scrivener, Karen L.; Saeidpour, Mahsa; Wadsö, Lars

    2015-07-15

    The AFm phase, one of the main products formed during the hydration of Portland and calcium aluminate cement based systems, belongs to the layered double hydrate (LDH) family having positively charged layers and water plus charge-balancing anions in the interlayer. It is known that these phases present different hydration states (i.e. varying water content) depending on the relative humidity (RH), temperature and anion type, which might be linked to volume changes (swelling and shrinkage). Unfortunately the stability conditions of these phases are insufficiently reported. This paper presents novel experimental results on the different hydration states of the most important AFm phases: monocarboaluminate, hemicarboaluminate, strätlingite, hydroxy-AFm and monosulfoaluminate, and the thermodynamic properties associated with changes in their water content during absorption/desorption. This data opens the possibility to model the response of cementitious systems during drying and wetting and to engineer systems more resistant to harsh external conditions.

  4. AFM indentation study of breast cancer cells

    SciTech Connect

    Li, Q.S.; Lee, G.Y.H.; Ong, C.N.; Lim, C.T.

    2008-10-03

    Mechanical properties of individual living cells are known to be closely related to the health and function of the human body. Here, atomic force microscopy (AFM) indentation using a micro-sized spherical probe was carried out to characterize the elasticity of benign (MCF-10A) and cancerous (MCF-7) human breast epithelial cells. AFM imaging and confocal fluorescence imaging were also used to investigate their corresponding sub-membrane cytoskeletal structures. Malignant (MCF-7) breast cells were found to have an apparent Young's modulus significantly lower (1.4-1.8 times) than that of their non-malignant (MCF-10A) counterparts at physiological temperature (37 deg. C), and their apparent Young's modulus increase with loading rate. Both confocal and AFM images showed a significant difference in the organization of their sub-membrane actin structures which directly contribute to their difference in cell elasticity. This change may have facilitated easy migration and invasion of malignant cells during metastasis.

  5. LET Spectrum Measurements In CR-39 PNTD With AFM

    NASA Astrophysics Data System (ADS)

    Johnson, C. E.; DeWitt, J. M.; Benton, E. R.; Yasuda, N.; Benton, E. V.

    2011-06-01

    Energetic protons, neutrons, and heavy ions undergoing collisions with target nuclei of varying Z can produce residual heavy recoil fragments via intra-nuclear cascade/evaporation reactions. The particles produced in these non-elastic collisions generally have such extremely short range (˜<10 μm) that they cannot be directly observed by conventional detection methods including CR-39 plastic nuclear track detector (PNTD) that has been chemically etched for analysis by standard visible light microscopy. However, high-LET recoil fragments having range on the order of several cell diameters can be produced in tissue during radiotherapy using proton and carbon beams. We have developed a method to analyze short-range, high-LET tracks in CR-39 plastic nuclear track detector (PNTD) using short duration chemical etching (˜<1 μm) following by automated atomic force microscope (AFM) scanning. The post-scan data processing used in this work was based on semi-automated matrix analysis opposed to traditional grey-scale image analysis. This method takes advantage of the 3-D data obtained via AFM to achieve robust discrimination of nuclear tracks from other features inherently present in the post-etch detector surface. Through automation of AFM scanning, sufficient AFM scan frames were obtained to attain an LET spectrum spanning the LET range from 200-1500 keV/μm. In addition to our experiments, simulations were carried out with the Monte Carlo transport code, FLUKA. To demonstrate this method, CR-39 PNTD was exposed to the proton therapy beam at Loma Linda University Medical Center (LLUMC) at 60 and 230 MeV. Additionally, detectors were exposed to 1 GeV protons at the NASA Space Radiation Laboratory (NSRL) at Brookhaven National Laboratory (BNL). For these exposures CR-39 PNTD, Al and Cu target foils were used between detector layers.

  6. LET Spectrum Measurements In CR-39 PNTD With AFM

    SciTech Connect

    Johnson, C. E.; DeWitt, J. M.; Benton, E. R.; Yasuda, N.; Benton, E. V.

    2011-06-01

    Energetic protons, neutrons, and heavy ions undergoing collisions with target nuclei of varying Z can produce residual heavy recoil fragments via intra-nuclear cascade/evaporation reactions. The particles produced in these non-elastic collisions generally have such extremely short range ({approx}<10 {mu}m) that they cannot be directly observed by conventional detection methods including CR-39 plastic nuclear track detector (PNTD) that has been chemically etched for analysis by standard visible light microscopy. However, high-LET recoil fragments having range on the order of several cell diameters can be produced in tissue during radiotherapy using proton and carbon beams. We have developed a method to analyze short-range, high-LET tracks in CR-39 plastic nuclear track detector (PNTD) using short duration chemical etching ({approx}<1 {mu}m) following by automated atomic force microscope (AFM) scanning. The post-scan data processing used in this work was based on semi-automated matrix analysis opposed to traditional grey-scale image analysis. This method takes advantage of the 3-D data obtained via AFM to achieve robust discrimination of nuclear tracks from other features inherently present in the post-etch detector surface. Through automation of AFM scanning, sufficient AFM scan frames were obtained to attain an LET spectrum spanning the LET range from 200-1500 keV/{mu}m. In addition to our experiments, simulations were carried out with the Monte Carlo transport code, FLUKA. To demonstrate this method, CR-39 PNTD was exposed to the proton therapy beam at Loma Linda University Medical Center (LLUMC) at 60 and 230 MeV. Additionally, detectors were exposed to 1 GeV protons at the NASA Space Radiation Laboratory (NSRL) at Brookhaven National Laboratory (BNL). For these exposures CR-39 PNTD, Al and Cu target foils were used between detector layers.

  7. Quantitative nano-mechanics of biological cells with AFM

    NASA Astrophysics Data System (ADS)

    Sokolov, Igor

    2013-03-01

    The importance of study of living cells is hard to overestimate. Cell mechanics is a relatively young, yet not a well-developed area. Besides just a fundamental interest, large practical need has emerged to measure cell mechanics quantitatively. Recent studies revealed a significant correlation between stiffness of biological cells and various human diseases, such as cancer, malaria, arthritis, and even aging. However, really quantitative studies of mechanics of biological cells are virtually absent. It is not even clear if the cell, being a complex and heterogeneous object, can be described by the elastic modulus at all. Atomic force microscopy (AFM) is a natural instrument to study properties of cells in their native environments. Here we will demonstrate that quantitative measurements of elastic modulus of cells with AFM are possible. Specifically, we will show that the ``cell body'' (cell without ``brush'' surface layer, a non-elastic layer surrounding cells) typically demonstrates the response of a homogeneous elastic medium up to the deformation of 10-20%, but if and only if a) the cellular brush layer is taken into account, b) rather dull AFM probes are used. This will be justified with the help of the strong condition of elastic behavior of material: the elastic modulus is shown to be independent on the indentation depth. We will also demonstrate that an attempt either to ignore the brush layer or to use sharp AFM probes will result in the violation of the strong condition, which implies impossibility to use the concept of the elastic modulus to describe cell mechanics in such experiments. Examples of quantitative measurements of the Young's modulus of the cell body and the cell brush parameters will be given for various cells. Address when submitting: Clarkson University, Potsdam, NY 13699

  8. LET spectrum measurements in Cr-39 PNTD with AFM

    SciTech Connect

    Johnson, Carl Edward; De Witt, Joel M; Benton, Eric R; Yasuda, Nakahiro; Benton, Eugene V

    2010-01-01

    Energetic protons, neutrons, and heavy ions undergoing collisions with target nuclei of varying Z can produce residual heavy recoil fragments via intra-nuclear cascade/evaporation reactions. The particles produced in these non-elastic collisions generally have such extremely short range ({approx}< 10 {mu}m) that they cannot be directly observed by conventional detection methods including CR-39 plastic nuclear track detector (PNTD) that has been chemically etched for analysis by standard visible light microscopy. However, high-LET recoil fragments having range on the order of several cell diameters can be produced in tissue during radiotherapy using proton and carbon beams. We have developed a method to analyze short-range, high-LET tracks in CR-39 plastic nuclear track detector (PNTD) using short duration chemical etching ({approx}< 1 {mu}m) followed by automated atomic force microscope (AFM) scanning. The post-scan data processing used in this work was based on semi-automated matrix analysis opposed to traditional grey-scale image analysis. This method takes advantage of the 3-D data obtained via AFM to achieve robust discrimination of nuclear tracks from other features. Through automation of AFM scanning, sufficient AFM scan frames were obtained to attain an LET spectrum spanning the LET range from 200-1500 keV/{mu}m. In addition to our experiments, simulations were carried out with the Monte Carlo transport code, FLUKA. To demonstrate this method, CR-39 PNTD was exposed to the proton therapy beam at Loma Linda University Medical Center (LLUMC) at 60 and 230 MeV. Additionally, detectors were exposed to I GeV protons at the NASA Space Radiation Laboratory (NSRL) at Brookhaven National Laboratory (BNL). For these exposures CR-39 PNTD, Al and Cu target foils were used between detector layers.

  9. Dislocation nucleation in bcc Ta single crystals studied by nanoindentation

    SciTech Connect

    Biener, M M; Biener, J; Hodge, A M; Hamza, A V

    2007-08-08

    The study of dislocation nucleation in closed-packed metals by nanoindentation has recently attracted much interest. Here, we address the peculiarities of the incipient plasticity in body centered cubic (bcc) metals using low index Ta single-crystals as a model system. The combination of nanoindentation with high-resolution atomic force microscopy provides us with experimental atomic-scale information on the process of dislocation nucleation and multiplication. Our results reveal a unique deformation behavior of bcc Ta at the onset of plasticity which is distinctly different from that of closed-packed metals. Most noticeable, we observe only one rather than a sequence of discontinuities in the load-displacement curves. This and other differences are discussed in context of the characteristic plastic deformation behavior of bcc metals.

  10. Pileup Behavior in Sharp Nanoindentation of AISI 1045 Steel

    NASA Astrophysics Data System (ADS)

    Zhu, L. N.; Xu, B. S.; Wang, H. D.; Wang, C. B.

    Experimental measurements have been used to investigate the pileup behavior during nanoindentation with a sharp indenter. The AISI 1045 steels treated by quenching and annealing were examined. The results show that during sharp nanoindentation process, the amount of pileup is related to the residual stress state, the indentation depth and the work hardening. The quenched steel with compressive residual stress will tend to pile up, and the stress-free annealed steel can decrease the pileup height. It is found that the pileup height gradually increases for the two steels as the indentation depth becomes larger. It is also shown that the low work hardening of the two steels can also result in the pileup deformation.

  11. Plastic deformation in zirconium nitride observed by nanoindentation and TEM

    NASA Astrophysics Data System (ADS)

    Egeland, G. W.; Wheeler, K.; Peralta, P.; McClellan, K. J.; Maloy, S. A.; Bond, G. M.

    2011-09-01

    A study on zirconium nitride using TEM and nanoindentation was performed to assess the significant surface plasticity found to be introduced by sample polishing. Cross-sectional TEM results show strong evidence of plasticity via dislocations produced directly from surface grinding and polishing. These dislocations were found to glide on the {0 1 1}<0 1¯ 1> slip system. Using nanoindentation to observe the effects of surface dislocation density, a critical shear stress was found that relates to dislocations nucleation and multiplication. Continued chemo-mechanical polishing increased the critical shear stress to approximately 1600 mN by reducing surface dislocations. It is postulated that vacancy clusters and oxide microcrystallites produced during surface processing provide dislocation nucleation and/or multiplication sites. Gentle chemo-mechanical polishing for several hours greatly reduced or eliminated preexisting dislocations such that the critical shear stress for nucleation approaches the theoretical limit (˜ G/5).

  12. Nano-indentation study on the (001) face of KDP crystal based on SPH method

    NASA Astrophysics Data System (ADS)

    Xiaoguang, Guo; Ziyuan, Liu; Hang, Gao; Dongming, Guo

    2015-08-01

    In order to avoid the defects of mesh distortion when dealing with large deformation problems through using the finite element method, a mess-free simulation method—smooth particle hydrodynamics (SPH) has been introduced. The material constitutive model of KDP crystal has been established based on the elastic-plastic theory. Then the nano-indentation on the (001) face of KDP crystal has been carried out using SPH method. Simulation results show that the maximum equivalent stress and the maximum plastic strain concentrate on the area that located near the tip of the indenter during the loading process. The distribution shape of Von Mises stress is similar to concentric circles. During the unloading process, no obvious variation of plastic strain distribution exists. The maximum Von Mises stress is mainly located at the indentation and its edge at the end of the unloading process. The approximate direct proportion relationship between the maximum indentation depth and the depth of the maximum Von Mises stress distribution has been discovered when the maximum load is lower than 8 mN. In addition, the nano-indentation experiments on KDP crystal's (001) face have been carried out. Both the material parameters and the adjusted stress-strain curve have been verified. The hindering role of the affected layer has been found and analyzed. Project supported by the National Basic Research Program of China (No. 51135002), and the Science Fund for Creative Research Groups (No. 51321004).

  13. Evaluation of irradiation hardening of proton irradiated stainless steels by nanoindentation

    NASA Astrophysics Data System (ADS)

    Yabuuchi, Kiyohiro; Kuribayashi, Yutaka; Nogami, Shuhei; Kasada, Ryuta; Hasegawa, Akira

    2014-03-01

    Ion irradiation experiments are useful for investigating irradiation damage. However, estimating the irradiation hardening of ion-irradiated materials is challenging because of the shallow damage induced region. Therefore, the purpose of this study is to prove usefulness of nanoindentation technique for estimation of irradiation hardening for ion-irradiated materials. SUS316L austenitic stainless steel was used and it was irradiated by 1 MeV H+ ions to a nominal displacement damage of 0.1, 0.3, 1, and 8 dpa at 573 K. The irradiation hardness of the irradiated specimens were measured and analyzed by Nix-Gao model. The indentation size effect was observed in both unirradiated and irradiated specimens. The hardness of the irradiated specimens changed significantly at certain indentation depths. The depth at which the hardness varied indicated that the region deformed by the indenter had reached the boundary between the irradiated and unirradiated regions. The hardness of the irradiated region was proportional to the inverse of the indentation depth in the Nix-Gao plot. The bulk hardness of the irradiated region, H0, estimated by the Nix-Gao plot and Vickers hardness were found to be related to each other, and the relationship could be described by the equation, HV = 0.76H0. Thus, the nanoindentation technique demonstrated in this study is valuable for measuring irradiation hardening in ion-irradiated materials.

  14. Thin film adhesion by nanoindentation-induced superlayers. Final report

    SciTech Connect

    Gerberich, William W.; Volinsky, A.A.

    2001-06-01

    This work has analyzed the key variables of indentation tip radius, contact radius, delamination radius, residual stress and superlayer/film/interlayer properties on nanoindentation measurements of adhesion. The goal to connect practical works of adhesion for very thin films to true works of adhesion has been achieved. A review of this work titled ''Interfacial toughness measurements of thin metal films,'' which has been submitted to Acta Materialia, is included.

  15. Conductance of AFM Deformed Carbon Nanotubes

    NASA Technical Reports Server (NTRS)

    Svizhenko, Alexei; Maiti, Amitesh; Anatram, M. P.; Biegel, Bryan (Technical Monitor)

    2002-01-01

    This viewgraph presentation provides information on the electrical conductivity of carbon nanotubes upon deformation by atomic force microscopy (AFM). The density of states and conductance were computed using four orbital tight-binding method with various parameterizations. Different chiralities develop bandgap that varies with chirality.

  16. Contact nanomechanical measurements with the AFM

    NASA Astrophysics Data System (ADS)

    Geisse, Nicholas

    2013-03-01

    The atomic force microscope (AFM) has found broad use in the biological sciences largely due to its ability to make measurements on unfixed and unstained samples under liquid. In addition to imaging at multiple spatial scales ranging from micro- to nanometer, AFMs are commonly used as nanomechanical probes. This is pertinent for cell biology, as it has been demonstrated that the geometrical and mechanical properties of the extracellular microenvironment are important in such processes as cancer, cardiovascular disease, muscular dystrophy, and even the control of cell life and death. Indeed, the ability to control and quantify these external geometrical and mechanical parameters arises as a key issue in the field. Because AFM can quantitatively measure the mechanical properties of various biological samples, novel insights to cell function and to cell-substrate interactions are now possible. As the application of AFM to these types of problems is widened, it is important to understand the performance envelope of the technique and its associated data analyses. This talk will discuss the important issues that must be considered when mechanical models are applied to real-world data. Examples of the effect of different model assumptions on our understanding of the measured material properties will be shown. Furthermore, specific examples of the importance of mechanical stimuli and the micromechanical environment to the structure and function of biological materials will be presented.

  17. A Batch Fabricated SECM-AFM Probe

    NASA Astrophysics Data System (ADS)

    Dobson, P. S.; Macpherson, J. V.; Holder, M.; Weaver, J. M. R.

    2003-12-01

    A scheme for the fabrication of combined Scanning Electrochemical Microscopy — Atomic Force Microscopy (SECM-AFM) probes is presented for both silicon nitride and silicon cantilevers. The advantages over exsisting methods used for their production is explained. The process flow is described and initial results from electrodeposition of silver are presented.

  18. A Multifunctional Frontloading Approach for Repeated Recycling of a Pressure-Controlled AFM Micropipette.

    PubMed

    Roder, Phillip; Hille, Carsten

    2015-01-01

    Fluid force microscopy combines the positional accuracy and force sensitivity of an atomic force microscope (AFM) with nanofluidics via a microchanneled cantilever. However, adequate loading and cleaning procedures for such AFM micropipettes are required for various application situations. Here, a new frontloading procedure is described for an AFM micropipette functioning as a force- and pressure-controlled microscale liquid dispenser. This frontloading procedure seems especially attractive when using target substances featuring high costs or low available amounts. Here, the AFM micropipette could be filled from the tip side with liquid from a previously applied droplet with a volume of only a few μL using a short low-pressure pulse. The liquid-loaded AFM micropipettes could be then applied for experiments in air or liquid environments. AFM micropipette frontloading was evaluated with the well-known organic fluorescent dye rhodamine 6G and the AlexaFluor647-labeled antibody goat anti-rat IgG as an example of a larger biological compound. After micropipette usage, specific cleaning procedures were tested. Furthermore, a storage method is described, at which the AFM micropipettes could be stored for a few hours up to several days without drying out or clogging of the microchannel. In summary, the rapid, versatile and cost-efficient frontloading and cleaning procedure for the repeated usage of a single AFM micropipette is beneficial for various application situations from specific surface modifications through to local manipulation of living cells, and provides a simplified and faster handling for already known experiments with fluid force microscopy. PMID:26636981

  19. A Multifunctional Frontloading Approach for Repeated Recycling of a Pressure-Controlled AFM Micropipette

    PubMed Central

    Roder, Phillip; Hille, Carsten

    2015-01-01

    Fluid force microscopy combines the positional accuracy and force sensitivity of an atomic force microscope (AFM) with nanofluidics via a microchanneled cantilever. However, adequate loading and cleaning procedures for such AFM micropipettes are required for various application situations. Here, a new frontloading procedure is described for an AFM micropipette functioning as a force- and pressure-controlled microscale liquid dispenser. This frontloading procedure seems especially attractive when using target substances featuring high costs or low available amounts. Here, the AFM micropipette could be filled from the tip side with liquid from a previously applied droplet with a volume of only a few μL using a short low-pressure pulse. The liquid-loaded AFM micropipettes could be then applied for experiments in air or liquid environments. AFM micropipette frontloading was evaluated with the well-known organic fluorescent dye rhodamine 6G and the AlexaFluor647-labeled antibody goat anti-rat IgG as an example of a larger biological compound. After micropipette usage, specific cleaning procedures were tested. Furthermore, a storage method is described, at which the AFM micropipettes could be stored for a few hours up to several days without drying out or clogging of the microchannel. In summary, the rapid, versatile and cost-efficient frontloading and cleaning procedure for the repeated usage of a single AFM micropipette is beneficial for various application situations from specific surface modifications through to local manipulation of living cells, and provides a simplified and faster handling for already known experiments with fluid force microscopy. PMID:26636981

  20. Pair vs many-body potentials: Influence on elastic and plastic behavior in nanoindentation of fcc metals

    NASA Astrophysics Data System (ADS)

    Ziegenhain, Gerolf; Hartmaier, Alexander; Urbassek, Herbert M.

    2009-09-01

    Molecular-dynamics simulation can give atomistic information on the processes occurring in nanoindentation experiments. In particular, the nucleation of dislocation loops, their growth, interaction and motion can be studied. We investigate how realistic the interatomic potentials underlying the simulations have to be in order to describe these complex processes. Specifically we investigate nanoindentation into a Cu single crystal. We compare simulations based on a realistic many-body interaction potential of the embedded-atom-method type with two simple pair potentials, a Lennard-Jones and a Morse potential. We find that qualitatively many aspects of nanoindentation are fairly well reproduced by the simple pair potentials: elastic regime, critical stress and indentation depth for yielding, dependence on the crystal orientation, and even the level of the hardness. The quantitative deficits of the pair potential predictions can be traced back: (i) to the fact that the pair potentials are unable in principle to model the elastic anisotropy of cubic crystals and (ii) as the major drawback of pair potentials we identify the gross underestimation of the stable stacking fault energy. As a consequence these potentials predict the formation of too large dislocation loops, the too rapid expansion of partials, too little cross slip and in consequence a severe overestimation of work hardening.

  1. Critical issues in making small-depth mechanical property measurements by nanoindentation with continuous stiffness measurement

    SciTech Connect

    Pharr, George Mathews; Strader, Jeremy H.; Oliver, W. C.

    2009-01-01

    Experiments were performed on a (100) copper single crystal to examine the influences that small displacement oscillations used in continuous stiffness measurement techniques have on hardness and elastic-modulus measurements in nanoindentation experiments. For the commonly used 2-nm oscillation, significant errors were observed in the measured properties, especially the hardness, at penetration depths as large as 100 nm. The errors originate from the large amount of dynamic unloading that occurs in materials like copper that have high contact stiffness resulting from their high modulus-to-hardness ratios. A simple model for the loading and unloading behavior of an elastic-plastic material is presented that quantitatively describes the errors and can be used to partially correct for them. By correcting the data in accordance with model and performing measurements at smaller displacement oscillation amplitudes, the errors can be reduced. The observations have important implications for the interpretation of the indentation size effect.

  2. Membrane-based actuation for high-speed single molecule force spectroscopy studies using AFM.

    PubMed

    Sarangapani, Krishna; Torun, Hamdi; Finkler, Ofer; Zhu, Cheng; Degertekin, Levent

    2010-07-01

    Atomic force microscopy (AFM)-based dynamic force spectroscopy of single molecular interactions involves characterizing unbinding/unfolding force distributions over a range of pulling speeds. Owing to their size and stiffness, AFM cantilevers are adversely affected by hydrodynamic forces, especially at pulling speeds >10 microm/s, when the viscous drag becomes comparable to the unbinding/unfolding forces. To circumvent these adverse effects, we have fabricated polymer-based membranes capable of actuating commercial AFM cantilevers at speeds >or=100 microm/s with minimal viscous drag effects. We have used FLUENT, a computational fluid dynamics (CFD) software, to simulate high-speed pulling and fast actuation of AFM cantilevers and membranes in different experimental configurations. The simulation results support the experimental findings on a variety of commercial AFM cantilevers and predict significant reduction in drag forces when membrane actuators are used. Unbinding force experiments involving human antibodies using these membranes demonstrate that it is possible to achieve bond loading rates >or=10(6) pN/s, an order of magnitude greater than that reported with commercial AFM cantilevers and systems. PMID:20054686

  3. Strength by atomic force microscopy (AFM): Molecular dynamics of water layer squeezing on magnesium oxide

    NASA Astrophysics Data System (ADS)

    Kendall, K.; Dhir, Aman; Yong, Chin W.

    2010-11-01

    Localised strength testing of materials is often carried out in an atomic force microscope (AFM), as foreseen by Kelly in his book Strong Solids (Clarendon Press, Oxford, 1966). During AFM indentation experiments, contamination can strongly influence the observed strength and theoretical interpretation of the results is a major problem. Here, we use molecular dynamics computer modelling to describe the contact of NaCl and MgO crystal probes onto surfaces, comparable to an AFM experiment. Clean NaCl gave elastic, brittle behaviour in contact simulations at 300 K, whereas MgO was more plastic, leading to increased toughness. This paper also considers the strength of an oxide substrate contaminated by water molecules and tested by indentation with a pyramidal probe of oxide crystal. Recent theory on the effect of liquid contaminant layers on surface strength has been mainly focussed on Lennard Jones (LJ) molecules with some studies on alcohols and water, described by molecular dynamics, which allows the molecules to be squeezed out as the crystal lattice is deformed. In this work, we have focused on water by studying the forces between a magnesium oxide (MgO) atomic force microscope (AFM) probe and an MgO slab. Force versus separation has been plotted as the AFM probe was moved towards and away from the substrate. Simulation results showed that the water layers could be removed in steps, giving up to four force peaks. The last monolayer of water could not be squeezed out, even at pressures where MgO deformed plastically. Interestingly, with water present, strength was reduced, but more in tensile than compressive measurements. In conclusion, water contaminating the oxide surface in AFM strength testing is structured. Water layer squeezing removal can be predicted by molecular modelling, which may be verified by AFM experiments to show that water can influence the strength of perfect crystals at the nanometre scale.

  4. Detection of Pathogens Using AFM and SPR

    NASA Astrophysics Data System (ADS)

    Vaseashta, Ashok

    2005-03-01

    A priori detection of pathogens in food and water has become a subject of paramount importance. Several recent incidents have resulted in the government passing stringent regulations for tolerable amounts of contamination of food products. Identification and/or monitoring of bacterial contamination in food are critical. The conventional methods of pathogen detection require time-consuming steps to arrive disembark at meaningful measurement in a timely manner as the detection time exceeds the time in which perishable food recycles through the food chain distribution. The aim of this presentation is to outline surface plasmon resonance (SPR) and atomic force microscopy (AFM) as two methods for fast detect6ion of pathogens. Theoretical basis of SPR and experimental results of SPR and AFM on E. coli O157:H7 and prion are presented.

  5. Critical issues in measuring the mechanical properties of hard films on soft substrates by nanoindentation techniques

    SciTech Connect

    Hay, J.C.; Pharr, G.M.

    1997-12-31

    This study explores the difficulties encountered when using conventional nanoindentation techniques to measure the Young`s modulus and hardness of hard films on soft substrates. In general, the indentation measurement of film/substrate systems is affected by four material properties: the Young`s modulus and hardness of the film, and the Young`s modulus and hardness of the substrate. For the particular case of a hard film on a soft substrate, there is a tendency for the material around the hardness impression to sink-in which results from the large difference in yielding of the two materials. In this study, a model system consisting of NiP on annealed Cu was used to explore the behavior. This system is interesting because the film and substrate have similar Young`s moduli, minimizing the elastic behavior as a variable. In contrast, the hardness of NiP is approximately 7--8 GPa, and that of the annealed copper is less than 1 GPa, providing a factor of 10 difference in the plastic flow characteristics. Experimental results indicate that standard analytical methods for determining the contact depth, hardness and Young`s modulus do not work well for the case of a hard film on a soft substrate. At shallow contact depths, the measured indentation modulus is close to that of the film, but at larger depths sink-in phenomena result in an overestimation of the contact area, and an indentation modulus which is less than the Young`s modulus of both the film and substrate. Atomic force microscopy (AFM) and scanning electron microscopy (SEM) provide critical details of the physical processes involved, and illustrate how the standard data analyses overestimate the true contact area.

  6. Characterizing Cell Mechanics with AFM and Microfluidics

    NASA Astrophysics Data System (ADS)

    Walter, N.; Micoulet, A.; Suresh, S.; Spatz, J. P.

    2007-03-01

    Cell mechanical properties and functionality are mainly determined by the cytoskeleton, besides the cell membrane, the nucleus and the cytosol, and depend on various parameters e.g. surface chemistry and rigidity, surface area and time available for cell spreading, nutrients and drugs provided in the culture medium. Human epithelial pancreatic and mammary cancer cells and their keratin intermediate filaments are the main focus of our work. We use Atomic Force Microscopy (AFM) to study cells adhering to substrates and Microfluidic Channels to probe cells in suspension, respectively. Local and global properties are extracted by varying AFM probe tip size and the available adhesion area for cells. Depth-sensing, instrumented indentation tests with AFM show a clear difference in contact stiffness for cells that are spread of controlled substrates and those that are loosely attached. Microfluidic Channels are utilized in parallel to evaluate cell deformation and ``flow resistance'', which are dependent on channel cross section, flow rate, cell nucleus size and the mechanical properties of cytoskeleton and membrane. The results from the study are used to provide some broad and quantitative assessments of the connections between cellular/subcellular mechanics and biochemical origins of disease states.

  7. Extraction of elastic modulus of porous ultra-thin low-k films by two-dimensional finite-element simulations of nanoindentation

    NASA Astrophysics Data System (ADS)

    Okudur, O. O.; Vanstreels, K.; De Wolf, I.; Hangen, U.

    2016-01-01

    Continuous scaling of integrated circuits has led to the introduction of highly porous low dielectric constant (low-k) materials, whose inferior mechanical properties raise concerns regarding the reliability of integrated circuits. Nanoindentation is proven to be a straightforward method to study mechanical properties of films. However, in the case of low-k, the measurement and analysis are complex due to the porous nature of the films and reduced film thicknesses which give rise to substrate effects. A methodology that combines nanoindentation experiments with finite-element simulations is proposed and validated in this study to extract the substrate-free elastic modulus of porous ultra-thin low-k films. Furthermore, it is shown that imperfections of the nanoindentation probe significantly affect the finite-element results. An effective analytical method that captures the actual nanoindenter behavior upon indentation is proposed by taking both tip radius and conical imperfections into account. Using this method combined with finite element modeling, the elastic modulus of sub-100 nm thick low-k films is successfully extracted. Standard indentation tests clearly overestimated the actual modulus for such thin films, which emphasizes the importance of the proposed methodology.

  8. Thermal activation in Au-based bulk metallic glass characterized by high-temperature nanoindentation

    SciTech Connect

    Nieh, Tai-Gang; Yang, Bing; Wadsworth, Jeffrey

    2007-01-01

    High-temperature nanoindentation experiments have been conducted on a Au49Ag5.5Pd2.3Cu26.9Si16.3 bulk metallic glass from 30 to 140 C, utilizing loading rates ranging from 0.1 to 100 mN/s. Generally, the hardness decreased with increasing temperature. An inhomogeneous-to-homogeneous flow transition was clearly observed when the test temperature approaches the glass transition temperature. Analyses of the pop-in pattern and hardness variation showed that the inhomogeneous-to-homogeneous transition temperature was loading-rate dependent. Using a free-volume model, we successfully deduced the size of the basic flow units and the activation energy for the homogeneous flow. In addition, the strain-rate dependency of the transition temperature was predicted.

  9. Hardness and deformation mechanisms of highly elastic carbon nitride thin films as studied by nanoindentation

    SciTech Connect

    Hainsworth, S.V.; Page, T.F.; Sjoestroem, H.; Sundgren, J.E.

    1997-05-01

    Carbon nitride (CN{sub x}) thin films (0.18 < x < 0.43), deposited by magnetron sputtering of C in a N{sub 2} discharge, have been observed to be extremely resistant to plastic deformation during surface contact (i.e., exhibit a purely elastic response over large strains). Elastic recoveries as high as 90% have been measured by nanoindentation. This paper addresses the problems of estimating Young`s modulus (E) and hardness (H) in such cases and shows how different strategies involving analysis of both loading and unloading curves and measuring the work of indentation each present their own problems. The results of some cyclic contact experiments are also presented and possible deformation mechanisms in the fullerene-like CN{sub x} structures discussed.

  10. Influence of sintering temperatures on hardness and Young's modulus of tricalcium phosphate bioceramic by nanoindentation technique

    SciTech Connect

    Wang, C.X. . E-mail: c.wang@bham.ac.uk; Zhou, X.; Wang, M.

    2004-07-15

    Nanoindentation experiments on tricalcium phosphate (TCP) bioceramic sintered at different temperatures were performed with a Berkovich indenter for determining hardness and elastic modulus from load and displacement data. The hardness and Young's modulus increased with the increase of sintering temperature up to 1300 deg. C, but the Young's modulus decreased with the further increase of sintering temperatures at 1400 and 1500 deg. C. X-ray diffraction (XRD) results showed that the transformation {beta}{yields}{alpha}-TCP happened when the sintering temperature reached around 1400 deg. C, which contributed to the decreases of modulus at 1400 and 1500 deg. C. Scanning electron microscopy (SEM) results showed that the sintering effect was improved with the increase in sintering temperature.

  11. A software tool for STED-AFM correlative super-resolution microscopy

    NASA Astrophysics Data System (ADS)

    Koho, Sami; Deguchi, Takahiro; Löhmus, Madis; Näreoja, Tuomas; Hänninen, Pekka E.

    2015-03-01

    Multi-modal correlative microscopy allows combining the strengths of several imaging techniques to provide unique contrast. However it is not always straightforward to setup instruments for such customized experiments, as most microscope manufacturers use their own proprietary software, with limited or no capability to interface with other instruments - this makes correlation of the multi-modal data extremely challenging. We introduce a new software tool for simultaneous use of a STimulated Emission Depletion (STED) microscope with an Atomic Force Microscope (AFM). In our experiments, a Leica TCS STED commercial super-resolution microscope, together with an Agilent 5500ilm AFM microscope was used. With our software, it is possible to synchronize the data acquisition between the STED and AFM instruments, as well as to perform automatic registration of the AFM images with the super-resolution STED images. The software was realized in LabVIEW; the registration part was also implemented as an ImageJ script. The synchronization was realized by controlling simple trigger signals, also available in the commercial STED microscope, with a low-cost National Instruments USB-6501 digital I/O card. The registration was based on detecting the positions of the AFM tip inside the STED fieldof-view, which were then used as registration landmarks. The registration should work on any STED and tip-scanning AFM microscope combination, at nanometer-scale precision. Our STED-AFM correlation method has been tested with a variety of nanoparticle and fixed cell samples. The software will be released under BSD open-source license.

  12. Nanoindentation in Materials Research: Past, Present, and Future

    SciTech Connect

    Oliver, Warren; Pharr, George Mathews

    2010-01-01

    The method we introduced in 1992 for measuring hardness and elastic modulus by nanoindentation testing has been widely adopted and used in the characterization of mechanical behavior at small scales. Since its original development, the method has undergone numerous refinements and changes brought about by improvements to testing equipment and techniques, as well as advances in our understanding of the mechanics of elastic-plastic contact. In this article, we briefly review the history of the method, comment on its capabilities and limitations, and discuss some of the emerging areas in materials research where it has played, or promises to play, an important role.

  13. Nanoindentation as a composition microprobe for nanolayer composites

    SciTech Connect

    Tambwe, M.F.; Stone, D.S.; Hirvonen, J.P.; Hannula, S.P.; Suni, I.

    1997-11-01

    Aluminum and tungsten differ by a factor of about 6 in Young`s modulus. For this reason, modulus measurements made by nanoindentation are sensitive to small variations in the relative amounts of aluminum and tungsten that make up the laminate composites. The volume fractions of the layers estimated based on the elasticity model for indentation of a transversely isotropic film on substrate agree well with the compositions measured by Rutherford Backscattering (RBS) except for the 3 nm (nominal) specimen, which, the authors have reason to believe based on x-ray diffraction measurements, contains intermetallic compounds.

  14. Nanoindentation of soft solids by a flat punch

    NASA Astrophysics Data System (ADS)

    Wang, G. F.; Niu, X. R.

    2015-08-01

    Measuring the surface tension and elastic modulus of soft materials and biological tissues under different physiological and pathological conditions is of significance for understanding various phenomena associated with deformation. In this paper, the nanoindentation of a circular flat punch on a soft solid is analyzed with the influence of surface tension. By solving the corresponding singular integral equation, the relation between load and indent depth is obtained. When the radius of the flat punch shrinks to the same order as the ratio of surface tension to elastic modulus, surface tension significantly affects the indentation load-depth relation, which provides a facile method to measure surface tension in soft solids and biological tissues.

  15. Peculiarities of plastic deformation nucleation in copper under nanoindentation

    SciTech Connect

    Kryzhevich, Dmitrij S. Korchuganov, Aleksandr V.; Zolnikov, Konstantin P.; Psakhie, Sergey G.

    2015-10-27

    The computer simulation results on the atomic structure of the copper crystallite and its behavior in nanoindentation demonstrate the key role of local structural transformations in nucleation of plasticity. The generation of local structural transformations can be considered as an elementary event during the formation of higher scale defects, including partial dislocations and stacking faults. The cause for local structural transformations, both direct fcc-hcp and reverse hcp-fcc, is an abrupt local increase in atomic volume. A characteristic feature is that the values of local volume jumps in direct and reverse structural transformations are comparable with that in melting and lie in the range 5–7%.

  16. Nanoindentation and scratch studies on magnetron sputtered Ti thin films.

    PubMed

    Kataria, S; Ramaseshan, R; Dash, S; Tyagi, A K

    2009-09-01

    Ti thin films sputter deposited on D9 steel at two different temperatures were studied for their mechanical behavior under static and sliding contact conditions using nanoindentation and scratch tests. The film hardness measured at the surface of the coatings exhibited a value of 2.5 GPa, for both conditions. From the scratch test, it is understood that coatings deposited at 200 degrees C substrate temperature showed superior adhesion strength. Critical load to failure for these coatings was evaluated at 2 N. PMID:19928247

  17. Peculiarities of modeling of nanoindentation of coating-substrate system

    NASA Astrophysics Data System (ADS)

    Eremina, Galina M.; Smolin, Alexey Yu.; Psakhie, Sergey G.

    2015-10-01

    In this paper we discuss some features that are important in modeling nanoindentation of strength coating deposited on metallic substrate. The modeling is performed by movable cellular automaton method, which is a representative of the discrete element methods in computational solid mechanics. Taking into account such factors as capability of the substrate material to harden, friction between the surface and the indenter as well as the presence of an intermediate layer between the coating and the substrate, it is shown that they can deeply affect the mechanical behavior of the system.

  18. Development and validation of a novel data analysis procedure for spherical nanoindentation

    NASA Astrophysics Data System (ADS)

    Pathak, Siddhartha

    This dissertation presents a novel approach for converting the raw load-displacement data measured in spherical nanoindentation into much more meaningful indentation stress-strain curves. This new method entails a novel definition of the indentation strain and a new procedure for establishing the effective zero point in the raw dataset---both with and without the use of the continuous stiffness measurement (CSM) data. The concepts presented here have been validated by simulations and experiments on isotropic metallic samples of aluminum and tungsten. It is demonstrated that these new indentation stress-strain curves accurately capture the loading and unloading elastic moduli, the indentation yield points, as well as the post-yield characteristics in the tested samples. Subsequently this approach has been applied on a wide range of material systems including metals, carbon nanotubes (CNTs), ceramics and bone. In metals, these data analysis techniques have been highly successful in explaining several of the surface preparation artifacts typically encountered during nanoindentation measurements. This approach has also been extended to anisotropic polycrystalline samples, where a judicious combination of Orientation Imaging Microscopy (OIM) and nanoindentation were used to estimate, for the first time, the changes in slip resistance in deformed grains of Fe-3%Si steel. Similar studies on dense CNT brushes, with ˜10 times higher density than CNT brushes produced by other methods, demonstrate the higher modulus (˜17-20 GPa) and orders of magnitude higher resistance to buckling in these brushes than vapor phase deposited CNT brushes or carbon walls, showing their promise for energy-absorbing coatings. Even for a complex hierarchical material system like bone, these techniques have elucidated trends in the elastic and yield behavior at the lamellar level in the femora (thigh bone) of different inbred mouse strains. Thus bone with a higher mineral-to-matrix ratio

  19. Effect of Crystal Orientation on Nanoindentation Behavior in Magnesium

    NASA Astrophysics Data System (ADS)

    Somekawa, Hidetoshi; Schuh, Christopher A.

    2016-06-01

    The effect of crystal orientation on nanoindentation behavior at both quasi-static and high strain rates was investigated using single-crystalline magnesium oriented in basal and prismatic configurations. Both the basal and prismatic planes had similar activation volumes, 55 and 73 b 3 for deformation at room temperature, as well as a small temperature dependence up to 423 K (150 °C). Microstructural observations beneath the indentations revealed that { 10bar{1}2 } type deformation twins were formed in both orientations irrespective of testing temperature. With twins forming beneath the indenter and multiple orientations of loading, it is believed that cross-slip and/or multiple slip are likely rate-controlling for global deformation, which also aligns with observations on nanoindentation of polycrystalline coarse-grained magnesium. The locations of the twins were consistent with expectations based on indentation mechanics as assessed by finite element simulations. The finite element simulations also predicted that an indenter tip with a shaper tip radius would tend to promote { 10bar{1}2 } twins.

  20. Effect of Crystal Orientation on Nanoindentation Behavior in Magnesium

    NASA Astrophysics Data System (ADS)

    Somekawa, Hidetoshi; Schuh, Christopher A.

    2016-04-01

    The effect of crystal orientation on nanoindentation behavior at both quasi-static and high strain rates was investigated using single-crystalline magnesium oriented in basal and prismatic configurations. Both the basal and prismatic planes had similar activation volumes, 55 and 73b 3 for deformation at room temperature, as well as a small temperature dependence up to 423 K (150 °C). Microstructural observations beneath the indentations revealed that { 10bar{1}2 } type deformation twins were formed in both orientations irrespective of testing temperature. With twins forming beneath the indenter and multiple orientations of loading, it is believed that cross-slip and/or multiple slip are likely rate-controlling for global deformation, which also aligns with observations on nanoindentation of polycrystalline coarse-grained magnesium. The locations of the twins were consistent with expectations based on indentation mechanics as assessed by finite element simulations. The finite element simulations also predicted that an indenter tip with a shaper tip radius would tend to promote { 10bar{1}2 } twins.

  1. Nanoindentation and the micromechanics of Van Gogh oil paints

    NASA Astrophysics Data System (ADS)

    Salvant, Johanna; Barthel, Etienne; Menu, Michel

    2011-08-01

    Understanding the mechanical properties of ancient paintings is a major issue for conservation and restoration. One strategy is to measure the mechanical properties of reconstructed paints: however, the aging process is poorly known, so it is also desirable to measure mechanical properties directly on ancient paint samples. Using nanoindentation, we have characterized submillimetric samples recovered from restoration of two Van Gogh paintings and compared the results with reconstructed paint samples. We demonstrate that the reduced modulus and hardness of historical paints can be measured at a very local scale, even differentiating between each paint layer. Our reconstructed paint samples exhibit elastic moduli comparable to values of the literature, but the values measured on the two 19th century paint samples are found to be significantly larger. Similarly, the compositional dependence of the elastic modulus is consistent with literature results for our reconstructed samples while our preliminary results for ancient samples do not readily fall into the same pattern. These results all point out to a significant impact of long term aging, in a manner which is difficult to predict in our present state of understanding. They demonstrate that nanoindentation is a very adequate tool to improve our knowledge of art paint mechanics and aging.

  2. Effect of helium implantation on mechanical properties of EUROFER97 evaluated by nanoindentation

    NASA Astrophysics Data System (ADS)

    Roldán, M.; Fernández, P.; Rams, J.; Jiménez-Rey, D.; Ortiz, C. J.; Vila, R.

    2014-05-01

    Helium effects on EUROFER97 mechanical properties were studied by means of nanoindentation. The steel was implanted with He ions in a stair-like profile configuration using energies from 2 to 15 MeV at room temperature. Firstly, a deep nanoindentation study was carried out on as-received state (normalized + tempered) in order to obtain a reliable properties database at the nanometric scale, including aspects such as indentation size effect. The nanoindentation hardness of tests on He implanted samples showed a hardness increase depending on the He concentration. The hardness increase follows the He implantation concentration profile with a good accuracy according to BCA calculations using MARLOWE code, considering the whole volume affected by the nanoindentation tests. The results obtained in this work shown that nanoindentation technique permits to assess any change of hardness properties due to ion implantation.

  3. SU-8 hollow cantilevers for AFM cell adhesion studies

    NASA Astrophysics Data System (ADS)

    Martinez, Vincent; Behr, Pascal; Drechsler, Ute; Polesel-Maris, Jérôme; Potthoff, Eva; Vörös, Janos; Zambelli, Tomaso

    2016-05-01

    A novel fabrication method was established to produce flexible, transparent, and robust tipless hollow atomic force microscopy (AFM) cantilevers made entirely from SU-8. Channels of 3 μm thickness and several millimeters length were integrated into 12 μm thick and 40 μm wide cantilevers. Connected to a pressure controller, the devices showed high sealing performance with no leakage up to 6 bars. Changing the cantilever lengths from 100 μm to 500 μm among the same wafer allowed the targeting of various spring constants ranging from 0.5 to 80 N m‑1 within a single fabrication run. These hollow polymeric AFM cantilevers were operated in the optical beam deflection configuration. To demonstrate the performance of the device, single-cell force spectroscopy experiments were performed with a single probe detaching in a serial protocol more than 100 Saccharomyces cerevisiae yeast cells from plain glass and glass coated with polydopamine while measuring adhesion forces in the sub-nanoNewton range. SU-8 now offers a new alternative to conventional silicon-based hollow cantilevers with more flexibility in terms of complex geometric design and surface chemistry modification.

  4. BOREAS AFM-6 Surface Meteorological Data

    NASA Technical Reports Server (NTRS)

    Wilczak, James; Hall, Forrest G. (Editor); Newcomer, Jeffrey A. (Editor); Smith, David E. (Technical Monitor)

    2000-01-01

    The Boreal Ecosystem-Atmosphere Study (BOREAS) Airborne Fluxes and Meteorology (AFM)-6 team from the National Oceanic and Atmospheric Adminsitration/Environment Technology Laboratory (NOAA/ETL) collected surface meteorological data from 21 May to 20 Sep 1994 near the Southern Study Area-Old Jack Pine (SSA-OJP) tower site. The data are in tabular ASCII files. The surface meteorological data are available from the Earth Observing System Data and Information System (EOSDIS) Oak Ridge National Laboratory (ORNL) Distributed Active Archive Center (DAAC). The data files are available on a CD-ROM (see document number 20010000884).

  5. A rapid and automated relocation method of an AFM probe for high-resolution imaging.

    PubMed

    Zhou, Peilin; Yu, Haibo; Shi, Jialin; Jiao, Niandong; Wang, Zhidong; Wang, Yuechao; Liu, Lianqing

    2016-09-30

    The atomic force microscope (AFM) is one of the most powerful tools for high-resolution imaging and high-precision positioning for nanomanipulation. The selection of the scanning area of the AFM depends on the use of the optical microscope. However, the resolution of an optical microscope is generally no larger than 200 nm owing to wavelength limitations of visible light. Taking into consideration the two determinants of relocation-relative angular rotation and positional offset between the AFM probe and nano target-it is therefore extremely challenging to precisely relocate the AFM probe to the initial scan/manipulation area for the same nano target after the AFM probe has been replaced, or after the sample has been moved. In this paper, we investigate a rapid automated relocation method for the nano target of an AFM using a coordinate transformation. The relocation process is both simple and rapid; moreover, multiple nano targets can be relocated by only identifying a pair of reference points. It possesses a centimeter-scale location range and nano-scale precision. The main advantages of this method are that it overcomes the limitations associated with the resolution of optical microscopes, and that it is label-free on the target areas, which means that it does not require the use of special artificial markers on the target sample areas. Relocation experiments using nanospheres, DNA, SWCNTs, and nano patterns amply demonstrate the practicality and efficiency of the proposed method, which provides technical support for mass nanomanipulation and detection based on AFM for multiple nano targets that are widely distributed in a large area. PMID:27559679

  6. Fracture toughness of bleached enamel: Effect of applying three different nanobiomaterials by nanoindentation test

    PubMed Central

    Khoroushi, Maryam; Mazaheri, Hamid; Saneie, Tahere; Samimi, Pouran

    2016-01-01

    Background: Despite the absence of dispute about the efficacy of bleaching agents, a prime concern is about their compromising effect on the enamel structure. This in vitro study investigated whether the addition of three different biomaterials, including nano-bioactive glass (n-BG)/nano-hydroxy apetite (n-HA)/nano-amorphous calcium phosphate (n-ACP), to bleaching agents can affect the fracture toughness (FT) and vickers hardness number (VHN) of bovine enamel. Materials and Methods: The crowns of the newly extracted permanent bovine incisors teeth were separated from the root and sectioned along their central line; one half serving as the control specimen and the other half as the test specimen. After mounting and polishing procedure, all the control specimens (C) were subjected to nano-indentation test to obtain the baseline values of FT. Then, the control specimens were exposed to a 38% hydrogen peroxide for four times, each time for 10 min. The test specimens were divided into three groups and treated as follows, with the same protocol used for the control specimens: Group 1; ACP + hydrogen peroxide (HP) mixed gel; Group 2 BG + HP mixed gel; and Group 3 HA + HP mixed gel. FT measurements with nano-indentation were carried out subsequent to bleaching experiments. Data were analyzed using SPSS and Kruskal–Wallis test (α = 0.05). Results: A significant difference in young's modulus (YM), VHN, and FT at baseline and subsequent to bleaching in control group was observed. However, no significant differences were found in YM, VHN, and FT between the test groups, compared to the respective baseline values. Conclusion: Under the limitations of the current study, it can be concluded that the n-HA, n-ACP, and n-BG could be potential biomaterials used to reduce the adverse effects of tooth bleaching. PMID:27307669

  7. Strain shielding from mechanically activated covalent bond formation during nanoindentation of graphene delays the onset of failure.

    PubMed

    Kumar, Sandeep; Parks, David M

    2015-03-11

    Mechanical failure of an ideal crystal is dictated either by an elastic instability or a soft-mode instability. Previous interpretations of nanoindentation experiments on suspended graphene sheets,1,2 however, indicate an anomaly: the inferred strain in the graphene sheet directly beneath the diamond indenter at the measured failure load is anomalously large compared to the fracture strains predicted by both soft-mode and acoustic analyses. Through multiscale modeling combining the results of continuum, atomistic, and quantum calculations, and analysis of experiments, we identify a strain-shielding effect initiated by mechanochemical interactions at the graphene-indenter interface as the operative mechanism responsible for this anomaly. Transmission electron micrographs and a molecular model of the diamond indenter's tip suggest that the tip surface contains facets comprising crystallographic {111} and {100} planes. Ab initio and molecular dynamics (MD) simulations confirm that a covalent bond (weld) formation between graphene and the crystallographic {111} and {100} facets on the indenter's surface can be induced by compressive contact stresses of the order achieved in nanoindentation tests. Finite element analysis (FEA) and MD simulations of nanoindentation reveal that the shear stiction provided by the induced covalent bonding restricts relative slip of the graphene sheet at its contact with the indenter, thus initiating a local strain-shielding effect. As a result, subsequent to stress-induced bonding at the graphene-indenter interface, the spatial variation of continuing incremental strain is substantially redistributed, locally shielding the region directly beneath the indenter by limiting the buildup of strain while imparting deformation to the surrounding regions. The extent of strain shielding is governed by the strength of the shear stiction, which depends upon the level of hydrogen saturation at the indenter's surface. We show that at intermediate levels

  8. A hybrid approach to determining cornea mechanical properties in vivo using a combination of nano-indentation and inverse finite element analysis.

    PubMed

    Abyaneh, M H; Wildman, R D; Ashcroft, I A; Ruiz, P D

    2013-11-01

    An analysis of the material properties of porcine corneas has been performed. A simple stress relaxation test was performed to determine the viscoelastic properties and a rheological model was built based on the Generalized Maxwell (GM) approach. A validation experiment using nano-indentation showed that an isotropic GM model was insufficient for describing the corneal material behaviour when exposed to a complex stress state. A new technique was proposed for determining the properties, using a combination of nano-indentation experiment, an isotropic and orthotropic GM model and inverse finite element method. The good agreement using this method suggests that this is a promising technique for measuring material properties in vivo and further work should focus on the reliability of the approach in practice. PMID:23816808

  9. Nanotribological and nanomechanical properties of skin with and without cream treatment using atomic force microscopy and nanoindentation.

    PubMed

    Bhushan, Bharat

    2012-02-01

    Various beauty care products involve surface interaction between the product and the skin surface they are applied to. Friction, adhesion and wear during sliding between the treated surface and the rubbing surfaces need to be optimized. Skin cream is used to improve skin health and create a smooth, soft, and flexible surface with moist perception by altering the surface roughness, friction, adhesion, elastic modulus, and surface charge of the skin surface. Rheology of skin cream as a function of cream thickness and strain rate and the binding interaction between skin cream and skin surface and operating environment are some of the important factors affecting the smooth feel and repair of the skin surface. Atomic force microscopy (AFM) and nanoindentation have recently become important tools for studying the micro/nanoscale properties of human hair, hair conditioner, skin, and skin cream. In this paper, we present an overview of the nanotribological and nanomechanical properties of skin with and without cream treatment as a function of operating environment. Relevant mechanisms are discussed. Next, the result of a triboelectrification study of skin with and without cream treatment is presented. Finally, an overview of attempts to develop a synthetic skin for research purposes is presented. PMID:22104280

  10. Mechanical Characterization of Photo-crosslinkable Hydrogels with AFM

    NASA Astrophysics Data System (ADS)

    McKenna, Alyssa; Byun, Myunghwan; Hayward, Ryan; Aidala, Katherine

    2012-02-01

    Stimuli-responsive hydrogel films formed from photo-crosslinkable polymers are versatile materials for controlled drug delivery devices, three-dimensional micro-assemblies, and components in microfluidic systems. For such applications, it is important to understand both the mechanical properties and the dynamics responses of these materials. We describe the use of atomic force microscope (AFM) based indentation experiments to characterize the properties of poly(N-isopropylacrylamide) copolymer films, crosslinked by activation of pendent benzophenone units using ultraviolet light. In particular, we study how the elastic modulus of the material, determined using the Johnson, Kendall, and Roberts model, depends on UV dose, and simultaneously investigate stress relaxation in these materials in the context of viscoelastic and poroelastic relaxation models.

  11. [AFM fishing of proteins under impulse electric field].

    PubMed

    Ivanov, Yu D; Pleshakova, T O; Malsagova, K A; Kaysheva, A L; Kopylov, A T; Izotov, A A; Tatur, V Yu; Vesnin, S G; Ivanova, N D; Ziborov, V S; Archakov, A I

    2016-05-01

    A combination of (atomic force microscopy)-based fishing (AFM-fishing) and mass spectrometry allows to capture protein molecules from solutions, concentrate and visualize them on an atomically flat surface of the AFM chip and identify by subsequent mass spectrometric analysis. In order to increase the AFM-fishing efficiency we have applied pulsed voltage with the rise time of the front of about 1 ns to the AFM chip. The AFM-chip was made using a conductive material, highly oriented pyrolytic graphite (HOPG). The increased efficiency of AFM-fishing has been demonstrated using detection of cytochrome b5 protein. Selection of the stimulating pulse with a rise time of 1 ns, corresponding to the GHz frequency range, by the effect of intrinsic emission from water observed in this frequency range during water injection into the cell. PMID:27562998

  12. Nanoindentation study of size effects in nickel-graphene nanocomposites

    NASA Astrophysics Data System (ADS)

    Chang, Shu-Wei; Nair, Arun K.; Buehler, Markus J.

    2013-04-01

    Metal-graphene nanocomposites find applications in nanoscale devices, as functional materials and can serve as a test bed to gain insight into fundamental deformation mechanisms of metals under geometric confinement. Here, we report full atomistic nanoindentation simulations for nickel-graphene nanocomposites with varied numbers of layers of graphene sheets to investigate the size effects on the hardness, and to understand how emerging dislocation loops interact with the nickel-graphene interface under varied geometric confinements. A detailed analysis of the plastic deformation mechanism shows that as dislocation loops reach the nickel-graphene interface, the local bending of the graphene sheet is altered and further dislocation propagation is blocked. An increase in the number of graphene layers decreases the hardness, but increases the maximum elastic deformation of the nickel-graphene nanocomposites. These findings indicate that the mechanical properties of nickel-graphene nanocomposites can be engineered by controlling the thickness of nickel and graphene layers, respectively.

  13. Influence of indenter tip geometry on elastic deformation during nanoindentation

    SciTech Connect

    Bei, Hongbin; George, Easo P; Hay, J. L.; Pharr, George Mathews

    2005-01-01

    Nanoindentation with a Berkovich indenter is commonly used to investigate the mechanical behavior of small volumes of materials. To date, most investigators have made the simplifying assumption that the tip is spherical. In reality, indenter tips are much more complex. Here, we develop a new method to describe the tip shape using the experimentally determined area function of the indenter at small depths (0--100 nm). Our analysis accurately predicts the elastic load-displacement curve and allows the theoretical strength of a material to be determined from pop-in data. Application of our new method to single crystal Cr{sub 3}Si shows that the predicted theoretical strengths are within 12% of the ideal strength G/2{pi}, where G is the shear modulus.

  14. Nano-Ordered Wear Property of Magnesium Obtaining Nanoindentation

    NASA Astrophysics Data System (ADS)

    Somekawa, Hidetoshi; Tomita, Kazuhiro; Toda, Miwako; Hirayama, Tomoko; Matsuoka, Takashi

    2015-09-01

    The nano-scale wear properties of single-crystalline and polycrystalline magnesium were investigated using the nanoindentation technique. The results for single crystals revealed that the crystal orientation affected the wear rate in the case that no deformation twinning was formed, e.g., under conditions of low applied loads. However, when deformation twinning formed during scratch testing, the wear properties became worse, i.e., the wear rate increased. One reason was that twin boundaries did not play a role as dislocation sources and sinks; the dislocations at twin boundaries brought about the expansion and growth for deformation twinning. As for the impact of grain boundaries on the wear properties, the wear rate for fine-grained magnesium was similar to that for single crystals. This result indicated that the existence of grain boundaries did not effectively improve the wear properties of magnesium, as in large-scale wear testing, such as the pin-on-disk configuration.

  15. Subsurface damage of single crystalline silicon carbide in nanoindentation tests.

    PubMed

    Yan, Jiwang; Gai, Xiaohui; Harada, Hirofumi

    2010-11-01

    The response of single crystalline silicon carbide (SiC) to a Berkovich nanoindenter was investigated by examining the indents using a transmission electron microscope and the selected area electron diffraction technique. It was found that the depth of indentation-induced subsurface damage was far larger than the indentation depth, and the damaging mechanism of SiC was distinctly different from that of single crystalline silicon. For silicon, a broad amorphous region is formed underneath the indenter after unloading; for SiC, however, no amorphous phase was detected. Instead, a polycrystalline structure with a grain size of ten nanometer level was identified directly under the indenter tip. Micro cracks, basal plane dislocations and possible cross slips were also found around the indent. These finding provide useful information for ultraprecision manufacturing of SiC wafers. PMID:21138038

  16. BOREAS AFM-06 Mean Temperature Profile Data

    NASA Technical Reports Server (NTRS)

    Wilczak, James; Hall, Forrest G. (Editor); Newcomer, Jeffrey A. (Editor); Smith, David E. (Technical Monitor)

    2000-01-01

    The Boreal Ecosystem-Atmosphere Study (BOREAS) Airborne Fluxes and Meteorology (AFM)-6 team from the National Oceanic and Atmospheric Adminsitration/Environment Technology Laboratory (NOAA/ETL) operated a 915-MHz wind/Radio Acoustic Sounding System (RASS) profiler system in the Southern Study Area (SSA) near the Old Jack Pine (OJP) tower from 21 May 1994 to 20 Sep 1994. The data set provides temperature profiles at 15 heights, containing the variables of virtual temperature, vertical velocity, the speed of sound, and w-bar. The data are stored in tabular ASCII files. The mean temperature profile data are available from the Earth Observing System Data and Information System (EOSDIS) Oak Ridge National Laboratory (ORNL) Distributed Active Archive Center (DAAC). The data files are available on a CD-ROM (see document number 20010000884).

  17. BOREAS AFM-6 Boundary Layer Height Data

    NASA Technical Reports Server (NTRS)

    Wilczak, James; Hall, Forrest G. (Editor); Newcomer, Jeffrey A. (Editor); Smith, David E. (Technical Monitor)

    2000-01-01

    The Boreal Ecosystem-Atmosphere Study (BOREAS) Airborne Fluxes and Meteorology (AFM)-6 team from National Oceanic and Atmospheric Adminsitration/Environment Technology Laboratory (NOAA/ETL) operated a 915-MHz wind/Radio Acoustic Sounding System (RASS) profiler system in the Southern Study Area (SSA) near the Old Jack Pine (OJP) site. This data set provides boundary layer height information over the site. The data were collected from 21 May 1994 to 20 Sep 1994 and are stored in tabular ASCII files. The boundary layer height data are available from the Earth Observing System Data and Information System (EOSDIS) Oak Ridge National Laboratory (ORNL) Distributed Active Archive Center (DAAC). The data files are available on a CD-ROM (see document number 20010000884).

  18. BOREAS AFM-06 Mean Wind Profile Data

    NASA Technical Reports Server (NTRS)

    Wilczak, James; Hall, Forrest G. (Editor); Newcomer, Jeffrey A. (Editor); Smith, David E. (Technical Monitor)

    2000-01-01

    The Boreal Ecosystem-Atmosphere Study (BOREAS) Airborne Fluxes and Meteorology (AFM)-6 team from the National Oceanic and Atmospheric Administration/Environment Technology Laboratory (NOAA/ETL) operated a 915-MHz wind/Radio Acoustic Sounding System (RASS) profiler system in the Southern Study Area (SSA) near the Old Jack Pine (OJP) tower from 21 May 1994 to 20 Sep 1994. The data set provides wind profiles at 38 heights, containing the variables of wind speed; wind direction; and the u-, v-, and w-components of the total wind. The data are stored in tabular ASCII files. The mean wind profile data are available from the Earth Observing System Data and Information System (EOSDIS) Oak Ridge National Laboratory (ORNL) Distributed Active Archive Center (DAAC). The data files are available on a CD-ROM (see document number 20010000884).

  19. Afm Measrurements of Martian Soil Particles Using Mems Technology - Results from the PHOENIX Mission

    NASA Astrophysics Data System (ADS)

    Gautsch, S.; Parrat, D.; de Rooij, N. F.; Staufer, U.; Morookian, J. M.; Hecht, M. H.; Vijendran, S.; Sykulska, H.; Pike, W. T.

    2011-12-01

    Light scattering experiments conducted on Mars indicated that soil particles have dimensions around 1 μm. Particles in that range play an important role in the gas exchange between sub-surface water ice and the atmosphere. Their shape can help tracing the geological history and may indicate past presence of liquid water. NASA's Phoenix mission therefore decided to analyze soil and dust particles in the sub-micrometer to a few micrometer range using an atomic force microscope (AFM) for the first time on another planet. The co-axially mounted AFM was capable of resolving particles with 10nm lateral resolution. A MEMS approach combined with mechatronic concepts for the scanner was selected for implementing the AFM. For redundancy, the sensor chip featured eight silicon cantilevers each with a 7 to 8 μm high tip. The cantilevers could be cleaved off if contaminated. During NASA's Phoenix Mission, which operated on the red planet from May to October 2008, we could demonstrate successful AFM operations. The instrument has executed 85 experiments of which 26 were needed for calibration. Of the remaining experiments about half (28) returned images where signatures of particles could be discerned.

  20. Spherical nanoindentation stress-strain curves of commercially pure titanium and Ti-6Al-4V

    DOE Data Explorer

    Weaver, Jordan S. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Priddy, Matthew W. [Georgia Inst. of Technology, Atlanta, GA (United States); McDowell, David L. [Georgia Inst. of Technology, Atlanta, GA (United States); Kalidindi, Surya R. [Georgia Inst. of Technology, Atlanta, GA (United States)

    2016-07-27

    Spherical nanoindentation combined with electron back-scattered diffraction was employed to characterize the grain-scale elastic and plastic anisotropy of single crystal alpha-Ti for commercially pure (CP-Ti) and alloyed (Ti-64) titanium. In addition, alpha-beta Ti (single colony) grains were characterized. The data set includes the nanoindentation force, displacement, and contact stiffness, the nanoindentation stress-strain analysis, and the alpha-Ti crystal orientations. Details of the samples and experimental protocols can be found in Weaver et al. (2016) Acta Materialia doi:10.1016/j.actamat.2016.06.053.

  1. Investigation of Strain-Induced Martensitic Transformation in Metastable Austenite using Nanoindentation

    SciTech Connect

    Ahn, T.-H.; Oh, C.-S.; Kim, D. H.; Oh, K. H.; Bei, Hongbin; George, Easo P; Han, H. N.

    2010-01-01

    Strain-induced martensitic transformation of metastable austenite was investigated by nanoindentation of individual austenite grains in multi-phase steel. A cross-section prepared through one of these indented regions using focused ion beam milling was examined by transmission electron microscopy. The presence of martensite underneath the indent indicates that the pop-ins observed on the load-displacement curve during nanoindentation correspond to the onset of strain-induced martensitic transformation. The pop-ins can be understood as resulting from the selection of a favorable martensite variant during nanoindentation.

  2. Mapping strain fields induced in Zr-based bulk metallic glasses during in-situ nanoindentation by X-ray nanodiffraction

    NASA Astrophysics Data System (ADS)

    Gamcová, J.; Mohanty, G.; Michalik, Š.; Wehrs, J.; Bednarčík, J.; Krywka, C.; Breguet, J. M.; Michler, J.; Franz, H.

    2016-01-01

    A pioneer in-situ synchrotron X-ray nanodiffraction approach for characterization and visualization of strain fields induced by nanoindentation in amorphous materials is introduced. In-situ nanoindentation experiments were performed in transmission mode using a monochromatic and highly focused sub-micron X-ray beam on 40 μm thick Zr-based bulk metallic glass under two loading conditions. Spatially resolved X-ray diffraction scans in the deformed volume of Zr-based bulk metallic glass covering an area of 40 × 40 μm2 beneath the pyramidal indenter revealed two-dimensional map of elastic strains. The largest value of compressive elastic strain calculated from diffraction data at 1 N load was -0.65%. The region of high elastic compressive strains (<-0.3%) is located beneath the indenter tip and has radius of 7 μm.

  3. Application of instrumented nanoindentation in preformulation studies of pharmaceutical active ingredients and excipients.

    PubMed

    Egart, Mateja; Janković, Biljana; Srčič, Stane

    2016-09-01

    Nanoindentation allows quantitative determination of a material's response to stress such as elastic and plastic deformation or fracture tendency. Key instruments that have enabled great advances in nanomechanical studies are the instrumented nanoindenter and atomic force microscopy. The versatility of these instruments lies in their capability to measure local mechanical response, in very small volumes and depths, while monitoring time, displacement and force with high accuracy and precision. This review highlights the application of nanoindentation for mechanical characterization of pharmaceutical materials in the preformulation phase (primary investigation of crystalline active ingredients and excipients). With nanoindentation, mechanical response can be assessed with respect to crystal structure. The technique is valuable for mechanical screening of a material at an early development phase in order to predict and better control the processes in which a material is exposed to stress such as milling and compression. PMID:27383883

  4. Molecular Dynamics Simulation of Nanoindentation-induced Mechanical Deformation and Phase Transformation in Monocrystalline Silicon

    PubMed Central

    2008-01-01

    This work presents the molecular dynamics approach toward mechanical deformation and phase transformation mechanisms of monocrystalline Si(100) subjected to nanoindentation. We demonstrate phase distributions during loading and unloading stages of both spherical and Berkovich nanoindentations. By searching the presence of the fifth neighboring atom within a non-bonding length, Si-III and Si-XII have been successfully distinguished from Si-I. Crystallinity of this mixed-phase was further identified by radial distribution functions.

  5. Particle deformation induced by AFM tapping under different setpoint voltages

    NASA Astrophysics Data System (ADS)

    Wu, Chung-Lin; Farkas, Natalia; Dagata, John A.; He, Bo-Ching; Fu, Wei-En

    2014-09-01

    The measured height of polystyrene nanoparticles varies with setpoint voltage during atomic force microscopy (AFM) tapping-mode imaging. Nanoparticle height was strongly influenced by the magnitude of the deformation caused by the AFM tapping forces, which was determined by the setpoint voltage. This influence quantity was studied by controlling the operational AFM setpoint voltage. A test sample consisting of well-dispersed 60-nm polystyrene and gold nanoparticles co-adsorbed on poly-l-lysine-coated mica was studied in this research. Gold nanoparticles have not only better mechanical property than polystyrene nanoparticles, but also obvious facets in AFM phase image. By using this sample of mixed nanoparticles, it allows us to confirm that the deformation resulted from the effect of setpoint voltage, not noise. In tapping mode, the deformation of polystyrene nanoparticles increased with decreasing setpoint voltage. Similar behavior was observed with both open loop and closed loop AFM instruments.

  6. In situ characterization of formation and growth of high-pressure phases in single-crystal silicon during nanoindentation

    NASA Astrophysics Data System (ADS)

    Huang, Hu; Yan, Jiwang

    2016-04-01

    Pressure-induced intermediate phases of silicon exhibit unique characteristics in mechanics, chemistry, optics, and electrics. Clarifying the formation and growth processes of these new phases is essential for the preparation and application of them. For in situ characterization of the formation and growth of high-pressure phases in single-crystal silicon, a quantitative parameter, namely displacement change of indenter (Δ h) during the unloading holding process in nanoindentation, was proposed. Nanoindentation experiments under various unloading holding loads and loading/unloading rates were performed to investigate their effects on Δ h. Results indicate that Δ h varies significantly before and after the occurrence of pop-out; for the same maximum indentation load, it tends to increase with the decrease in the holding load and to increase with the increase in the loading/unloading rate. Thus, the value of Δ h can be regarded as an indicator that reflects the formation and growth processes of the high-pressure phases. Using Δ h, the initial position for the nucleation of the high-pressure phases, their growth, and their correlation to the loading/unloading rate were predictable.

  7. Microrheology using a custom-made AFM

    NASA Astrophysics Data System (ADS)

    Kosgodagan Acharige, Sebastien; Benzaquen, Michael; Steinberger, Audrey

    In the past few years, a new method was developed to measure local properties of liquids (X. Xiong et al., Phys. Rev. E 80, 2009). This method consists of gluing a micron-sized glass fiber at the tip of an AFM cantilever and probing the liquid with it. In ENS Lyon, this method was perfected (C. Devailly et al., EPL, 106 5, 2014) with the help of an interferometer developped in the same laboratory (L. Bellon et al., Opt. Commun. 207 49, 2002 and P. Paolino et al., Rev. Sci. Instrum. 84, 2013), which background noise can reach 10-14 m /√{ Hz } . This method allows us to measure a wide range of viscosities (1 mPa . s to 500 mPa . s) of transparent and opaque fluids using a small sample volume ( 5 mL). In this presentation, I will briefly describe the interferometer developped in ENS Lyon, then explain precisely the microrheology measurements and then compare the experimental results to a model developped by M. Benzaquen. This work is supported financially by the ANR project NANOFLUIDYN (Grant Number ANR-13-BS10-0009).

  8. Manufacturing process of nanofluidics using afm probe

    NASA Astrophysics Data System (ADS)

    Karingula, Varun Kumar

    A new process for fabricating a nano fluidic device that can be used in medical application is developed and demonstrated. Nano channels are fabricated using a nano tip in indentation mode on AFM (Atomic Force Microscopy). The nano channels are integrated between the micro channels and act as a filter to separate biomolecules. Nano channels of 4 to7 m in length, 80nm in width, and at varying depths from 100nm to 850 nm allow the resulting device to separate selected groups of lysosomes and other viruses. Sharply developed vertical micro channels are produced from a deep reaction ion etching followed by deposition of different materials, such as gold and polymers, on the top surface, allowing the study of alternative ways of manufacturing a nanofluidic device. PDMS (Polydimethylsiloxane) bonding is performed to close the top surface of the device. An experimental setup is used to test and validate the device by pouring fluid through the channels. A detailed cost evaluation is conducted to compare the economical merits of the proposed process. It is shown that there is a 47:7% manufacturing time savings and a 60:6% manufacturing cost savings.

  9. BOREAS AFM-07 SRC Surface Meteorological Data

    NASA Technical Reports Server (NTRS)

    Osborne, Heather; Hall, Forrest G. (Editor); Newcomer, Jeffrey A. (Editor); Young, Kim; Wittrock, Virginia; Shewchuck, Stan; Smith, David E. (Technical Monitor)

    2000-01-01

    The Saskatchewan Research Council (SRC) collected surface meteorological and radiation data from December 1993 until December 1996. The data set comprises Suite A (meteorological and energy balance measurements) and Suite B (diffuse solar and longwave measurements) components. Suite A measurements were taken at each of ten sites, and Suite B measurements were made at five of the Suite A sites. The data cover an approximate area of 500 km (North-South) by 1000 km (East-West) (a large portion of northern Manitoba and northern Saskatchewan). The measurement network was designed to provide researchers with a sufficient record of near-surface meteorological and radiation measurements. The data are provided in tabular ASCII files, and were collected by Aircraft Flux and Meteorology (AFM)-7. The surface meteorological and radiation data are available from the Earth Observing System Data and Information System (EOSDIS) Oak Ridge National Laboratory (ORNL) Distributed Active Archive Center (DAAC). The data files are available on a CD-ROM (see document number 20010000884).

  10. Effect of interlayer sliding on the estimation of elastic modulus of multilayer graphene in nanoindentation simulation

    NASA Astrophysics Data System (ADS)

    Han, Jihoon; Ryu, Seunghwa; Kim, Dong-Kyu; Woo, Wanchuck; Sohn, Dongwoo

    2016-06-01

    Nanoindentation experiments and simulations are carried out to estimate the elastic modulus of freely-suspended-multilayer graphene. However, due to the difficulty of clamping all layers of multilayer graphene in experiments, and to the ambiguity of imposing the clamped boundary conditions in numerical simulations, the estimated values of elastic modulus exhibit large variation. In particular, interlayer sliding can affect the estimation of elastic modulus. From a series of molecular dynamics simulations, we demonstrate that the estimated elastic modulus of multilayer graphene depends on the level of interlayer sliding involved in boundary conditions. Under fully clamped boundary conditions that prevent interlayer sliding, the elastic modulus is constant regardless of the number of layers. In contrast, under weakly clamped boundary conditions that involve interlayer sliding, the elastic modulus decreases with increasing number of layers. In the case of weakly clamped conditions, a few wrinkles form in the interlayer and then coalesce into a single large wrinkle due to interlayer sliding. Our findings provide an understanding of the variation of elastic modulus observed in other experimental and numerical studies.

  11. Reducing the nucleation barrier in magnetocaloric Heusler alloys by nanoindentation

    NASA Astrophysics Data System (ADS)

    Niemann, R.; Hahn, S.; Diestel, A.; Backen, A.; Schultz, L.; Nielsch, K.; Wagner, M. F.-X.; Fähler, S.

    2016-06-01

    Magnetocaloric materials are promising as solid state refrigerants for more efficient and environmentally friendly cooling devices. The highest effects have been observed in materials that exhibit a first-order phase transition. These transformations proceed by nucleation and growth which lead to a hysteresis. Such irreversible processes are undesired since they heat up the material and reduce the efficiency of any cooling application. In this article, we demonstrate an approach to decrease the hysteresis by locally changing the nucleation barrier. We created artificial nucleation sites and analyzed the nucleation and growth processes in their proximity. We use Ni-Mn-Ga, a shape memory alloy that exhibits a martensitic transformation. Epitaxial films serve as a model system, but their high surface-to-volume ratio also allows for a fast heat transfer which is beneficial for a magnetocaloric regenerator geometry. Nanoindentation is used to create a well-defined defect. We quantify the austenite phase fraction in its proximity as a function of temperature which allows us to determine the influence of the defect on the transformation.

  12. Nanoindentation of functionally graded hybrid polymer/metal thin films

    NASA Astrophysics Data System (ADS)

    Nunes, J.; Piedade, A. P.

    2013-11-01

    Hybrid functionally graded coatings (2D-FGC) were deposited by magnetron co-sputtering from poly(tetrafluoroethylene) (PTFE) and AISI 316L stainless steel (316L) targets. The carbon and fluorine content varied from 7.3 to 23.7 at.% and from 0 to 57 at.%, respectively. The surface modification was developed to change the surface of 316L vascular stents in order to improve the biocompatibility of the outmost layer of the metallic biomaterial. In-depth XPS analysis revealed the presence of a graded chemical composition accompanied by the variation of the film structure. These results were complemented by those of transmission electron microscopy (TEM) analysis that highlighted the nanocomposite nature of the coatings. The nanomechanical characterization of 2D-FGC was performed by nanoindentation at several loads on the thin films deposited onto two different steel substrates: 316L and AISI M2. The study allowed establishing 0.7 mN as the load that characterized the coatings without substrate influence. Both hardness and Young modulus decrease with the increase of fluorine content due to the evolution in chemical composition, chemical bonds and structure.

  13. Relationship between model bacterial peptidoglycan network structures and AFM force-distance curves

    NASA Astrophysics Data System (ADS)

    Brown, Aidan; Wickham, Robert; Touhami, Ahmed; Dutcher, John

    2010-03-01

    Recent atomic force microscopy (AFM) measurements have involved pulling on Gram-negative bacterial sacculi with the AFM tip as a means of distinguishing between different proposed structures of the peptidoglycan network. The goal of the present study is to provide the theoretical connection between a given network structure and its response to the pulling force. We model the glycan strands as hinged rods, and the peptide cross-links as wormlike chains. Using Monte Carlo simulation to equilibrate the three-dimensional network, subject to a fixed AFM tip-to-substrate distance, we can compute the force exerted by the network on the AFM tip. The effects of adhesion of the sacculi to the substrate and enzymatic action on the network are included. We have modeled both the layered and the scaffold model for the peptidoglycan network structure. We have compared our theoretical force-distance curves for each network structure with experimental curves to determine which structure provides the best agreement with experiment.

  14. Segmental calibration for commercial AFM in vertical direction

    NASA Astrophysics Data System (ADS)

    Shi, Yushu; Gao, Sitian; Lu, Mingzhen; Li, Wei; Xu, Xuefang

    2013-01-01

    Atomic force microscopy (AFM) is most widely applied in scientific research and industrial production. AFM is a scanning probe imaging and measuring device, useful for physical and chemical studies. Depends on its basic structure, microscopic surface pattern can be measured and captured by mechanically scanning. Its vertical and horizon resolution can reach to 0.01nm and 0.1nm. Commonly the measurement values of commercial AFM are directly from scanning piezoelectric tube, so that it not a traceable value. In order to solve the problem of commercial AFM's traceability, step height standard references are applied to calibrate the piezoelectric ceramic housing in scanning tube. All of the serial of step height standard references, covering the commercial AFM vertical scale, are calibrated by Metrology AFM developed by National Institute of Metrology (NIM), China. Three interferometers have been assembled in its XYZ axis, therefore the measurement value can directly trace to laser wavelength. Because of nonlinear characteristic of PZT, the method of segmental calibration is proposed. The measurement scale can be divided into several subsections corresponding to the calibrated values of the series of step height standards references. By this method the accuracy of measurements can be ensured in each segment measurement scale and the calibration level of the whole instrument can be promoted. In order to get a standard step shape by commercial AFM, substrate removal method is applied to deal with the bow shape problem.

  15. Modeling the Nano-indentation of Self-healing Materials

    NASA Astrophysics Data System (ADS)

    Duki, Solomon F.; Kolmakov, German V.; Yashin, Victor V.; Kowalewski, Tomasz; Matyjaszewski, Krzysztof; Balazs, Anna C.

    2011-03-01

    We use computational modeling to determine the mechanical response of crosslinked nanogels to an atomic force microscope (AFM) tip that is moved through the sample. We focus on two-dimensional systems where the nanogels are interconnected by both strong and labile bonds. We model each nanogel as a deformable particle using the modified lattice spring model that is applicable to a broad range of elastic materials.We utilize the Bell model to describe the bonds between these nanogel particles, and subsequently, simulate the rupturing of bonds due the force exerted by the moving indenter. The ruptured labile bonds can readily reform and thus, can effectively mend the cavities formed by the moving AFM tip. We determine how the fraction of labile bonds, the nanogel stiffness, and the size and velocity of the moving tip affect the self-healing behavior of the material. We find that samples containing just 10 % of labile bonds can heal to approximately 90 % of their original, undeformed morphology.

  16. Raman and AFM study of gamma irradiated plastic bottle sheets

    SciTech Connect

    Ali, Yasir; Kumar, Vijay; Dhaliwal, A. S.; Sonkawade, R. G.

    2013-02-05

    In this investigation, the effects of gamma irradiation on the structural properties of plastic bottle sheet are studied. The Plastic sheets were exposed with 1.25MeV {sup 60}Co gamma rays source at various dose levels within the range from 0-670 kGy. The induced modifications were followed by micro-Raman and atomic force microscopy (AFM). The Raman spectrum shows the decrease in Raman intensity and formation of unsaturated bonds with an increase in the gamma dose. AFM image displays rough surface morphology after irradiation. The detailed Raman analysis of plastic bottle sheets is presented here, and the results are correlated with the AFM observations.

  17. Dynamics of the nanoneedle probe in trolling mode AFM.

    PubMed

    Abdi, Ahmad; Pishkenari, Hossein Nejat; Keramati, Ramtin; Minary-Jolandan, Majid

    2015-05-22

    Atomic force microscopy (AFM), as an indispensable tool for nanoscale characterization, presents major drawbacks for operation in a liquid environment arising from the large hydrodynamic drag on the vibrating cantilever. The newly introduced 'Trolling mode' (TR-mode) AFM resolves this complication by using a specialized nanoneedle cantilever that keeps the cantilever outside of the liquid. Herein, a mechanical model with a lumped mass was developed to capture the dynamics of such a cantilever with a nanoneedle tip. This new developed model was applied to investigate the effects of the needle-liquid interface on the performance of the AFM, including the imaging capability in liquid. PMID:25915451

  18. AFM Studies of Conformational Changes in Proteins and Peptides

    NASA Astrophysics Data System (ADS)

    Ploscariu, Nicoleta; Sukthankar, Pinakin; Tomich, John; Szoszkiewicz, Robert

    2015-03-01

    Here, we present estimates of molecular stiffness and mechanical energy dissipation factors for some examples of proteins and peptides. The results are obtained from AFM force spectroscopy measurements. To determine molecular stiffness and mechanical energy dissipation factors we developed a model based on measuring several resonance frequencies of an AFM cantilever in contact with either single protein molecule or peptides adsorbed on arbitrary surface. We used compliant AFM cantilevers with a small aspect ratio - a ratio of length to width - in air and in liquid, including biologically relevant phosphate buffered saline medium. Department of Physics.

  19. Extraction of flow properties of single crystal silicon carbide by nanoindentation and finite element simulation

    SciTech Connect

    Shim, Sang Hoon; Jang, Jae-il; Pharr, George Mathews

    2008-01-01

    A method is presented for estimating the plastic flow behavior of single crystal silicon carbide by nanoindentation experiments using a series of triangular pyramidal indenters with different centerline-to-face angles (35.3?to 75?in this work) in combination with 2-dimensional axisymmetric finite element (FE) simulations. The method is based on Tabor's concepts of characteristic strain, e_char, and constraint factor, C_q, which allow indentation hardness values obtained with indenters of different angles to be related to the flow properties of the indented material. The procedure utilizes FE simulations applied in an iterative manner in order to establish the yield strength and work hardening exponent from the experimentally measured dependence of the hardness on indenter angle. The methodology is applied to a hard, brittle ceramic material, 6H SiC, whose flow behavior cannot be determined by conventional tension or compression testing. It is shown that the friction between the indenter and the material plays a significant role, especially for very sharp indenters.

  20. Simultaneous nanoindentation and electron tunneling through alkanethiol self-assembled monolayers.

    PubMed

    Engelkes, Vincent B; Frisbie, C Daniel

    2006-05-25

    Electrical tunnel junctions consisting of alkanethiol molecules self-assembled on Au-coated Si substrates and contacted with Au-coated atomic force microscopy tips were characterized under varying junction loads in a conducting-probe atomic force microscopy configuration. Junction load was cycled in the fashion of a standard nanoindentation experiment; however, junction conductance rather than probe depth was measured directly. The junction conductance data have been analyzed with typical contact mechanics (Derjaguin-Müller-Toporov) and tunneling equations to extract the monolayer modulus (approximately 50 GPa), the contact transmission (approximately 2 x 10(-6)), contact area, and probe depth as a function of load. The monolayers are shown to undergo significant plastic deformation under compression, yielding indentations approximately 7 Angstroms deep for maximum junction loads of approximately 50 nN. Comparison of mechanical properties for different chain lengths was also performed. The film modulus decreased with the number of carbons in the molecular chain for shorter-chain films. This trend abruptly reversed once 12 carbons were present along the backbone. PMID:16706460

  1. Delamination analysis of metal-ceramic multilayer coatings subject to nanoindentation

    DOE PAGESBeta

    Jamison, Ryan Dale; Shen, Yu -Lin

    2016-01-22

    Internal damage has been experimentally observed in aluminum (Al)/silicon carbide (SiC) multilayer coatings subject to nanoindentation loading. Post-indentation characterization has identified that delamination at the coating/substrate interface is the most prominent form of damage. In this study the finite element method is employed to study the effect of delamination on indentation-derived hardness and Young's modulus. The model features alternating Al/SiC nanolayers above a silicon (Si) substrate, in consistence with the actual material system used in earlier experiments. Cohesive elements with a traction–separation relationship are used to facilitate delamination along the coating/substrate interface. Delamination is observed numerically to be sensitive tomore » the critical normal and shear stresses that define the cohesive traction–separation behavior. Axial tensile stress below the edge of indentation contact is found to be the largest contributor to damage initiation and evolution. Delamination results in a decrease in both indentation-derived hardness and Young's modulus. As a result, a unique finding is that delamination can occur during the unloading process of indentation, depending on the loading condition and critical tractions.« less

  2. Single versus successive pop-in modes in nanoindentation tests of single crystals

    DOE PAGESBeta

    Xia, Yuzhi; Gao, Yanfei; Pharr, George M.; Bei, Hongbin

    2016-05-24

    From recent nanoindentation experiments, two types of pop-in modes have been identified: a single pop-in with a large displacement excursion, or a number of pop-ins with comparable and small displacement excursions. Theoretical analyses are developed here to study the roles played by indenter tip radius, pre-existing defect density, heterogeneous nucleation source type, and lattice resistance on the pop-in modes. The evolution of dislocation structures in earlier pop-ins provides input to modeling a stochastic, heterogeneous mechanism that may be responsible for the subsequent pop-ins. It is found that when the first pop-in occurs near theoretical shear stress, the pop-in mode ismore » determined by the lattice resistance and tip radius. When the first pop-in occurs at low shear stress, whether the successive pop-in mode occurs depends on how the heterogeneous dislocation nucleation source density increases as compared to the increase of the total dislocation density. Lastly, the above transitions are found to correlate well with the ratio of indenter tip radius to the mean spacing of dislocation nucleation sources.« less

  3. Evaluation of radiation hardening in ion-irradiated Fe based alloys by nanoindentation

    NASA Astrophysics Data System (ADS)

    Liu, Xiangbing; Wang, Rongshan; Ren, Ai; Jiang, Jing; Xu, Chaoliang; Huang, Ping; Qian, Wangjie; Wu, Yichu; Zhang, Chonghong

    2014-01-01

    Nanoindentation in combination with ion irradiation offers the possibility to quantify irradiation hardening due to radiation damage. Irradiation experiments for Fe-1.0wt.%Cu alloys, China A508-3 steels, and 16MND5 steels were carried out at about 100 °C by proton and Fe-ions with the energy of 240 keV, 3 MeV respectively. The constant stiffness measurement (CSM) with a diamond Berkovich indenter was used to obtain the depth profile of hardness. The results showed that under 240 keV proton irradiation (peak damage up to 0.5 dpa), Fe-1.0wt.%Cu alloys exhibited the largest hardening (∼55%), 16MND5 steels resided in medium hardening (∼46%), and China A508-3(2) steels had the least hardening (∼10%). Under 3 MeV Fe ions irradiation (peak damage up to 1.37 dpa), both China A508-3(1) and 16MND5 steels showed the same hardening (∼26%). The sequence of irradiation tolerance for these materials is China A508-3(2) > 16MND5 ≈ China A508-3(1) > Fe-1.0wt.%Cu. Based on the determination of the transition depth, the nominal hardness H0irr was also calculated by Kasada method.

  4. Implications of the contact radius to line step (CRLS) ratio in AFM for nanotribology measurements.

    PubMed

    Helt, James M; Batteas, James D

    2006-07-01

    Investigating the mechanisms of defect generation and growth at surfaces on the nanometer scale typically requires high-resolution tools such as the atomic force microscope (AFM). To accurately assess the kinetics and activation parameters of defect production over a wide range of loads (F(z)), the AFM data should be properly conditioned. Generally, AFM wear trials are performed over an area defined by the length of the slow (L(sscan)) and fast scan axes. The ratio of L(sscan) to image resolution (res, lines per image) becomes an important experimental parameter in AFM wear trials because it defines the magnitude of the line step (LS = L(sscan)/res), the distance the AFM tip steps along the slow scan axis. Comparing the contact radius (a) to the line step (LS) indicates that the overlap of successive scans will result unless the contact radius-line step ratio (CRLS) is < or =(1)/(2). If this relationship is not considered, then the scan history (e.g., contact frequency) associated with a single scan is not equivalent at different loads owing to the scaling of contact radius with load (a proportional variant F(z)(1/3)). Here, we present a model in conjunction with empirical wear tests on muscovite mica to evaluate the effects of scan overlap on surface wear. Using the Hertz contact mechanics definition of a, the CRLS model shows that scan overlap pervades AFM wear trials even under low loads. Such findings indicate that simply counting the number of scans (N(scans)) in an experiment underestimates the full history conveyed to the surface by the tip and translates into an error in the actual extent to which a region on the surface is contacted. Utilizing the CRLS method described here provides an approach to account for image scan history accurately and to predict the extent of surface wear. This general model also has implications for any AFM measurement where one wishes to correlate scan-dependent history to image properties as well as feature resolution in scanned

  5. Characterization of Local Mechanical Properties of Polymer Thin Films and Polymer Nanocomposites via AFM indentations

    NASA Astrophysics Data System (ADS)

    Cheng, Xu

    AFM indentation has become a tool with great potential in the characterization of nano-mechanical properties of materials. Thanks to the nanometer sized probes, AFM indentation is capable of capturing the changes of multiple properties within the range of tens of nanometers, such task would otherwise be difficult by using other experiment instruments. Despite the great potentials of AFM indentation, it operates based on a simple mechanism: driving the delicate AFM probe to indent the sample surface, and recording the force-displacement response. With limited information provided by AFM indentation, efforts are still required for any practice to successfully extract the desired nano-scale properties from specific materials. In this thesis, we focus on the mechanical properties of interphase between polymer and inorganic materials. It is known that in nanocomposites, a region of polymer exist around nanoparticles with altered molecular structures and improved properties, which is named as interphase polymer. The system with polymer thin films and inorganic material substrates is widely used to simulate the interphase effect in nanocomposites. In this thesis, we developed an efficient and reliable method to process film/substrate samples and characterize the changes of local mechanical properties inside the interphase region with ultra-high resolution AFM mechanical mapping technique. Applying this newly developed method, the interphase of several film/substrate pairs were examined and compared. The local mechanical properties on the other side of the polymer thin film, the free surface side, was also investigated using AFM indentation equipped with surface modified probes. In order to extract the full spectrum of local elastic modulus inside the surface region in the range of only tens of nanometers, the different contact mechanics models were studied and compared, and a Finite Element model was also established. Though the film/substrate system has been wide used as

  6. Ability of Lactobacillus rhamnosus GAF01 to remove AFM1 in vitro and to counteract AFM1 immunotoxicity in vivo.

    PubMed

    Abbès, Samir; Salah-Abbès, Jalila Ben; Sharafi, Hakimeh; Jebali, Rania; Noghabi, Kambiz Akbari; Oueslati, Ridha

    2013-01-01

    Aflatoxin M1 (AFM1) has been detected in many parts of the world both in raw milk and many dairy products, causing great economic losses and human disease. Unfortunately, there are few studies dealing with AFM1 immunotoxicity/interactions with lactic acid bacteria for potential application as a natural preventive agent. The aim of this study was to isolate (from dairy products) food-grade probiotic bacteria able to degrade/bind AFM1 in vitro and evaluate whether the same organism(s) could impart a protective role against AFM1-induced immunotoxicity in exposed Balb/c mice. Bacteria (Lactobacillus plantarum MON03 and L. rhamnosus GAF01) were isolated from Tunisian artisanal butter and then tested for abilities to eliminate AFM1 from phosphate-buffered saline (PBS) and reconstituted milk (containing 0.05, 0.10, and 0.20 µg AFM1/ml) after 0, 6, and 24 h at 37°C. Results showed that the selected bacteria could 'remove' AFM1 both in PBS and skimmed milk. The binding abilities of AFM1 by L. plantarum MON03 and L. rhamnosus GAF01 strains (at 10(8) CFU/ml) in PBS and reconstituted milk ranged, respectively, from 16.1-78.6% and 15.3-95.1%; overall, L. rhamnosus showed a better potential for removal than L. plantarum. 'Removal' appeared to be by simple binding; the bacteria/AFM1 complex was stable and only a very small proportion of mycotoxin was released back into the solution. L. rhamnosus GAF01 had the highest binding capacity and was selected for use in the in vivo study. Those results indicated that use of the organism prevented AFM1-induced effects on total white and red blood cells, and lymphocyte subtypes, after 15 days of host treatment. These studies clearly indicated that L. rhamnosus GAF01 was able to bind AFM1 in vitro and-by mechanisms that might also be related to a binding effect-counteract AFM1-induced immunotoxicity. Moreover, by itself, this bacterium was not toxic and could potentially be used as an additive in dairy products and in biotechnology for

  7. Atomic force microscopy combined with optical tweezers (AFM/OT)

    NASA Astrophysics Data System (ADS)

    Pierini, F.; Zembrzycki, K.; Nakielski, P.; Pawłowska, S.; Kowalewski, T. A.

    2016-02-01

    The role of mechanical properties is essential to understand molecular, biological materials, and nanostructures dynamics and interaction processes. Atomic force microscopy (AFM) is the most commonly used method of direct force evaluation, but due to its technical limitations this single probe technique is unable to detect forces with femtonewton resolution. In this paper we present the development of a combined atomic force microscopy and optical tweezers (AFM/OT) instrument. The focused laser beam, on which optical tweezers are based, provides us with the ability to manipulate small dielectric objects and to use it as a high spatial and temporal resolution displacement and force sensor in the same AFM scanning zone. We demonstrate the possibility to develop a combined instrument with high potential in nanomechanics, molecules manipulation and biological studies. AFM/OT equipment is described and characterized by studying the ability to trap dielectric objects and quantifying the detectable and applicable forces. Finally, optical tweezers calibration methods and instrument applications are given.

  8. Nanoscale structural features determined by AFM for single virus particles.

    PubMed

    Chen, Shu-wen W; Odorico, Michael; Meillan, Matthieu; Vellutini, Luc; Teulon, Jean-Marie; Parot, Pierre; Bennetau, Bernard; Pellequer, Jean-Luc

    2013-11-21

    In this work, we propose "single-image analysis", as opposed to multi-image averaging, for extracting valuable information from AFM images of single bio-particles. This approach allows us to study molecular systems imaged by AFM under general circumstances without restrictions on their structural forms. As feature exhibition is a resolution correlation, we have performed AFM imaging on surfaces of tobacco mosaic virus (TMV) to demonstrate variations of structural patterns with probing resolution. Two AFM images were acquired with the same tip at different probing resolutions in terms of pixel width, i.e., 1.95 and 0.49 nm per pixel. For assessment, we have constructed an in silico topograph based on the three-dimensional crystal structure of TMV as a reference. The prominent artifacts observed in the AFM-determined shape of TMV were attributed to tip convolutions. The width of TMV rod was systematically overestimated by ~10 nm at both probing resolutions of AFM. Nevertheless, the effects of tip convolution were less severe in vertical orientation so that the estimated height of TMV by AFM imaging was in close agreement with the in silico X-ray topograph. Using dedicated image processing algorithms, we found that at low resolution (i.e., 1.95 nm per pixel), the extracted surface features of TMV can be interpreted as a partial or full helical repeat (three complete turns with ~7.0 nm in length), while individual protein subunits (~2.5 nm) were perceivable only at high resolution. The present study shows that the scales of revealed structural features in AFM images are subject to both probing resolution and processing algorithms for image analysis. PMID:24056758

  9. Comparison of mechanical testing methods for biomaterials: Pipette aspiration, nanoindentation, and macroscale testing.

    PubMed

    Buffinton, Christine Miller; Tong, Kelly J; Blaho, Roberta A; Buffinton, Elise M; Ebenstein, Donna M

    2015-11-01

    Characterization of the mechanical properties of biological materials is often complicated by small volume, irregular geometry, fragility, and environmental sensitivity. Pipette aspiration and nanoindentation testing deal well with these limitations and have seen increasing use in biomaterial characterization, but little research has been done to systematically validate these techniques for soft materials. This study compared the results of pipette aspiration, nanoindentation, and bulk uniaxial tension and compression in determining the small-strain elastic moduli of a range of biomedically-relevant materials, a series of silicone elastomers and polyacrylamide hydrogels. A custom apparatus was developed for pipette aspiration testing, a commercial Hysitron instrument with custom spherical tip was used for nanoindentation, and standard commercial machines were used for tension and compression testing. The measured small-strain elastic moduli ranged from 27 to 368 kPa for the silicones and 11 to 44 kPa for the polyacrylamide gels. All methods detected expected trends in material stiffness, except for the results from one inconsistent silicone. Pipette aspiration and nanoindentation measured similar elastic moduli for silicone materials, but pipette aspiration measured consistently larger stiffness in the hydrogels, which may be explained by the gels' resistance to tension. Despite the difference in size scale among the testing methods, size does not appear to influence the results. These results suggest that both pipette aspiration and nanoindentation are suitable for measuring mechanical properties of soft biomaterials and appear to have no more limitations than bulk techniques. PMID:26295450

  10. Strength and Mechanical Response of NaCl Using In-Situ Transmission Electron Microscopy Compression and Nanoindentation.

    PubMed

    Lin, Kai-Peng; Fang, Te-Hua; Kang, Sho-Hui

    2016-03-01

    Strength and mechanical properties of single crystal sodium chloride (NaCl) are characterized. Critical deformation variations of NaCl pillared structures and films are estimated using in-situ transmission electron microscope (TEM) compression tests and nanoindentation experiments. Young's modulus and contact stiffness of NaCl pillars with diameters of 300 to 500 nm were 10.4-23.9 GPa, and 159-230 N/m, respectively. The nanohardness and Vickers hardness of the NaCl (001) film were 282-596 and 196-260 MPa, respectively. The results could provide useful information for understanding the mechanical properties, contact and local deformation of NaCl pillars and films. PMID:27455676

  11. Characterization of ion beam irradiated 304 stainless steel utilizing nanoindentation and Laue microdiffraction

    NASA Astrophysics Data System (ADS)

    Lupinacci, A.; Chen, K.; Li, Y.; Kunz, M.; Jiao, Z.; Was, G. S.; Abad, M. D.; Minor, A. M.; Hosemann, P.

    2015-03-01

    Characterizing irradiation damage in materials utilized in light water reactors is critical for both material development and application reliability. Here we use both nanoindentation and Laue microdiffraction to characterize both the mechanical response and microstructure evolution due to irradiation. Two different irradiation conditions were considered in 304 stainless steel: 1 dpa and 10 dpa. In addition, an annealed condition of the 10 dpa specimen for 1 h at 500 °C was evaluated. Nanoindentation revealed an increase in hardness due to irradiation and also revealed that hardness saturated in the 10 dpa case. Broadening using Laue microdiffraction peaks indicates a significant plastic deformation in the irradiated area that is in good agreement with both the SRIM calculations and the nanoindentation results.

  12. Nanoindentation Study of Resin Impregnated Sandstone and Early-Age Cement Paste Specimens

    NASA Astrophysics Data System (ADS)

    Zhu, W.; Fonteyn, M. T. J.; Hughes, J.; Pearce, C.

    Nanoindentation testing requires well prepared samples with a good surface finish. Achieving a good surface finish is difficult for heterogeneous materials, particularly those with weak and fragile structures/phases, which are easily damaged or lost during preparation. The loss of weak structures can be drastically reduced by impregnating the sample with a resin before cutting and polishing. This technique is commonly used in SEM microscopy but has not been used for nanoindentation-testing before. This paper reports an investigation to extract micro-mechanical properties of different phases in resin impregnated sandstone and 1-day hydrated cement samples. The results appeared to show that it is feasible to use resin impregnated specimens for nanoindentation study of both materials.

  13. Experimental determination of micromachined discrete and continuous device spring constants using nanoindentation method

    NASA Astrophysics Data System (ADS)

    Chan, M. L.; Tay, Francis E.; Logeeswaran, V. J.; Zeng, Kaiyang; Shen, Lu; Chau, Fook S.

    2002-04-01

    A rapid and accurate static and quasi-static method for determining the out-of-plane spring constraints of cantilevers and a micromachined vibratory sensor is presented. In the past, much of the effort in nanoindentation application was to investigate the thin-film mechanical properties. In this paper, we have utilized the nanoindentation method to measure directly some micromachined device (e.g. microgyroscope) spring constants. The cantilevers and devices tested were fabricated using the MUMPS process and an SOI process (patent pending). Spring constants are determined using a commercial nanoindentation apparatus UMIS-2000 configured with both Berkovich and spherical indenter tip that can be placed onto the device with high accuracy. Typical load resolution is 20micrometers N to 0.5N and a displacement resolution of 0.05nm. Information was deduced from the penetration depth versus load curves during both loading and unloading.

  14. Relationship between Yield Point Phenomena and the Nanoindentation Pop-in Behavior of Steel

    SciTech Connect

    Ahn, T.-H.; Oh, C.-S.; Lee, K.; George, Easo P; Han, H. N.

    2012-01-01

    Pop-ins on nanoindentation load-displacement curves of a ferritic steel were correlated with yield drops on its tensile stress-strain curves. To investigate the relationship between these two phenomena, nanoindentation and tensile tests were performed on annealed specimens, prestrained specimens, and specimens aged for various times after prestraining. Clear nanoindentation pop-ins were observed on annealed specimens, which disappeared when specimens were indented right after the prestrain, but reappeared to varying degrees after strain aging. Yield drops in tensile tests showed similar disappearance and appearance, indicating that the two phenomena, at the nano- and macro-scale, respectively, are closely related and influenced by dislocation locking by solutes (Cottrell atmospheres).

  15. Study of relaxation and transport processes by means of AFM based dielectric spectroscopy

    SciTech Connect

    Miccio, Luis A.

    2014-05-15

    Since its birth a few years ago, dielectric spectroscopy studies based on atomic force microscopy (AFM) have gained a growing interest. Not only the frequency and temperature ranges have become broader since then but also the kind of processes that can be studied by means of this approach. In this work we analyze the most adequate experimental setup for the study of several dielectric processes with a spatial resolution of a few nanometers by using force mode AFM based dielectric spectroscopy. Proof of concept experiments were performed on PS/PVAc blends and PMMA homopolymer films, for temperatures ranging from 300 to 400 K. Charge transport processes were also studied by this approach. The obtained results were analyzed in terms of cantilever stray contribution, film thickness and relaxation strength. We found that the method sensitivity is strongly coupled with the film thickness and the relaxation strength, and that it is possible to control it by using an adequate experimental setup.

  16. Atomic-scale microstructure underneath nanoindentation in Al-Cr-N ceramic films

    NASA Astrophysics Data System (ADS)

    Zhuang, Chunqiang; Li, Zhipeng; Lin, Songsheng

    2015-12-01

    In this work, Al-Cr-N ceramic films deformed by nanoindentation were peeled off from silicon substrates and their atomic-scale microstructures underneath the indenter were investigated by high resolution transmission electron microscope (HR-TEM). Dislocations were formed underneath the indenter and they accumulated along nano-grain boundaries. The accumulative dislocations triggered the crack initiation along grain boundaries, and further resulted in the crack propagation. Dislocations were also observed in nano-grains on the lateral contact area. A model was proposed to describe the variation of microstructures under nanoindentation.

  17. Atomic-scale microstructure underneath nanoindentation in Al-Cr-N ceramic films

    SciTech Connect

    Zhuang, Chunqiang Li, Zhipeng; Lin, Songsheng

    2015-12-15

    In this work, Al-Cr-N ceramic films deformed by nanoindentation were peeled off from silicon substrates and their atomic-scale microstructures underneath the indenter were investigated by high resolution transmission electron microscope (HR-TEM). Dislocations were formed underneath the indenter and they accumulated along nano-grain boundaries. The accumulative dislocations triggered the crack initiation along grain boundaries, and further resulted in the crack propagation. Dislocations were also observed in nano-grains on the lateral contact area. A model was proposed to describe the variation of microstructures under nanoindentation.

  18. Cleaning of diamond nanoindentation probes with oxygen plasma and carbon dioxide snow

    SciTech Connect

    Morris, Dylan J.

    2009-12-15

    Diamond nanoindentation probes may perform thousands of indentations over years of service life. There is a broad agreement that the probes need frequent cleaning, but techniques for doing so are mostly anecdotes shared between experimentalists. In preparation for the measurement of the shape of a nanoindentation probe by a scanning probe microscope, cleaning by carbon dioxide snow jets and oxygen plasma was investigated. Repeated indentation on a thumbprint-contaminated surface formed a compound that was very resistant to removal by solvents, CO{sub 2} snow, and plasma. CO{sub 2} snow cleaning is found to be a generally effective cleaning procedure.

  19. Cellular mechanoadaptation to substrate mechanical properties: contributions of substrate stiffness and thickness to cell stiffness measurements using AFM.

    PubMed

    Vichare, Shirish; Sen, Shamik; Inamdar, Mandar M

    2014-02-28

    Mechanosensing by adherent cells is usually studied by quantifying cell responses on hydrogels that are covalently linked to a rigid substrate. Atomic force microscopy (AFM) represents a convenient way of characterizing the mechanoadaptation response of adherent cells on hydrogels of varying stiffness and thickness. Since AFM measurements reflect the effective cell stiffness, therefore, in addition to measuring real cytoskeletal alterations across different conditions, these measurements might also be influenced by the geometry and physical properties of the substrate itself. To better understand how the physical attributes of the gel influence AFM stiffness measurements of cells, we have used finite element analysis to simulate the indentation of cells of various spreads resting on hydrogels of varying stiffness and thickness. Consistent with experimental results, our simulation results indicate that for well spread cells, stiffness values are significantly over-estimated when experiments are performed on cells cultured on soft and thin gels. Using parametric studies, we have developed scaling relationships between the effective stiffness probed by AFM and the bulk cell stiffness, taking cell and tip geometry, hydrogel properties, nuclear stiffness and cell contractility into account. Finally, using simulated mechanoadaptation responses, we have demonstrated that a cell stiffening response may arise purely due to the substrate properties. Collectively, our results demonstrate the need to take hydrogel properties into account while estimating cell stiffness using AFM indentation. PMID:24651595

  20. Nanoindentation of Isometric Viruses on Deterministically Corrugated Substrates.

    PubMed

    Hernando-Pérez, M; Zeng, C; Delalande, L; Tsvetkova, I B; Bousquet, A; Tayachi-Pigeonnat, M; Temam, R; Dragnea, B

    2016-01-21

    It has been just over 100 years since inventor Joseph Coyle perfected the egg carton-a package format that has known very little changes since its first appearance ( Dhillon , S. B. C. Inventor Created Better Way to Carry Eggs. In The Globe and Mail Vancouver , 2013 ). In this article, we extend Coyle's old idea to the study of mechanical properties of viruses. Virus stiffness, strength, and breaking force obtained by force spectroscopy atomic force microscopy (AFM) provide the knowledge required for designing nanocontainers for applications in biotechnology and medicine, and for understanding the fundamentals of virus-host interaction such as virus translocation from one cellular compartment to another. In previous studies, virus particles adsorbed on flat surfaces from a physiological buffer were subjected to directional deformation by a known force exerted via a microscopic probe. The affinity between the virus shell and surface is required to be strong enough to anchor particles on the substrate while they are indented or imaged, yet sufficiently weak to preserve the native structure and interactions prior deformation. The specific question addressed here is whether an experimental scheme characterized by increased contact area and stable mechanical equilibrium under directional compression would provide a more reliable characterization than the traditional flat substrate approach. PMID:26674071

  1. Poroviscoelastic finite element model including continuous fiber distribution for the simulation of nanoindentation tests on articular cartilage.

    PubMed

    Taffetani, M; Griebel, M; Gastaldi, D; Klisch, S M; Vena, P

    2014-04-01

    Articular cartilage is a soft hydrated tissue that facilitates proper load transfer in diarthroidal joints. The mechanical properties of articular cartilage derive from its structural and hierarchical organization that, at the micrometric length scale, encompasses three main components: a network of insoluble collagen fibrils, negatively charged macromolecules and a porous extracellular matrix. In this work, a constituent-based constitutive model for the simulation of nanoindentation tests on articular cartilage is presented: it accounts for the multi-constituent, non-linear, porous, and viscous aspects of articular cartilage mechanics. In order to reproduce the articular cartilage response under different loading conditions, the model considers a continuous distribution of collagen fibril orientation, swelling, and depth-dependent mechanical properties. The model's parameters are obtained by fitting published experimental data for the time-dependent response in a stress relaxation unconfined compression test on adult bovine articular cartilage. Then, model validation is obtained by simulating three independent experimental tests: (i) the time-dependent response in a stress relaxation confined compression test, (ii) the drained response of a flat punch indentation test and (iii) the depth-dependence of effective Poisson's ratio in a unconfined compression test. Finally, the validated constitutive model has been used to simulate multiload spherical nanoindentation creep tests. Upon accounting for strain-dependent tissue permeability and intrinsic viscoelastic properties of the collagen network, the model accurately fits the drained and undrained curves and time-dependent creep response. The results show that depth-dependent tissue properties and glycosaminoglycan-induced tissue swelling should be accounted for when simulating indentation experiments. PMID:24389384

  2. Imaging resolution of AFM with probes modified with FIB.

    PubMed

    Skibinski, J; Rebis, J; Wejrzanowski, T; Rozniatowski, K; Pressard, K; Kurzydlowski, K J

    2014-11-01

    This study concerns imaging of the structure of materials using AFM tapping (TM) and phase imaging (PI) mode, using probes modified with focused ion beam (FIB). Three kinds of modifications were applied - thinning of the cantilever, sharpening of the tip and combination of these two modifications. Probes shaped in that way were used for AFM investigations with Bruker AFM Nanoscope 8. As a testing material, titanium roughness standard supplied by Bruker was used. The results show that performed modifications influence the oscillation of the probes. In particular thinning of the cantilever enables one to acquire higher self-resonant frequencies, which can be advantageous for improving the quality of imaging in PI mode. It was found that sharpening the tip improves imaging resolution in tapping mode, which is consistent with existing knowledge, but lowered the quality of high frequency topography images. In this paper the Finite Element Method (FEM) was used to explain the results obtained experimentally. PMID:25080273

  3. AFM of biological complexes: what can we learn?

    PubMed Central

    Gaczynska, Maria; Osmulski, Pawel A.

    2009-01-01

    The term “biological complexes” broadly encompasses particles as diverse as multisubunit enzymes, viral capsids, transport cages, molecular nets, ribosomes, nucleosomes, biological membrane components and amyloids. The complexes represent a broad range of stability and composition. Atomic force microscopy offers a wealth of structural and functional data about such assemblies. For this review, we choose to comment on the significance of AFM to study various aspects of biology of selected nonmembrane protein assemblies. Such particles are large enough to reveal many structural details under the AFM probe. Importantly, the specific advantages of the method allow for gathering dynamic information about their formation, stability or allosteric structural changes critical for their function. Some of them have already found their way to nanomedical or nanotechnological applications. Here we present examples of studies where the AFM provided pioneering information about the biology of complexes, and examples of studies where the simplicity of the method is used toward the development of potential diagnostic applications. PMID:19802337

  4. Improvement in metrology on new 3D-AFM platform

    NASA Astrophysics Data System (ADS)

    Schmitz, Ingo; Osborn, Marc; Hand, Sean; Chen, Qi

    2008-10-01

    According to the 2007 edition of the ITRS roadmap, the requirement for CD uniformity of isolated lines on a binary or attenuated phase shift mask is 2.1nm (3σ) in 2008 and requires improvement to1.3 nm (3σ) in 2010. In order to meet the increasing demand for CD uniformity on photo masks, improved CD metrology is required. A next generation AFM, InSightTM 3DAFM, has been developed to meet these increased requirements for advanced photo mask metrology. The new system achieves 2X improvement in CD and depth precision on advanced photo masks features over the previous generation 3D-AFM. This paper provides measurement data including depth, CD, and sidewall angle metrology. In addition the unique capabilities of damage-free defect inspection and Nanoimprint characterization by 3D AFM are presented.

  5. Mounting of Escherichia coli spheroplasts for AFM imaging.

    SciTech Connect

    Sullivan, Claretta J; Morrell-Falvey, Jennifer L; Allison, David P; Doktycz, Mitchel John

    2005-11-01

    The cytoplasmic membrane of Escherichia coli (E. coli) is the location of numerous, chemically specific transporters and recognition elements. Investigation of this membrane in vivo by atomic force microscopy (AFM) requires removal of the cell wall and stable immobilization of the spheroplast. AFM images demonstrate that spheroplasts can be secured with warm gelatin applied to the mica substrate just before the addition of a spheroplast suspension. The resulting preparation can be repeatedly imaged by AFM over the course of several hours. Confocal fluorescence imaging confirms the association of the spheroplasts with the gelatin layer. Gelatin molecules are known to reorder into a network after heating. Entrapment within this gelatin network is believed to be responsible for the immobilization of spheroplasts on mica.

  6. Surface Morphological Studies on Nerve Cells by AFM

    NASA Astrophysics Data System (ADS)

    Durkaya, Goksel; Zhong, Lei; Rehder, Vincent; Dietz, Nikolaus

    2009-03-01

    Surface morphological properties of fixed and living nerve cells removed from the buccal ganglion of Helisoma trivolvis have been studied by using Atomic Force Microscopy (AFM). Identified, individual neurons were removed from the buccal ganglion of Helisoma trivolvis and plated into poly-L-lysine coated glass cover-slips. The growth of the nerve cells was stopped and fixed with 0.1% Glutaraldehyde and 4% Formaldehyde solution after extension of growth cones at the tip of the axons. Topography and softness of growth cone filopodia and overlying lamellopodium (veil) were probed by AFM. Information obtained from AFM's amplitude and phase channels have been used for determination of softness of the region probed. The results of structural studies on the cells are linked to their mechanical properties and internal molecular density distribution.

  7. A low-cost AFM setup with an interferometer for undergraduates and secondary-school students

    NASA Astrophysics Data System (ADS)

    Bergmann, Antje; Feigl, Daniela; Kuhn, David; Schaupp, Manuel; Quast, Günter; Busch, Kurt; Eichner, Ludwig; Schumacher, Jens

    2013-07-01

    Atomic force microscopy (AFM) is an important tool in nanotechnology. This method makes it possible to observe nanoscopic surfaces beyond the resolution of light microscopy. In order to provide undergraduate and secondary-school students with insights into this world, we have developed a very robust low-cost AFM setup with a Fabry-Perot interferometer as a detecting device. This setup is designed to be operated almost completely manually and its simplicity gives access to a profound understanding of the working principle. Our AFM is operated in a constant height mode, i.e. the topography of the sample surface is represented directly by the deflection of the cantilever. Thus, the measuring procedure can be understood even by secondary-school students; furthermore, it is the method with the lowest cost, totalling not more than 10-15 k Euros. Nevertheless, we are able to examine a large variety of sample topographies such as CD and DVD surfaces, IC structures, blood cells, butterfly wings or moth eyes. Furthermore, force-distance curves can be recorded and the tensile moduli of some materials can be evaluated. We present our setup in detail and describe its working principles. In addition, we show various experiments which have already been performed by students.

  8. Fabrication of nanochannels with ladder nanostructure at the bottom using AFM nanoscratching method.

    PubMed

    Yan, Yongda; Geng, Yanquan; Hu, Zhenjiang; Zhao, Xuesen; Yu, Bowen; Zhang, Qi

    2014-01-01

    This letter presents a novel atomic force microscopy (AFM)-based nanomanufacturing method combining the tip scanning with the high-precision stage movement to fabricate nanochannels with ladder nanostructure at the bottom by continuous scanning with a fixed scan size. Different structures can be obtained according to the matching relation of the tip feeding velocity and the precision stage moving velocity. This relationship was first studied in detail to achieve nanochannels with different ladder nanostructures at the bottom. Machining experiments were then performed to fabricate nanochannels on an aluminum alloy surface to demonstrate the capability of this AFM-based fabrication method presented in this study. Results show that the feed value and the tip orientation in the removing action play important roles in this method which has a significant effect on the machined surfaces. Finally, the capacity of this method to fabricate a large-scale nanochannel was also demonstrated. This method has the potential to advance the existing AFM tip-based nanomanufacturing technique of the formation these complex structures by increasing the removal speed, simplifying the processing procedure and achieving the large-scale nanofabrication. PMID:24940171

  9. Fabrication of nanochannels with ladder nanostructure at the bottom using AFM nanoscratching method

    PubMed Central

    2014-01-01

    This letter presents a novel atomic force microscopy (AFM)-based nanomanufacturing method combining the tip scanning with the high-precision stage movement to fabricate nanochannels with ladder nanostructure at the bottom by continuous scanning with a fixed scan size. Different structures can be obtained according to the matching relation of the tip feeding velocity and the precision stage moving velocity. This relationship was first studied in detail to achieve nanochannels with different ladder nanostructures at the bottom. Machining experiments were then performed to fabricate nanochannels on an aluminum alloy surface to demonstrate the capability of this AFM-based fabrication method presented in this study. Results show that the feed value and the tip orientation in the removing action play important roles in this method which has a significant effect on the machined surfaces. Finally, the capacity of this method to fabricate a large-scale nanochannel was also demonstrated. This method has the potential to advance the existing AFM tip-based nanomanufacturing technique of the formation these complex structures by increasing the removal speed, simplifying the processing procedure and achieving the large-scale nanofabrication. PMID:24940171

  10. Defect formation by pristine indenter at the initial stage of nanoindentation

    NASA Astrophysics Data System (ADS)

    Chen, I.-Hsien; Hsiao, Chun-I.; Behera, Rakesh K.; Hsu, Wen-Dung

    2013-12-01

    Nano-indentation is a sophisticated method to characterize mechanical properties of materials. This method samples a very small amount of material during each indentation. Therefore, this method is extremely useful to measure mechanical properties of nano-materials. The measurements using nanoindentation is very sensitive to the surface topology of the indenter and the indenting surfaces. The mechanisms involved in the entire process of nanoindentation require an atomic level understanding of the interplay between the indenter and the substrate. In this paper, we have used atomistic simulation methods with empirical potentials to investigate the effect of various types of pristine indenter on the defect nucleation and growth. Using molecular dynamics simulations, we have predicted the load-depth curve for conical, vickers, and sperical tip. The results are analyzed based on the coherency between the indenter tip and substrate surface for a fixed depth of 20 Å. The depth of defect nucleation and growth is observed to be dependent on the tip geometry. A tip with larger apex angle nucleates defects at a shallower depth. However, the type of defect generated is dependent on the crystalline orientation of the tip and substrate. For coherent systems, prismatic loops were generated, which released into the substrate along the close-packed directions with continued indentation. For incoherent systems, pyramidal shaped dislocation junctions formed in the FCC systems and disordered atomic clusters formed in the BCC systems. These defect nucleation and growth process provide the atomistic mechanisms responsible for the observed load-depth response during nanoindentation.

  11. BOREAS AFM-04 Twin Otter Aircraft Flux Data

    NASA Technical Reports Server (NTRS)

    MacPherson, J. Ian; Hall, Forrest G. (Editor); Knapp, David E. (Editor); Desjardins, Raymond L.; Smith, David E. (Technical Monitor)

    2000-01-01

    The BOREAS AFM-5 team collected and processed data from the numerous radiosonde flights during the project. The goals of the AFM-05 team were to provide large-scale definition of the atmosphere by supplementing the existing AES aerological network, both temporally and spatially. This data set includes basic upper-air parameters collected from the network of upper-air stations during the 1993, 1994, and 1996 field campaigns over the entire study region. The data are contained in tabular ASCII files. The data files are available on a CD-ROM (see document number 20010000884) or from the Oak Ridge National Laboratory (ORNL) Distributed Active Archive Center (DAAC).

  12. GPIM AF-M315E Propulsion System

    NASA Technical Reports Server (NTRS)

    Spores, Ronald A.; Masse, Robert; Kimbrel, Scott; McLean, Chris

    2014-01-01

    The NASA Space Technology mission Directorate's (STMD) Green Propellant Infusion Mission (GPIM) Technology Demonstration Mission (TDM) will demonstrate an operational AF-M315E green propellant propulsion system. Aerojet-Rocketdyne is responsible for the development of the propulsion system payload. This paper statuses the propulsion system module development, including thruster design and system design; Initial test results for the 1N engineering model thruster are presented. The culmination of this program will be high-performance, green AF-M315E propulsion system technology at TRL 7+, with components demonstrated to TRL 9, ready for direct infusion to a wide range of applications for the space user community.

  13. Study of nanoindentation mechanical response of nanocrystalline structures using molecular dynamics simulations

    NASA Astrophysics Data System (ADS)

    Li, Jia; Guo, Jiawen; Luo, Hao; Fang, Qihong; Wu, Hong; Zhang, Liangchi; Liu, Youwen

    2016-02-01

    Molecular dynamics (MD) simulations are performed to study the nanoindentation onto three different crystal structures including the single crystalline, polycrystalline, and nanotwinned polycrystalline copper. To reveal the effects of crystal structure and twin-lamellae-thickness on the response of nanoindentation, we evaluate the evolution of crystalline structure, dislocation, strain, indentation force, temperature, hardness, and elastic recovery coefficient in the deformation zone. The results of MD simulations show that the hardness, elastic recovery ratio and temperature of those three nanocrystalline copper strongly depend on crystal structure and twin-lamellae-thickness. It is also revealed that as nanoindenter goes deeper, the extent of plastic zone becomes substantially larger. Initial dislocation always nucleates at the beneath of indenter, and the discrete drops of indentation force observed at certain indentation depths, indicates dislocation bursts during the indentation process. In particular, the twining and detwining are dominant over the dislocation nucleation in driving plasticity in nanotwinned polycrystalline during nanoindentation, which are in good agreement with the previous work. Furthermore, we find that plastic deformation has a strong dependence on crystal structure. The plastic deformation of the single crystalline copper relies on the generation, propagation and reaction of dislocations, that of the polycrystalline copper depends on the dislocation-grain boundary (GB) interactions, and that of the nanotwinned polycrystalline copper relies upon the dislocation-twin boundary (TB) interactions as well as twining/detwining. This work not only provides insights into the effects of crystal structure and two-lamellae-thickness on the mechanical properties of copper under nanoindentation, but also shed lights onto the guideline of understanding other FCC nanocrystalline materials.

  14. A Method for Measuring the Hardness of the Surface Layer on Hot Forging Dies Using a Nanoindenter

    NASA Astrophysics Data System (ADS)

    Mencin, P.; van Tyne, C. J.; Levy, B. S.

    2009-11-01

    The properties and characteristics of the surface layer of forging dies are critical for understanding and controlling wear. However, the surface layer is very thin, and appropriate property measurements are difficult to obtain. The objective of the present study is to determine if nanoindenter testing provides a reliable method, which could be used to measure the surface hardness in forging die steels. To test the reliability of nanoindenter testing, nanoindenter values for two quenched and tempered steels (FX and H13) are compared to microhardness and macrohardness values. These steels were heat treated for various times to produce specimens with different values of hardness. The heat-treated specimens were tested using three different instruments—a Rockwell hardness tester for macrohardness, a Vickers hardness tester for microhardness, and a nanoindenter tester for fine scale evaluation of hardness. The results of this study indicate that nanoindenter values obtained using a Nanoindenter XP Machine with a Berkovich indenter reliably correlate with Rockwell C macrohardness values, and with Vickers HV microhardness values. Consequently, nanoindenter testing can provide reliable results for analyzing the surface layer of hot forging dies.

  15. AFM CHARACTERIZATION OF LASER INDUCED DAMAGE ON CDZNTE CRYSTAL SURFACES

    SciTech Connect

    Hawkins, S; Lucile Teague, L; Martine Duff, M; Eliel Villa-Aleman, E

    2008-06-10

    Semi-conducting CdZnTe (or CZT) crystals can be used in a variety of detector-type applications. CZT shows great promise for use as a gamma radiation spectrometer. However, its performance is adversely affected by point defects, structural and compositional heterogeneities within the crystals, such as twinning, pipes, grain boundaries (polycrystallinity), secondary phases and in some cases, damage caused by external forces. One example is damage that occurs during characterization of the surface by a laser during Raman spectroscopy. Even minimal laser power can cause Te enriched areas on the surface to appear. The Raman spectra resulting from measurements at moderate intensity laser power show large increases in peak intensity that is attributed to Te. Atomic Force Microscopy (AFM) was used to characterize the extent of damage to the CZT crystal surface following exposure to the Raman laser. AFM data reveal localized surface damage in the areas exposed to the Raman laser beam. The degree of surface damage to the crystal is dependent on the laser power, with the most observable damage occurring at high laser power. Moreover, intensity increases in the Te peaks of the Raman spectra are observed even at low laser power with little to no visible damage observed by AFM. AFM results also suggest that exposure to the same amount of laser power yields different amounts of surface damage depending on whether the exposed surface is the Te terminating face or the Cd terminating face of CZT.

  16. 3D Color Digital Elevation Map of AFM Sample

    NASA Technical Reports Server (NTRS)

    2008-01-01

    This color image is a three dimensional (3D) view of a digital elevation map of a sample collected by NASA's Phoenix Mars Lander's Atomic Force Microscope (AFM).

    The image shows four round pits, only 5 microns in depth, that were micromachined into the silicon substrate, which is the background plane shown in red. This image has been processed to reflect the levelness of the substrate.

    A Martian particle only one micrometer, or one millionth of a meter, across is held in the upper left pit.

    The rounded particle shown at the highest magnification ever seen from another world is a particle of the dust that cloaks Mars. Such dust particles color the Martian sky pink, feed storms that regularly envelop the planet and produce Mars' distinctive red soil.

    The particle was part of a sample informally called 'Sorceress' delivered to the AFM on the 38th Martian day, or sol, of the mission (July 2, 2008). The AFM is part of Phoenix's microscopic station called MECA, or the Microscopy, Electrochemistry, and Conductivity Analyzer.

    The AFM was developed by a Swiss-led consortium, with Imperial College London producing the silicon substrate that holds sampled particles.

    The Phoenix Mission is led by the University of Arizona, Tucson, on behalf of NASA. Project management of the mission is by NASA's Jet Propulsion Laboratory, Pasadena, Calif. Spacecraft development is by Lockheed Martin Space Systems, Denver.

  17. Introduction to Atomic Force Microscopy (AFM) in Biology.

    PubMed

    Kreplak, Laurent

    2016-01-01

    The atomic force microscope (AFM) has the unique capability of imaging biological samples with molecular resolution in buffer solution over a wide range of time scales from milliseconds to hours. In addition to providing topographical images of surfaces with nanometer- to angstrom-scale resolution, forces between single molecules and mechanical properties of biological samples can be investigated from the nano-scale to the micro-scale. Importantly, the measurements are made in buffer solutions, allowing biological samples to "stay alive" within a physiological-like environment while temporal changes in structure are measured-e.g., before and after addition of chemical reagents. These qualities distinguish AFM from conventional imaging techniques of comparable resolution, e.g., electron microscopy (EM). This unit provides an introduction to AFM on biological systems and describes specific examples of AFM on proteins, cells, and tissues. The physical principles of the technique and methodological aspects of its practical use and applications are also described. © 2016 by John Wiley & Sons, Inc. PMID:27479503

  18. AFM Structural Characterization of Drinking Water Biofilm under Physiological Conditions

    EPA Science Inventory

    Due to the complexity of mixed culture drinking water biofilm, direct visual observation under in situ conditions has been challenging. In this study, atomic force microscopy (AFM) revealed the three dimensional morphology and arrangement of drinking water relevant biofilm in air...

  19. In situ Stiffness Adjustment of AFM Probes by Two Orders of Magnitude

    PubMed Central

    de Laat, Marcel Lambertus Cornelis; Pérez Garza, Héctor Hugo; Ghatkesar, Murali Krishna

    2016-01-01

    The choice on which type of cantilever to use for Atomic Force Microscopy (AFM) depends on the type of the experiment being done. Typically, the cantilever has to be exchanged when a different stiffness is required and the entire alignment has to be repeated. In the present work, a method to adjust the stiffness in situ of a commercial AFM cantilever is developed. The adjustment is achieved by changing the effective length of the cantilever by electrostatic pull-in. By applying a voltage between the cantilever and an electrode (with an insulating layer at the point of contact), the cantilever snaps to the electrode, reducing the cantilever’s effective length. An analytical model was developed to find the pull-in voltage of the system. Subsequently, a finite element model was developed to study the pull-in behavior. The working principle of this concept is demonstrated with a proof-of-concept experiment. The electrode was positioned close to the cantilever by using a robotic nanomanipulator. To confirm the change in stiffness, the fundamental resonance frequency of the cantilever was measured for varying electrode positions. The results match with the theoretical expectations. The stiffness was adjusted in situ in the range of 0.2 N/m to 27 N/m, covering two orders of magnitude in one single cantilever. This proof-of-concept is the first step towards a micro fabricated prototype, that integrates the electrode positioning system and cantilever that can be used for actual AFM experiments. PMID:27077863

  20. Microstructure correlation in high-strength steels with continuous stiffness mode nanoindentation results. High-resolution vs. low-resolution nanoindentation

    NASA Astrophysics Data System (ADS)

    Hackney, Stephen A.; Bradley, John R.; Wood, Thomas D.; Miskioglu, Ibrahim

    2013-04-01

    This study utilizes instrumented nanoindentation to compare the mechanical response of a transformation-induced plasticity (TRIP) steel to that of a quench and partition steel (QP). The nanoindenter was operated using continuous stiffness mode, and the microstructure under the indent revealed by chemical etching was examined. Examination of the microstructure in the indents by scanning electron microscopy allows a direct correlation with nanoindentation properties. It is found that the hardness measured at an indentation depth of 1.1 μm is, on average, significantly greater in the QP steel than in the TRIP steel. The continuous hardness measurement also allows the microstructure observed at the center of the indent to be correlated with the hardness values when indentation depths are <0.1 μm. This high-resolution hardness measurement allows for a direct comparison of mechanical response for the individual retained austenite phase particles in the TRIP steel with the strengthening microconstituent in the QP steel. With this methodology, the surprising result is that the TRIP retained austenite particles have a higher hardness than the QP hardening microconstituent. It is proposed that the resolution of the apparent disagreement between the hardness measurements obtained at 1.1 μm depth (QP has the higher hardness) and the 0.1-μm depth hardness measurements of the microconstituents containing retained austenite (TRIP has the higher hardness) lies in the volume fraction of the microconstituent as the QP has a two- to threefold higher volume fraction of hardening phase as compared to TRIP.

  1. STM and AFM; Which is Better for Surface Structural Analysis? Non- contact AFM Studies on Ge/Si(105) Surface

    NASA Astrophysics Data System (ADS)

    Hasegawa, Yukio

    2006-03-01

    Scanning tunneling microscopy (STM) has been utilized to determine surface atomic structure with its highly resolved images. Probing surface electronic states near the Fermi energy (EF), STM images, however, do not necessarily represent the atomic structure of surfaces. It has been believed that atomic force microscopy (AFM) provides us surface topographic images without being disturbed by the electronic states. In order to prove the surpassing performance, we performed noncontact (nc) AFM on the Ge/Si(105) surface [1], which is a facet plane of the ?hut? clusters formed on Ge-deposited Si(001) surface. It is found that STM images taken on the surface, either filled- or empty-state images, do not show all surface atoms because of the electronic effect; some surface atoms have dangling bond states below EF and other surface atoms have states above EF. [2]. In a nc-AFM image, on the other hand, all surface atoms having a dangling bond are observed [3], directly representing an atomic structure of the surface. Electronic information can also be obtained in AFM by using a Kelvin-probe method. From atomically resolved potential profile we obtained, charge transfer among the dangling bond states is directly demonstrated. These results clearly demonstrate that highly-resolved nc-AFM with a Kelvin-probe method is an ideal tool for analysis of atomic structures and electronic properties of surfaces. This work was done in collaboration with T. Eguchi, K. Akiyama, T. An, and M. Ono, ISSP, Univ. Tokyo and JST, Y. Fujikawa and T. Sakurai, IMR. Tohoku Univ. T. Hashimoto, AIST, Y. Morikawa, ISIR, Osaka Univ. K. Terakura, Hokkaido Univ., and M.G. Lagally, University of Wisconsin-Madison. [1] T. Eguchi et al., Phys. Rev. Lett. 93, 266102 (2004). [2] Y. Fujikawa et al., Phys. Rev. Lett. 88, 176101 (2002). [3] T. Eguchi and Y. Hasegawa, Phys. Rev. Lett. 89, 256105 (2002)

  2. Solid State Microstructure of Poly(L-lactide-co-meso-lactide) Copolymers by AFM

    NASA Astrophysics Data System (ADS)

    Kanchanasopa, M.; Manias, E.; Runt, J.

    2002-03-01

    The focus in the present study is on characterization of the lamellar morphology of poly(L-lactide) and two L-lactide/meso-lactide random copolymers containing 3 and 6 the same (Mn = 65,000, PDI = 2) and crystallization behavior is therefore controlled by comonomer content. Degrees of crystallinity and crystallization rates decrease substantially with increasing meso-lactide content in the copolymers. Tapping mode AFM experiments on the surfaces of films, previously isothermally crystallized at selected temperatures, were conducted. Similar experiments were also performed on cross-sections, microtomed from the crystallized films. Tapping force plays an important role in all experiments, particularly for low crystallinity samples. Mean lamellar thicknesses derived from analysis of height images agree well with those determined previously from small-angle x-ray scattering experiments.

  3. Mechanical Characterization of Nanoporous Thin Films by Nanoindentation and Laser-induced Surface Acoustic Waves

    NASA Astrophysics Data System (ADS)

    Chow, Gabriel

    Thin films represent a critical sector of modern engineering that strives to produce functional coatings at the smallest possible length scales. They appear most commonly in semiconductors where they form the foundation of all electronic circuits, but exist in many other areas to provide mechanical, electrical, chemical, and optical properties. The mechanical characterization of thin films has been a continued challenge due foremost to the length scales involved. However, emerging thin films focusing on materials with significant porosity, complex morphologies, and nanostructured surfaces produce additional difficulties towards mechanical analysis. Nanoindentation has been the dominant thin film mechanical characterization technique for the last decade because of the quick results, wide range of sample applicability, and ease of sample preparation. However, the traditional nanoindentation technique encounters difficulties for thin porous films. For such materials, alternative means of analysis are desirable and the lesser known laser-induced surface acoustic wave technique (LiSAW) shows great potential in this area. This dissertation focuses on studying thin, porous, and nanostructured films by nanoindentation and LiSAW techniques in an effort to directly correlate the two methodologies and to test the limits and applicabilities of each technique on challenging media. The LiSAW technique is particularly useful for thin porous films because unlike indentation, the substrate is properly accounted for in the wave motion analysis and no plastic deformation is necessary. Additionally, the use of lasers for surface acoustic wave generation and detection allows the technique to be fully non-contact. This is desirable in the measurement of thin, delicate, and porous films where physical sample probing may not be feasible. The LiSAW technique is also valuable in overcoming nanoscale roughness, particularly for films that cannot be mechanically polished, since typical SAW

  4. Cell visco-elasticity measured with AFM and optical trapping at sub-micrometer deformations.

    PubMed

    Nawaz, Schanila; Sánchez, Paula; Bodensiek, Kai; Li, Sai; Simons, Mikael; Schaap, Iwan A T

    2012-01-01

    The measurement of the elastic properties of cells is widely used as an indicator for cellular changes during differentiation, upon drug treatment, or resulting from the interaction with the supporting matrix. Elasticity is routinely quantified by indenting the cell with a probe of an AFM while applying nano-Newton forces. Because the resulting deformations are in the micrometer range, the measurements will be affected by the finite thickness of the cell, viscous effects and even cell damage induced by the experiment itself. Here, we have analyzed the response of single 3T3 fibroblasts that were indented with a micrometer-sized bead attached to an AFM cantilever at forces from 30-600 pN, resulting in indentations ranging from 0.2 to 1.2 micrometer. To investigate the cellular response at lower forces up to 10 pN, we developed an optical trap to indent the cell in vertical direction, normal to the plane of the coverslip. Deformations of up to two hundred nanometers achieved at forces of up to 30 pN showed a reversible, thus truly elastic response that was independent on the rate of deformation. We found that at such small deformations, the elastic modulus of 100 Pa is largely determined by the presence of the actin cortex. At higher indentations, viscous effects led to an increase of the apparent elastic modulus. This viscous contribution that followed a weak power law, increased at larger cell indentations. Both AFM and optical trapping indentation experiments give consistent results for the cell elasticity. Optical trapping has the benefit of a lower force noise, which allows a more accurate determination of the absolute indentation. The combination of both techniques allows the investigation of single cells at small and large indentations and enables the separation of their viscous and elastic components. PMID:23028915

  5. MD simulation of nanoindentation on (001) and (111) surfaces of Ag-Ni multilayers

    NASA Astrophysics Data System (ADS)

    Zhao, Yinbo; Peng, Xianghe; Fu, Tao; Sun, Rong; Feng, Chao; Wang, Zhongchang

    2015-11-01

    We perform MD simulations of the nanoindentation on (001) and (111) surfaces of Ag-Ni multilayers with different modulation periods, and find that both the hardness and maximum force increase with the increase of modulation period, in agreement with the inverse Hall-Petch relation. A prismatic partial dislocation loop is observed in the Ni(111)/Ag(111) sample when the modulation period is relatively large. We also find that misfit dislocation network shows a square shape for the Ni(111)/Ag(111) interface, while a triangle shape for the Ni(001)/Ag(001) interface. The pyramidal defect zones are also observed in Ni(001)/Ag(001) sample, while the intersecting stacking faults are observed in Ni(111)/Ag(111) sample after dislocation traversing interface. The results offer insights into the nanoindentation behaviors in metallic multilayers, which should be important for clarifying strengthening mechanism in many other multilayers.

  6. The nano-mechanical signature of Ultra High Performance Concrete by statistical nanoindentation techniques

    SciTech Connect

    Sorelli, Luca Constantinides, Georgios; Ulm, Franz-Josef; Toutlemonde, Francois

    2008-12-15

    Advances in engineering the microstructure of cementitious composites have led to the development of fiber reinforced Ultra High Performance Concretes (UHPC). The scope of this paper is twofold, first to characterize the nano-mechanical properties of the phases governing the UHPC microstructure by means of a novel statistical nanoindentation technique; then to upscale those nanoscale properties, by means of continuum micromechanics, to the macroscopic scale of engineering applications. In particular, a combined investigation of nanoindentation, scanning electron microscope (SEM) and X-ray Diffraction (XRD) indicates that the fiber-matrix transition zone is relatively defect free. On this basis, a four-level multiscale model with defect free interfaces allows to accurately determine the composite stiffness from the measured nano-mechanical properties. Besides evidencing the dominant role of high density calcium silicate hydrates and the stiffening effect of residual clinker, the suggested model may become a useful tool for further optimizing cement-based engineered composites.

  7. Modelling the nanomechanical response of a micro particle-matrix system for nanoindentation tests.

    PubMed

    Cao, Yunyi; Duan, Pengfei; Chen, Jinju

    2016-05-13

    A lot of experimental, numerical simulation and analytical modelling work has been done on how the substrate affects the measured hardness and elastic modulus of the coating/substrate system for nanoindentation tests. Little work has been done on the elastic-plastic behaviour of micro particle-matrix systems. Clifford et al have proposed an empirical model to describe the spatially dependent composite modulus during nanoindentation tests for linear elastic particles embedded in a linear elastic matrix. However, no such models have been developed for elastic-plastic composites. In this study, finite element simulations were used to determine the elastic modulus and hardness of hard particles embedded in a soft matrix and vice versa. An extended Clifford model has been developed to determine the elastic modulus and hardness for elastic-plastic composites with various particle shapes and volume fractions. PMID:27041486

  8. Modelling the nanomechanical response of a micro particle–matrix system for nanoindentation tests

    NASA Astrophysics Data System (ADS)

    Cao, Yunyi; Duan, Pengfei; Chen, Jinju

    2016-05-01

    A lot of experimental, numerical simulation and analytical modelling work has been done on how the substrate affects the measured hardness and elastic modulus of the coating/substrate system for nanoindentation tests. Little work has been done on the elastic–plastic behaviour of micro particle–matrix systems. Clifford et al have proposed an empirical model to describe the spatially dependent composite modulus during nanoindentation tests for linear elastic particles embedded in a linear elastic matrix. However, no such models have been developed for elastic–plastic composites. In this study, finite element simulations were used to determine the elastic modulus and hardness of hard particles embedded in a soft matrix and vice versa. An extended Clifford model has been developed to determine the elastic modulus and hardness for elastic–plastic composites with various particle shapes and volume fractions.

  9. Surface hardening induced by high flux plasma in tungsten revealed by nano-indentation

    NASA Astrophysics Data System (ADS)

    Terentyev, D.; Bakaeva, A.; Pardoen, T.; Favache, A.; Zhurkin, E. E.

    2016-08-01

    Surface hardness of tungsten after high flux deuterium plasma exposure has been characterized by nanoindentation. The effect of plasma exposure was rationalized on the basis of available theoretical models. Resistance to plastic penetration is enhanced within the 100 nm sub-surface region, attributed to the pinning of geometrically necessary dislocations on nanometric deuterium cavities - signature of plasma-induced defects and deuterium retention. Sub-surface extension of thereby registered plasma-induced damage is in excellent agreement with the results of alternative measurements. The study demonstrates suitability of nano-indentation to probe the impact of deposition of plasma-induced defects in tungsten on near surface plasticity under ITER-relevant plasma exposure conditions.

  10. Atomistic mechanisms of amorphization during nanoindentation of SiC: A molecular dynamics study

    NASA Astrophysics Data System (ADS)

    Szlufarska, Izabela; Kalia, Rajiv K.; Nakano, Aiichiro; Vashishta, Priya

    2005-05-01

    Atomistic mechanisms underlying the nanoindentation-induced amorphization in SiC crystal has been studied by molecular dynamics simulations on parallel computers. The calculated load-displacement curve consists of a series of load drops, corresponding to plastic deformation, in addition to a shoulder at a smaller displacement, which is fully reversible upon unloading. The peaks in the load-displacement curve are shown to reflect the crystalline structure and dislocation activities under the surface. The evolution of indentation damage and defect accumulation are also discussed in terms of bond angles, local pressure, local shear stress, and spatial rearrangements of atoms. These structural analyses reveal that the defect-stimulated growth and coalescence of dislocation loops are responsible for the crystalline-to-amorphous transition. The shortest-path-ring analysis is effectively employed to characterize nanoindentation-induced structural transformations and dislocation activities.

  11. The adhesion behavior of carbon coating studied by re-indentation during in situ TEM nanoindentation

    NASA Astrophysics Data System (ADS)

    Fan, Xue; Diao, Dongfeng

    2016-01-01

    We report a nanoscale adhesion induced nano-response in terms of re-indentation during in situ transmission electron microscope (TEM) nanoindentation on the carbon coating with silicon substrate. The adhesive force generated with nanoindentation was measured, and re-indentation phenomenon during unloading with displacement sudden drop and external loading force change from tension to compression was found. The occurrence of re-indentation during unloading was ascribed to the adhesive force of the contact interface between the indenter and the coating surface. Adhesion energies released for re-indentation processes were quantitatively analyzed from the re-indentation load-displacement curves, and carbon coating reduced the impact of adhesion for silicon substrate. The adhesion induced nano-response of contact surfaces would affect the reliability and performance of nano devices.

  12. Determination of elastoplastic mechanical properties of the weld and heat affected zone metals in tailor-welded blanks by nanoindentation test

    NASA Astrophysics Data System (ADS)

    Ma, Xiangdong; Guan, Yingping; Yang, Liu

    2015-09-01

    The elastoplastic mechanical properties of the weld and heat affected zone metals have comparatively major impact on the forming process of tailor-welded blanks. A few scholars investigated the elastoplastic mechanical properties of the weld and heat affected zone, but they only simply assumed that it was a uniform distribution elastoplastic material different from the base materials. Four types of tailor-welded blanks which consist of ST12 and 304 stainless steel plates are selected as the research objects, the elastoplastic mechanical properties of the tailor-welded blanks weld and heat affected zone metals are obtained based on the nanoindentation tests, and the Erichsen cupping tests are conducted by combining numerical simulation with physical experiment. The nanoindentation tests results demonstrate that the elastoplastic mechanical properties of the weld and heat affected zone metals are not only different from the base materials, but also varying between the weld metals and the heat affected zone metals. Comparing the Erichsen cupping test resulted from numerical with that from experimental method, it is found that the numerical value of Erichsen cupping test which consider the elastoplastic mechanical properties of the weld and heat affected zone metals have a good agreement with the experimental result, and the relative error is only 4.8%. The proposed research provides good solutions for the inhomogeneous elastoplastic mechanical properties of the tailor-welded blanks weld and heat affected zone metals, and improves the control performance of tailor-welded blanks forming accuracy.

  13. Wedged AFM-cantilevers for parallel plate cell mechanics.

    PubMed

    Stewart, Martin P; Hodel, Adrian W; Spielhofer, Andreas; Cattin, Cedric J; Müller, Daniel J; Helenius, Jonne

    2013-04-01

    The combination of atomic force microscopy (AFM) and optical microscopy has gained popularity for mechanical analysis of living cells. In particular, recent AFM-based assays featuring tipless cantilevers and whole-cell deformation have yielded insights into cellular function, structure, and dynamics. However, in these assays the standard ≈10° tilt of the cantilever prevents uniaxial loading, which complicates assessment of cellular geometry and can cause cell sliding or loss of loosely adherent cells. Here, we describe an approach to modify tipless cantilevers with wedges and, thereby, achieve proper parallel plate mechanics. We provide guidance on material selection, the wedge production process, property and geometry assessment, and the calibration of wedged cantilevers. Furthermore, we demonstrate their ability to simplify the assessment of cell shape, prevent lateral displacement of round cells during compression, and improve the assessment of cell mechanical properties. PMID:23473778

  14. Insights into Epoxy Network Nanostructural Heterogeneity Using AFM-IR.

    PubMed

    Morsch, Suzanne; Liu, Yanwen; Lyon, Stuart B; Gibbon, Simon R

    2016-01-13

    The first direct observation of a chemically heterogeneous nanostructure within an epoxy resin is reported. Epoxy resins comprise the matrix component of many high performance composites, coatings and adhesives, yet the molecular network structure that underpins the performance of these industrially essential materials is not well understood. Internal nodular morphologies have repeatedly been reported for epoxy resins analyzed using SEM or AFM, yet the origin of these features remains a contentious subject, and epoxies are still commonly assumed to be chemically homogeneous. Uniquely, in this contribution we use the recently developed AFM-IR technique to eliminate previous differences in interpretation, and establish that nodule features correspond to heterogeneous network connectivity within an epoxy phenolic formulation. PMID:26694687

  15. Molecular modeling of enzyme attachment on AFM probes.

    PubMed

    Oliveira, Guedmiller S; Leite, Fabio L; Amarante, Adriano M; Franca, Eduardo F; Cunha, Richard A; Briggs, James M; Freitas, Luiz C G

    2013-09-01

    The immobilization of enzymes on atomic force microscope tip (AFM tip) surface is a crucial step in the development of nanobiosensors to be used in detection process. In this work, an atomistic modeling of the attachment of the acetyl coenzyme A carboxylase (ACC enzyme) on a functionalized AFM tip surface is proposed. Using electrostatic considerations, suitable enzyme-surface orientations with the active sites of the ACC enzyme available for interactions with bulk molecules were found. A 50 ns molecular dynamics trajectory in aqueous solution was obtained and surface contact area, hydrogen bonding and protein stability were analyzed. The enzyme-surface model proposed here with minor adjustment can be applied to study antigen-antibody interactions as well as enzyme immobilization on silica for chromatography applications. PMID:24029365

  16. AFM study of polymer lubricants on hard disk surfaces

    NASA Astrophysics Data System (ADS)

    Bao, G. W.; Troemel, M.; Li, S. F. Y.

    Thin liquid films of PFPE (perfluoropolyether) lubricants dip-coated on hard disk surfaces were imaged with non-contact mode AFM. Demnum lubricants with phosphazene additives exhibited strong interactions with a silicon tip due to the formation of liquid bridges between the lubricants and the tip, as indicated by a remarkable hysteresis loop between approach and retraction curves in force vs. distance measurements. Features resulting from capillary forces due to tip tapping to the lubricants were revealed, which demonstrated that the capillary forces could be used to lock the non-contacting tip at a certain separation from the substrate surface to obtain AFM images. Force vs. distance curves for Fomblin Z-dol lubricants showed negligible hysteresis effects and features corresponding to lateral distortion of the tip by the lubricants only were observed. In both cases, only when the tip was positioned far above the surfaces could the natural distributions of the lubricants be imaged.

  17. BOREAS AFM-5 Level-1 Upper Air Network Data

    NASA Technical Reports Server (NTRS)

    Barr, Alan; Hrynkiw, Charmaine; Newcomer, Jeffrey A. (Editor); Hall, Forrest G. (Editor); Smith, David E. (Technical Monitor)

    2000-01-01

    The Boreal Ecosystem-Atmosphere Study (BOREAS) Airborne Fluxes and Meteorology (AFM)-5 team collected and processed data from the numerous radiosonde flights during the project. The goals of the AFM-05 team were to provide large-scale definition of the atmosphere by supplementing the existing Atmospheric Environment Service (AES) aerological network, both temporally and spatially. This data set includes basic upper-air parameters collected from the network of upper-air stations during the 1993, 1994, and 1996 field campaigns over the entire study region. The data are contained in tabular ASCII files. The level-1 upper-air network data are available from the Earth Observing System Data and Information System (EOSDIS) Oak Ridge National Laboratory (ORNL) Distributed Active Archive Center (DAAC). The data files also are available on a CD-ROM (see document number 20010000884).

  18. Adhesion forces in AFM of redox responsive polymer grafts: Effects of tip hydrophilicity

    NASA Astrophysics Data System (ADS)

    Feng, Xueling; Kieviet, Bernard D.; Song, Jing; Schön, Peter M.; Vancso, G. Julius

    2014-02-01

    The adherence between silicon nitride AFM tips and redox-active poly(ferrocenylsilanes) (PFS) grafts on gold was investigated by electrochemical AFM force spectroscopy. Before the adhesion measurements silicon nitride AFM probes were cleaned with organic solvents (acetone and ethanol) or piranha solution. Interestingly, these different AFM tip cleaning procedures drastically affected the observed adhesion forces. Water contact angle measurements on the corresponding AFM probe chips showed that piranha treatment resulted in a significant increase of AFM probe chip surface hydrophilicity compared to the organic solvent treatment. Obviously this hydrophilicity change caused drastic, even opposite changes in the tip-PFS adhesive force measurement upon electrode potential change to reversibly oxidize and reduce the PFS grafts. Our findings are of pivotal importance for AFM tip adhesion measurements utilizing standard silicon nitride AFM tips. Probe hydrophilicity must be carefully taken into consideration and controlled.

  19. Effect of tip radius on the incipient plasticity of chromium studied by nanoindentation

    SciTech Connect

    Wu, Dong; Morris, James R; Nieh, T. G.

    2015-01-01

    The onset of plasticity in Cr was investigated by nanoindentation using indenters with tip radii ranging from 60 to 759 nm. The stress for incipient plasticity was found to increase with decreasing tip radius. The cumulative pop-in probability on load could be described successfully by a combined model over the full range of tip radius, indicating that the incipient plasticity might be triggered either by the homogeneous nucleation of dislocation or by the activation of existing dislocations underneath the indenter.

  20. Defect formation by pristine indenter at the initial stage of nanoindentation

    SciTech Connect

    Chen, I-Hsien; Hsiao, Chun-I; Behera, Rakesh K.; Hsu, Wen-Dung

    2013-12-07

    Nano-indentation is a sophisticated method to characterize mechanical properties of materials. This method samples a very small amount of material during each indentation. Therefore, this method is extremely useful to measure mechanical properties of nano-materials. The measurements using nanoindentation is very sensitive to the surface topology of the indenter and the indenting surfaces. The mechanisms involved in the entire process of nanoindentation require an atomic level understanding of the interplay between the indenter and the substrate. In this paper, we have used atomistic simulation methods with empirical potentials to investigate the effect of various types of pristine indenter on the defect nucleation and growth. Using molecular dynamics simulations, we have predicted the load-depth curve for conical, vickers, and sperical tip. The results are analyzed based on the coherency between the indenter tip and substrate surface for a fixed depth of 20 Å. The depth of defect nucleation and growth is observed to be dependent on the tip geometry. A tip with larger apex angle nucleates defects at a shallower depth. However, the type of defect generated is dependent on the crystalline orientation of the tip and substrate. For coherent systems, prismatic loops were generated, which released into the substrate along the close-packed directions with continued indentation. For incoherent systems, pyramidal shaped dislocation junctions formed in the FCC systems and disordered atomic clusters formed in the BCC systems. These defect nucleation and growth process provide the atomistic mechanisms responsible for the observed load-depth response during nanoindentation.

  1. Nanoindentation Studies Of Hard Nanocomposite Ti-B-N Thin Films

    SciTech Connect

    Rupa, P. Karuna Purnapu; Chakraborty, P. C.; Mishra, Suman Kumari

    2011-12-12

    Titanium boron nitride (Ti-B-N) films were deposited by reactive magnetron sputtering using single Titanium diboride (TiB{sub 2}) target in different Ar-N{sub 2} gas mixtures. The influence of N{sub 2}:Ar ratio on the microstructure and mechanical properties of the deposited films have been investigated. Atomic force microscopy analysis indicated the grain size decreases with incorporation of nitrogen in the films. Nanoindentation studies have shown the hardness decreases with nitrogen incorporation.

  2. Precision of nanoindentation protocols for measurement of viscoelasticity in cortical and trabecular bone.

    PubMed

    Isaksson, Hanna; Nagao, Shijo; Małkiewicz, Marta; Julkunen, Petro; Nowak, Roman; Jurvelin, Jukka S

    2010-08-26

    Nanoindentation has recently gained attention as a characterization technique for mechanical properties of biological tissues, such as bone, on the sub-micron level. However, optimal methods to characterize viscoelastic properties of bones are yet to be established. This study aimed to compare the time-dependent viscoelastic properties of bone tissue obtained with different nanoindentation methods. Bovine cortical and trabecular bone samples (n=8) from the distal femur and proximal tibia were dehydrated, embedded and polished. The material properties determined using nanoindentation were hardness and reduced modulus, as well as time-dependent parameters based on creep, loading-rate, dissipated energy and semi-dynamic testing under load control. Each loading protocol was repeated 160 times and the reproducibility was assessed based on the coefficient of variation (CV). Additionally, three well-characterized polymers were tested and CV values were calculated for reference. The employed methods were able to characterize time-dependent viscoelastic properties of bone. However, their reproducibility varied highly (CV 9-40%). The creep constant increased with increasing dwell time. The reproducibility was best with a 30s creep period (CV 18%). The dissipated energy was stable after three repeated load cycles, and the reproducibility improved with each cycle (CV 23%). The viscoelastic properties determined with semi-dynamic test increased with increase in frequency. These measurements were most reproducible at high frequencies (CV 9-10%). Our results indicate that several methods are feasible for the determination of viscoelastic properties of bone material. The high frequency semi-dynamic test showed the highest precision within the tested nanoindentation protocols. PMID:20478559

  3. Microscopic reflection difference spectroscopy for strain field of GaN induced by Berkovich nanoindentation

    NASA Astrophysics Data System (ADS)

    Gao, H. S.; Liu, Y.; Zhang, H. Y.; Wu, S. J.; Jiang, C. Y.; Yu, J. L.; Zhu, L. P.; Li, Y.; Huang, W.; Chen, Y. H.

    2014-02-01

    We have measured strain field of Berkovich nanoindentation by Raman mapping technique and microscopic reflection difference spectroscopy (μ-RDS). The validity of the μ-RDS method is verified by the accordance between the theoretical simulated result and the rotated measurement result. Comparing the two different methods, it is concluded that μ-RDS is sensitive and effective to measure anisotropic strain zone in the plane.

  4. Characterization of the elastic and viscoelastic properties of dentin by a nanoindentation creep test.

    PubMed

    Chuang, Shu-Fen; Lin, Shih-Yun; Wei, Pal-Jen; Han, Chang-Fu; Lin, Jen-Fin; Chang, Hsien-Chang

    2015-07-16

    Dentin is the main supporting structure of teeth, but its mechanical properties may be adversely affected by pathological demineralization. The purposes of this study were to develop a quantitative approach to characterize the viscoelastic properties of dentin after de- and re-mineralization, and to examine the elastic properties using a nanoindentation creep test. Dentin specimens were prepared to receive both micro- and nano-indentation tests at wet and dry states. These tests were repeatedly performed after demineralization (1% citric acid for 3 days) and remineralization (artificial saliva immersion for 28 days). The nanoindentation test was executed in a creep mode, and the resulting displacement-time responses were disintegrated into primary (transient) and secondary (viscous) creep. The structural changes and mineral densities of dentin were also examined under SEM and microCT, respectively. The results showed that demineralization removed superficial minerals of dentin to the depth of 400 μm, and affected its micro- and nano-hardness, especially in the hydrate state. Remineralization only repaired the minerals at the surface layer, and partially recovered the nanohardness. Both the primary the secondary creep increased in the demineralized dentin, while the hydration further enhanced creep deformation of untreated and remineralized dentin. Remineralization reduced the primary creep of dentin, but did not effectively increase the viscosity. In conclusion, water plasticization increases the transient and viscous creep strains of demineralized dentin and reduces load sustainability. The nanoindentation creep test is capable of analyzing the elastic and viscoelastic properties of dentin, and reveals crucial information about creep responses. PMID:25911251

  5. Nanoindentation of silicon nitride: A multimillion-atom molecular dynamics study

    NASA Astrophysics Data System (ADS)

    Walsh, Phillip; Omeltchenko, Andrey; Kalia, Rajiv K.; Nakano, Aiichiro; Vashishta, Priya; Saini, Subhash

    2003-01-01

    Nanoindentation of crystalline and amorphous silicon nitride films is studied using 10-million-atom molecular dynamics simulations. A rigid pyramid-shaped indenter tip is used. Load-displacement curves are computed and are used to derive hardness and elastic moduli of the simulated crystalline and amorphous films. Computer images of local pressure distributions and configuration snapshots show that plastic deformation in the film extends to regions far from the actual indent.

  6. Nanoindentation creep study on an ion beam irradiated oxide dispersion strengthened alloy

    NASA Astrophysics Data System (ADS)

    Huang, Zijing; Harris, Adrian; Maloy, Stuart A.; Hosemann, Peter

    2014-08-01

    Oxide dispersion strengthened (ODS) alloys are considered advanced structural materials for nuclear application due to their radiation tolerance and creep resistance. Ion beam irradiation is used to study the property changes due to displacement damage. In this work 1 dpa displacement damage in an ODS was produced followed by a nanoindentation creep study at temperatures up to 600 °C to evaluate the changes in mechanical properties due to irradiation. Converted yield strength (YS) and creep related parameters are reported.

  7. AFM and SThM Characterization of Graphene

    NASA Astrophysics Data System (ADS)

    Foy, Christopher; Sidorov, Anton; Chen, Xunchi; Ruan, Ming; Berger, Claire; de Heer, Walter; Jiang, Zhigang

    2012-03-01

    We report on detailed characterization of epitaxial grown graphene on SiC and chemical vapor deposition grown graphene on Cu foil using atomic force microscopy (AFM) and scanning thermal microscopy (SThM). We focus on the electronic and thermal properties of graphene grain boundaries, and thus providing valuable feedback to materials growth. Specifically, we perform thermal conductivity contrast mapping and surface potential mapping of graphene, and compare with that obtained on the Au electrodes and the substrate.

  8. Investigation of biopolymer networks by means of AFM

    NASA Astrophysics Data System (ADS)

    Keresztes, Z.; Rigó, T.; Telegdi, J.; Kálmán, E.

    Natural hydrogel alginate was investigated by means of atomic force microscopy (AFM) to gain microscale information on the morphological and rheological properties of the biopolymer network cross-linked by various cations. Local rheological properties of the gels measured by force spectroscopy gave correlation between increasing ion selectivity and increasing polymer elasticity. Adhesive forces acting between the surface of the gel and the probe, and also the intrinsic rheological properties of bulk polymers affect the microscopical image formation.

  9. Multimillion atom simulations of dynamics of oxidation of an aluminum nanoparticle and nanoindentation on ceramics.

    PubMed

    Vashishta, Priya; Kalia, Rajiv K; Nakano, Aiichiro

    2006-03-01

    We have developed a first-principles-based hierarchical simulation framework, which seamlessly integrates (1) a quantum mechanical description based on the density functional theory (DFT), (2) multilevel molecular dynamics (MD) simulations based on a reactive force field (ReaxFF) that describes chemical reactions and polarization, a nonreactive force field that employs dynamic atomic charges, and an effective force field (EFF), and (3) an atomistically informed continuum model to reach macroscopic length scales. For scalable hierarchical simulations, we have developed parallel linear-scaling algorithms for (1) DFT calculation based on a divide-and-conquer algorithm on adaptive multigrids, (2) chemically reactive MD based on a fast ReaxFF (F-ReaxFF) algorithm, and (3) EFF-MD based on a space-time multiresolution MD (MRMD) algorithm. On 1920 Intel Itanium2 processors, we have demonstrated 1.4 million atom (0.12 trillion grid points) DFT, 0.56 billion atom F-ReaxFF, and 18.9 billion atom MRMD calculations, with parallel efficiency as high as 0.953. Through the use of these algorithms, multimillion atom MD simulations have been performed to study the oxidation of an aluminum nanoparticle. Structural and dynamic correlations in the oxide region are calculated as well as the evolution of charges, surface oxide thickness, diffusivities of atoms, and local stresses. In the microcanonical ensemble, the oxidizing reaction becomes explosive in both molecular and atomic oxygen environments, due to the enormous energy release associated with Al-O bonding. In the canonical ensemble, an amorphous oxide layer of a thickness of approximately 40 angstroms is formed after 466 ps, in good agreement with experiments. Simulations have been performed to study nanoindentation on crystalline, amorphous, and nanocrystalline silicon nitride and silicon carbide. Simulation on nanocrystalline silicon carbide reveals unusual deformation mechanisms in brittle nanophase materials, due to

  10. Durability of crystalline phase in concrete microstructure modified by the mineral powders: evaluation by nanoindentation tests

    NASA Astrophysics Data System (ADS)

    Rajczakowska, Magdalena; Łydżba, Dariusz

    2016-03-01

    This paper presents the nanoindentation investigation of the evolution of concrete microstructure modified by the Internal Crystallization Technology mineral powders. The samples under study were retrieved from a fragment of a circular concrete lining of the vertical mine shaft at a depth of approximately 1,000 m. Due to the aggressive environment and exposure to contaminated water, the internal surface of the structure was deteriorated, decreasing its strength significantly. The mineral powders were applied directly on the surface lining. The specimens were investigated one month, three months and one year after the application of the aforementioned substance in order to verify the time dependence of the strengthening processes and durability of the crystalline phase. The microstructural changes of concrete were assessed with the use of nanoindentation technique. The testing procedure involved including the previously cut specimens in the epoxy resin and grinding and polishing in order to reduce the surface roughness. As a result of the nanoindentation tests the hardness as well as Young's modulus of the material were evaluated. The results were then compared and statistically analyzed. As a consequence, the disintegration time of the crystalline network in the pores of concrete was identified.

  11. Microstructure Characterization by Means of X-ray Micro-CT and Nanoindentation Measurements

    NASA Astrophysics Data System (ADS)

    Rajczakowska, Magdalena; Stefaniuk, Damian; Łydżba, Dariusz

    2015-03-01

    The aim of this paper is to present an example of the material microstructure characterization with the use of X-ray micro-CT and nanoindentation measurements. Firstly, the current scope of application of the aforementioned techniques is provided within different fields of science. Then, background of each of the methods is presented. The methodology of X-ray micro-CT is described with the emphasis on the Beer's law formulation. In addition, the basics of the nanoindentation technique are outlined and major formulas for the hardness and Young's modulus calculation are given. Finally, example results for a concrete sample are presented. The microstructure of the selected material is firstly characterized in terms of geometry using the results from the microtomograhy measurements, e.g., porosity and attenuation profiles, pore and aggregate size distribution, shape factor of pores, etc. Next, the results of the nanoindentation tests are provided, namely the hardness and Young's modulus versus the height of the sample. The influence of the number of tests and statistical analysis on the final results is underlined.

  12. Evaluation of the degradation of plasma sprayed thermal barrier coatings using nano-indentation.

    PubMed

    Kim, Dae-Jin; Cho, Sung-Keun; Choi, Jung-Hun; Koo, Jae-Mean; Seok, Chang-Sung; Kim, Moon-Young

    2009-12-01

    In this study, the disk type of a thermal barrier coating (TBC) system for a gas turbine blade was isothermally aged at 1100 degrees C for various times up to 400 hours. For each aging condition, the thickness of the thermally grown oxide (TGO) was measured by optical microscope and mechanical properties such as the elastic modulus and hardness were measured by micro-indentation and nano-indentation on the cross-section of a coating specimen. In the case of micro-indentation, the mechanical properties of a Ni-base superalloy substrate and MCrAlY bond coat material did not significantly change with an increase in exposure time. In the case of nano-indentation, the gamma-Ni phase and beta-NiAl phase in the bond coat and top coat material show no significant change in their properties. However, the elastic modulus and the hardness of TGO show a remarkable decrease from 100 h to 200 h then remain nearly constant after 200 h due to the internal delamination of TBC. It has been confirmed that the nano-indentation technique is a very effective way to evaluate the degradation of a thermal barrier coating system. PMID:19908771

  13. Effects of Crystalline Anisotropy and Indenter Size on Nanoindentation by Multiscale Simulation

    PubMed Central

    2010-01-01

    Nanoindentation processes in single crystal Ag thin film under different crystallographic orientations and various indenter widths are simulated by the quasicontinuum method. The nanoindentation deformation processes under influences of crystalline anisotropy and indenter size are investigated about hardness, load distribution, critical load for first dislocation emission and strain energy under the indenter. The simulation results are compared with previous experimental results and Rice-Thomson (R-T) dislocation model solution. It is shown that entirely different dislocation activities are presented under the effect of crystalline anisotropy during nanoindentation. The sharp load drops in the load–displacement curves are caused by the different dislocation activities. Both crystalline anisotropy and indenter size are found to have distinct effect on hardness, contact stress distribution, critical load for first dislocation emission and strain energy under the indenter. The above quantities are decreased at the indenter into Ag thin film along the crystal orientation with more favorable slip directions that easy trigger slip systems; whereas those will increase at the indenter into Ag thin film along the crystal orientation with less or without favorable slip directions that hard trigger slip systems. The results are shown to be in good agreement with experimental results and R-T dislocation model solution. PMID:20672077

  14. Depth Dependence of the Mechanical Properties of Human Enamel by Nanoindentation

    SciTech Connect

    Zhou, J; Hsiung, L L

    2006-02-17

    Nanoindentation has recently emerged to be the primary method to study the mechanical behavior and reliability of human enamel. Its hardness and elastic modulus were generally reported as average values with standard deviations that were calculated from the results of multiple nanoindentation tests. In such an approach, it is assumed that the mechanical properties of human enamel are constant, independent of testing parameters, like indent depth and loading rate. However, little is known if they affect the measurements. In this study, we investigated the dependence of the hardness and elastic modulus of human enamel on the indent depth. We found that in a depth range from 100 nm to 2000 nm the elastic moduli continuously decreased from {approx} 104 GPa to {approx} 70 GPa, and the hardnesses decreased from {approx} 5.7 GPa to {approx} 3.6 GPa. We then considered human enamel as a fiber-reinforced composite, and used the celebrated rule of mixture theory to quantify the upper and lower bounds of the elastic moduli, which were shown to cover the values measured in the current study and previous studies. Accordingly, we attributed the depth dependence of the hardness and modulus to the continuous microstructure evolution induced by nanoindenter.

  15. Spherical nanoindentation study of the deformation micromechanisms of LiTaO{sub 3} single crystals

    SciTech Connect

    Anasori, B.; Barsoum, M. W.; Sickafus, K. E.; Usov, I. O.

    2011-07-15

    Herein, spherical nanoindentation (NI) was used to investigate the room temperature deformation behavior of C-plane LiTaO{sub 3} single crystals loaded along the [0001] direction as a function of ion irradiation. When the NI load-displacement curves of 3 different nanoindenter radii (1.4 {mu}m, 5 {mu}m, and 21 {mu}m) were converted to NI stress-strain curves, good agreement between them was found. The surface first deforms elastically - with a Young's modulus of 205 {+-} 5 GPa, calculated from the stiffness versus contact radii curves and 207 {+-} 3 GPa measured using a Berkovich tip - and then plastically deforms at {approx_equal} 6 GPa. Repeated loading into the same location results in large, reproducible, fully reversible, nested hysteresis loops attributed to the formation of incipient kink bands (IKBs). The latter are coaxial fully reversible dislocation loops that spontaneously shrink when the load is removed. The IKBs most probably nucleate within the (1012) twins that form near the surface. The sharper radii resulted in twin nucleation at lower stresses. The changes in the reversible loops' shape and areas can be related to the width of the twins that form. The latter were proportional to the nanoindenter tip radii and confirmed by scanning electron microscopy and by the fact that larger threshold stresses were needed for IKB nucleation with the smaller tip sizes. No effect of irradiation was observed on the NI response, presumably because of the mildness of the irradiation damage.

  16. Nanoindentation hardness of soft films on hard substrates: Effects of the substrate

    SciTech Connect

    Tsui, T.Y.; Ross, C.A.; Pharr, G.M.

    1997-06-01

    The ability to accurately measure the mechanical properties of thin metallic films is important in the semiconductor industry as it relates to device reliability issues. One popular technique for measuring thin film mechanical properties is nanoindentation. This technique has the advantage of being able to measure properties such as hardness and elastic modulus without removing a film from its substrate. However, according to a widely-held rule of thumb, intrinsic film properties can be measured in a manner which is not influenced by the substrate only if the indentation depth is kept to less than 10% of the film thickness, which is often not practical. In this work, a method for making substrate independent hardness measurements of soft metallic films on hard substrates is proposed. The primary issue to be addressed is the substrate-induced enhancement of indentation pile-up and the ways in which this pile-up influences the contact area determined from analyses of nanoindentation load- displacement data. Based on experimental observations of soft aluminum films on silicon, glass, and sapphire substrates, a simple empirical relationship is derived which relates the amount of pile-up to the contact depth. From this relationship, a simple method is developed which allows the intrinsic hardness of the film to be measured by nanoindentation methods even when the indenter penetrates through the film into the substrate.

  17. Near-Field Spectroscopy with Nanoparticles Deposited by AFM

    NASA Technical Reports Server (NTRS)

    Anderson, Mark S.

    2008-01-01

    An alternative approach to apertureless near-field optical spectroscopy involving an atomic-force microscope (AFM) entails less complexity of equipment than does a prior approach. The alternative approach has been demonstrated to be applicable to apertureless near-field optical spectroscopy of the type using an AFM and surface enhanced Raman scattering (SERS), and is expected to be equally applicable in cases in which infrared or fluorescence spectroscopy is used. Apertureless near-field optical spectroscopy is a means of performing spatially resolved analyses of chemical compositions of surface regions of nanostructured materials. In apertureless near-field spectroscopy, it is common practice to utilize nanostructured probe tips or nanoparticles (usually of gold) having shapes and dimensions chosen to exploit plasmon resonances so as to increase spectroscopic-signal strengths. To implement the particular prior approach to which the present approach is an alternative, it is necessary to integrate a Raman spectrometer with an AFM and to utilize a special SERS-active probe tip. The resulting instrumentation system is complex, and the tasks of designing and constructing the system and using the system to acquire spectro-chemical information from nanometer-scale regions on a surface are correspondingly demanding.

  18. Tissue section AFM: In situ ultrastructural imaging of native biomolecules

    PubMed Central

    Graham, Helen K.; Hodson, Nigel W.; Hoyland, Judith A.; Millward-Sadler, Sarah J.; Garrod, David; Scothern, Anthea; Griffiths, Christopher E.M.; Watson, Rachel E.B.; Cox, Thomas R.; Erler, Janine T.; Trafford, Andrew W.; Sherratt, Michael J.

    2010-01-01

    Conventional approaches for ultrastructural high-resolution imaging of biological specimens induce profound changes in bio-molecular structures. By combining tissue cryo-sectioning with non-destructive atomic force microscopy (AFM) imaging we have developed a methodology that may be applied by the non-specialist to both preserve and visualize bio-molecular structures (in particular extracellular matrix assemblies) in situ. This tissue section AFM technique is capable of: i) resolving nm–µm scale features of intra- and extracellular structures in tissue cryo-sections; ii) imaging the same tissue region before and after experimental interventions; iii) combining ultrastructural imaging with complimentary microscopical and micromechanical methods. Here, we employ this technique to: i) visualize the macro-molecular structures of unstained and unfixed fibrillar collagens (in skin, cartilage and intervertebral disc), elastic fibres (in aorta and lung), desmosomes (in nasal epithelium) and mitochondria (in heart); ii) quantify the ultrastructural effects of sequential collagenase digestion on a single elastic fibre; iii) correlate optical (auto fluorescent) with ultrastructural (AFM) images of aortic elastic lamellae. PMID:20144712

  19. Nanoscale rippling on polymer surfaces induced by AFM manipulation

    PubMed Central

    2015-01-01

    Summary Nanoscale rippling induced by an atomic force microscope (AFM) tip can be observed after performing one or many scans over the same area on a range of materials, namely ionic salts, metals, and semiconductors. However, it is for the case of polymer films that this phenomenon has been widely explored and studied. Due to the possibility of varying and controlling various parameters, this phenomenon has recently gained a great interest for some technological applications. The advent of AFM cantilevers with integrated heaters has promoted further advances in the field. An alternative method to heating up the tip is based on solvent-assisted viscoplastic deformations, where the ripples develop upon the application of a relatively low force to a solvent-rich film. An ensemble of AFM-based procedures can thus produce nanoripples on polymeric surfaces quickly, efficiently, and with an unprecedented order and control. However, even if nanorippling has been observed in various distinct modes and many theoretical models have been since proposed, a full understanding of this phenomenon is still far from being achieved. This review aims at summarizing the current state of the art in the perspective of achieving control over the rippling process on polymers at a nanoscale level. PMID:26733086

  20. AFM imaging of functionalized carbon nanotubes on biological membranes

    NASA Astrophysics Data System (ADS)

    Lamprecht, C.; Liashkovich, I.; Neves, V.; Danzberger, J.; Heister, E.; Rangl, M.; Coley, H. M.; McFadden, J.; Flahaut, E.; Gruber, H. J.; Hinterdorfer, P.; Kienberger, F.; Ebner, A.

    2009-10-01

    Multifunctional carbon nanotubes are promising for biomedical applications as their nano-size, together with their physical stability, gives access into the cell and various cellular compartments including the nucleus. However, the direct and label-free detection of carbon nanotube uptake into cells is a challenging task. The atomic force microscope (AFM) is capable of resolving details of cellular surfaces at the nanometer scale and thus allows following of the docking of carbon nanotubes to biological membranes. Here we present topographical AFM images of non-covalently functionalized single walled (SWNT) and double walled carbon nanotubes (DWNT) immobilized on different biological membranes, such as plasma membranes and nuclear envelopes, as well as on a monolayer of avidin molecules. We were able to visualize DWNT on the nuclear membrane while at the same time resolving individual nuclear pore complexes. Furthermore, we succeeded in localizing individual SWNT at the border of incubated cells and in identifying bundles of DWNT on cell surfaces by AFM imaging.

  1. Oxide nanocrystal based nanocomposites for fabricating photoplastic AFM probes.

    PubMed

    Ingrosso, Chiara; Martin-Olmos, Cristina; Llobera, Andreu; Innocenti, Claudia; Sangregorio, Claudio; Striccoli, Marinella; Agostiano, Angela; Voigt, Anja; Gruetzner, Gabi; Brugger, Jürgen; Perez-Murano, Francesc; Curri, Maria Lucia

    2011-11-01

    We report on the synthesis, characterization and application of a novel nanocomposite made of a negative tone epoxy based photoresist modified with organic-capped Fe(2)O(3) nanocrystals (NCs). The mechanical properties of the nanocomposite drastically improve upon incorporation of a suitable concentration of NCs in the polymer, without deteriorating its photolithography performance. High aspect ratio 3D microstructures made of the nanocomposite have been fabricated with a uniform surface morphology and with a resolution down to few micrometres. The embedded organic-capped Fe(2)O(3) NCs drastically increase the stiffness and hardness of the epoxy based photoresist matrix, making the final material extremely interesting for manufacturing miniaturized polymer based mechanical devices and systems. In particular, the nanocomposite has been used as structural material for fabricating photoplastic Atomic Force Microscopy (AFM) probes with integrated tips showing outstanding mechanical response and high resolution imaging performance. The fabricated probes consist of straight cantilevers with low stress-gradient and high quality factors, incorporating sharp polymeric tips. They present considerably improved performance compared to pure epoxy based photoresist AFM probes, and to commercial silicon AFM probes. PMID:21858377

  2. Lateral tip control effects in CD-AFM metrology: the large tip limit

    NASA Astrophysics Data System (ADS)

    Dixson, Ronald; Goldband, Ryan S.; Orji, Ndubuisi G.

    2015-10-01

    Critical dimension atomic force microscopes (CD-AFMs) use flared tips and two-dimensional sensing and control of the tip-sample interaction to enable scanning of features with near-vertical or even reentrant sidewalls. Sidewall sensing in CD-AFM usually involves lateral dither of the tip, which was the case in the first two generations of instruments. Current, third generation instruments also utilize a control algorithm and fast response piezo actuator to position the tip in a manner that resembles touch-triggering of coordinate measuring machine (CMM) probes. All methods of tip position control, however, induce an effective tip width that may deviate from the actual geometrical tip width. The National Institute of Standards and Technology (NIST) has been investigating the dependence of effective tip width on the dither settings and lateral stiffness of the tip, as well as the possibility of material effects due to sample composition. We have concluded that these effects will not generally result in a residual bias, provided that the tip calibration and sample measurement are performed under the same conditions. To further validate our prior conclusions about the dependence of effective tip width on lateral stiffness, we recently performed experiments using a very large non-CD tip with an etched plateau of approximately 2 μm width. The effective lateral stiffness of these tips is at least 20 times greater than typical CD-AFM tips, and these results supported our prior conclusions about the expected behavior for larger tips. The bottom-line importance of these latest observations is that we can now reasonably conclude that a dither slope of 3 nm/V is the baseline response due to the induced motion of the cantilever base.

  3. An advanced AFM sensor: its profile accuracy and low probe wear property for high aspect ratio patterns

    NASA Astrophysics Data System (ADS)

    Watanabe, Masahiro; Baba, Shuichi; Nakata, Toshihiko; Kurenuma, Toru; Kunitomo, Yuichi; Edamura, Manabu

    2007-03-01

    Design rule shrinkage and wider adoption of new device structures such as STI, copper damascene interconnects, and deep trench structures have made the need for in-line process monitoring of step heights and profiles of device structures more urgent. To monitor active device patterns, as opposed to test patterns as in OCD, AFM is the only non-destructive 3D monitoring tool. The barriers to using AFM in-line monitoring are its slow throughput and the accuracy degradation associated with probe tip wear and spike noise caused by unwanted oscillation on the steep slopes of high-aspect-ratio patterns. Our proprietary AFM scanning method, StepIn TM mode, is the method best suited to measuring high-aspect-ratio pattern profiles. Because the probe is not dragged on the sample surface as in conventional AFM, the profile trace fidelity across steep slopes is excellent. Because the probe does not oscillate and hit the sample at a high frequency, as in AC scanning mode, this mode is free from unwanted spurious noises on steep sample slopes and incurs extremely little probe tip wear. To take full advantage of the above properties, we have developed an AFM sensor that is optimized for in-line use and produces accurate profile data at high speeds and incurs little probe tip wear. The control scheme we have developed for the AFM sensor, which we call "Advanced StepIn TM", elaborately analyses the contact force signal, enabling efficient probe tip scanning and a low and stable contact force. With a developed AFM sensor that realizes this concept, we conducted an intensive evaluation on the effect of low and stable contact force scan. Probes with HDC (high density carbon) tips were used for the evaluation. The experiment proves that low contact force enhances the measured profile fidelity by preventing probe tip slip on steep slopes. Dynamics simulation of these phenomena was also conducted, and its results agreed well with the experimental results. The low contact force scan also

  4. Nanoindentation studies of full and empty viral capsids and the effects of capsid protein mutations on elasticity and strength

    NASA Astrophysics Data System (ADS)

    Michel, J. P.; Ivanovska, I. L.; Gibbons, M. M.; Klug, W. S.; Knobler, C. M.; Wuite, G. J. L.; Schmidt, C. F.

    2006-04-01

    The elastic properties of capsids of the cowpea chlorotic mottle virus have been examined at pH 4.8 by nanoindentation measurements with an atomic force microscope. Studies have been carried out on WT capsids, both empty and containing the RNA genome, and on full capsids of a salt-stable mutant and empty capsids of the subE mutant. Full capsids resisted indentation more than empty capsids, but all of the capsids were highly elastic. There was an initial reversible linear regime that persisted up to indentations varying between 20% and 30% of the diameter and applied forces of 0.6-1.0 nN; it was followed by a steep drop in force that is associated with irreversible deformation. A single point mutation in the capsid protein increased the capsid stiffness. The experiments are compared with calculations by finite element analysis of the deformation of a homogeneous elastic thick shell. These calculations capture the features of the reversible indentation region and allow Young's moduli and relative strengths to be estimated for the empty capsids. atomic force microscopy | cowpea chlorotic mottle virus | finite element analysis | biomechanics

  5. Lateral Tip Control Effects in CD-AFM Metrology: The Large Tip Limit

    PubMed Central

    Dixson, Ronald G.; Orji, Ndubuisi G.; Goldband, Ryan S.

    2016-01-01

    Sidewall sensing in critical dimension atomic force microscopes (CD-AFMs) usually involves continuous lateral dithering of the tip or the use of a control algorithm and fast response piezo actuator to position the tip in a manner that resembles touch-triggering of coordinate measuring machine (CMM) probes. All methods of tip position control, however, induce an effective tip width that may deviate from the actual geometrical tip width. Understanding the influence and dependence of the effective tip width on the dither settings and lateral stiffness of the tip can improve the measurement accuracy and uncertainty estimation for CD-AFM measurements. Since CD-AFM typically uses tips that range from 15 nm to 850 nm in geometrical width, the behavior of effective tip width throughout this range should be understood. The National Institute of Standards and Technology (NIST) has been investigating the dependence of effective tip width on the dither settings and lateral stiffness of the tip, as well as the possibility of material effects due to sample composition. For tip widths of 130 nm and lower, which also have lower lateral stiffness, the response of the effective tip width to lateral dither is greater than for larger tips. However, we have concluded that these effects will not generally result in a residual bias, provided that the tip calibration and sample measurement are performed under the same conditions. To validate that our prior conclusions about the dependence of effective tip width on lateral stiffness are valid for large CD-tips, we recently performed experiments using a very large non-CD tip with an etched plateau of approximately 2 μm width. The effective lateral stiffness of these tips is at least 20 times greater than typical CD-AFM tips, and these results supported our prior conclusions about the expected behavior for larger tips. The bottom-line importance of these latest observations is that we can now reasonably conclude that a dither slope of 3 nm

  6. Quantifying molecule-surface interactions using AFM-based single-molecule manipulation

    NASA Astrophysics Data System (ADS)

    Tautz, F. S.; Wagner, C.; Temirov, R.; Fournier, N.; Green, M.; Esat, T.; Leinen, P.; Groetsch, A.; Ruiz, V. G.; Tkatchenko, A.; Li, C.; Muellen, K.; Rohlfing, M.

    2015-03-01

    Scanning probe microscopy plays an important role in the investigation of molecular adsorption. Promising, is the possibility to probe the molecule-surface interaction while tuning its strength through AFM tip-induced single-molecule manipulation. Here, we outline a strategy to achieve quantitative understanding of such manipulation experiments. The example of qPlus sensor based PTCDA molecule lifting experiments is used to demonstrate how different aspects of the molecule-surface interaction, namely the short-range adsorption potential, the asymptotic van der Waals potential, local chemical bonds which are the source of the surface corrugation, and molecule-molecule interactions can be measured with SPM and interpreted by the help of force-field simulations.

  7. Solvent-mediated repair and patterning of surfaces by AFM

    SciTech Connect

    Elhadj, S; Chernov, A; De Yoreo, J

    2007-10-30

    A tip-based approach to shaping surfaces of soluble materials with nanometer-scale control is reported. The proposed method can be used, for example, to eliminate defects and inhomogeneities in surface shape, repair mechanical or laser-induced damage to surfaces, or perform 3D lithography on the length scale of an AFM tip. The phenomenon that enables smoothing and repair of surfaces is based on the transport of material from regions of high- to low-curvature within the solution meniscus formed in a solvent-containing atmosphere between the surface in question and an AFM tip scanned over the surface. Using in situ AFM measurements of the kinetics of surface remodeling on KDP (KH{sub 2}PO{sub 4}) crystals in humid air, we show that redistribution of solute material during relaxation of grooves and mounds is driven by a reduction in surface free energy as described by the Gibbs-Thomson law. We find that the perturbation from a flat interface evolves according to the diffusion equation where the effective diffusivity is determined by the product of the surface stiffness and the step kinetic coefficient. We also show that, surprisingly, if the tip is instead scanned over or kept stationary above an atomically flat area of the surface, a convex structure is formed with a diameter that is controlled by the dimensions of the meniscus, indicating that the presence of the tip and meniscus reduces the substrate chemical potential beneath that of the free surface. This allows one to create nanometer-scale 3D structures of arbitrary shape without the removal of substrate material or the use of extrinsic masks or chemical compounds. Potential applications of these tip-based phenomena are discussed.

  8. Applications of AFM for atomic manipulation and spectroscopy

    NASA Astrophysics Data System (ADS)

    Custance, Oscar

    2009-03-01

    Since the first demonstration of atom-by-atom assembly [1], atomic manipulation with scanning tunneling microscopy has yielded stunning realizations in nanoscience. A new exciting panorama has been recently opened with the possibility of manipulating atoms at surfaces using atomic force microscopy (AFM) [2-5]. In this talk, we will present two different approaches that enable patterning structures at semiconductor surfaces by manipulating individual atoms with AFM and at room temperature [2, 3]. We will discuss the physics behind each protocol through the analysis of the measured forces associated with these manipulations [3-5]. Another challenging issue in scanning probe microscopy is the ability to disclose the local chemical composition of a multi-element system at atomic level. Here, we will introduce a single-atom chemical identification method, which is based on detecting the forces between the outermost atom of the AFM tip and the atoms at a surface [6]. We demonstrate this identification procedure on a particularly challenging system, where any discrimination attempt based solely on topographic measurements would be impossible to achieve. [4pt] References: [0pt] [1] D. M. Eigler and E. K. Schweizer, Nature 344, 524 (1990); [0pt] [2] Y. Sugimoto, M. Abe, S. Hirayama, N. Oyabu, O. Custance and S. Morita, Nature Materials 4, 156 (2005); [0pt] [3] Y. Sugimoto, P. Pou, O. Custance, P. Jelinek, M. Abe, R. Perez and S. Morita, Science 322, 413 (2008); [0pt] [4] Y. Sugimoto, P. Jelinek, P. Pou, M. Abe, S. Morita, R. Perez and O. Custance, Phys. Rev. Lett. 98, 106104 (2007); [0pt] [5] M. Ternes, C. P. Lutz, C. F. Hirjibehedin, F. J. Giessibl and A. J. Heinrich, Science 319, 1066 (2008); [0pt] [6] Y. Sugimoto, P. Pou, M. Abe, P. Jelinek, R. Perez, S. Morita, and O. Custance, Nature 446, 64 (2007)

  9. Adsorption Studies with AFM of Human Plasma Fibrinogen on Silicon Surfaces

    NASA Astrophysics Data System (ADS)

    Gause, Sheena; Kong, Wendy; Rowe

    2007-11-01

    Fibrinogen (FGN) plays an important role in the clotting of blood. Human plasma fibrinogen (HPF) is a protein that readily adsorbs on biomaterial surfaces. The purpose of this experiment was to use the Atomic Force Microscope to study the adsorption of HPF molecules or FGN onto several silicon surfaces with different orientations and resistivities. The size of the FGN molecules found to be somewhat different of Si(111), (100) and (110) were compared to the size of the FGN molecules in solution (45 nm in length, the end dynodes measures to be 6.5 nm in diameter, and the middle dynode measures to be 5 nm in diameter. For this study, the CPR (Thermo-microscope) Atomic Force Microscope (AFM) was used to observe the amount of fibrinogen molecules adsorbed by Si (111) with a resistance of .0281-.0261 φ cm, Si (111) with a resistance of 1 φ cm, Si (100), and Si (110) surfaces. In finding any single fibrinogen molecules, the appropriate image scans and measurements were taken. After collection and analysis of the data, it was found from AFM that the fibrinogen molecules found on Si (110) mostly resembled fibrinogen molecules found in solution. The other images showed that the fibrinogen molecules adsorbed on Silicon substrates is significantly greater (˜10-20 %) than those in solution.

  10. Direct measurement of optical force induced by near-field plasmonic cavity using dynamic mode AFM

    SciTech Connect

    Guan, Dongshi; Hang, Zhi Hong; Marset, Zsolt; Liu, Hui; Kravchenko, Ivan I.; Chan, Ho Bun; Chan, C. T.; Tong, Penger

    2015-11-20

    Plasmonic nanostructures have attracted much attention in recent years because of their potential applications in optical manipulation through near-field enhancement. Continuing experimental efforts have been made to develop accurate techniques to directly measure the near-field optical force induced by the plasmonic nanostructures in the visible frequency range. In this work, we report a new application of dynamic mode atomic force microscopy (DM-AFM) in the measurement of the enhanced optical force acting on a nano-structured plasmonic resonant cavity. The plasmonic cavity is made of an upper gold-coated glass sphere and a lower quartz substrate patterned with an array of subwavelength gold disks. In the near-field when the sphere is positioned close to the disk array, plasmonic resonance is excited in the cavity and the induced force by a 1550 nm infrared laser is found to be increased by an order of magnitude compared with the photon pressure generated by the same laser light. Lastly, the experiment demonstrates that DM-AFM is a powerful tool for the study of light induced forces and their enhancement in plasmonic nanostructures.

  11. Direct measurement of optical force induced by near-field plasmonic cavity using dynamic mode AFM

    DOE PAGESBeta

    Guan, Dongshi; Hang, Zhi Hong; Marset, Zsolt; Liu, Hui; Kravchenko, Ivan I.; Chan, Ho Bun; Chan, C. T.; Tong, Penger

    2015-11-20

    Plasmonic nanostructures have attracted much attention in recent years because of their potential applications in optical manipulation through near-field enhancement. Continuing experimental efforts have been made to develop accurate techniques to directly measure the near-field optical force induced by the plasmonic nanostructures in the visible frequency range. In this work, we report a new application of dynamic mode atomic force microscopy (DM-AFM) in the measurement of the enhanced optical force acting on a nano-structured plasmonic resonant cavity. The plasmonic cavity is made of an upper gold-coated glass sphere and a lower quartz substrate patterned with an array of subwavelength goldmore » disks. In the near-field when the sphere is positioned close to the disk array, plasmonic resonance is excited in the cavity and the induced force by a 1550 nm infrared laser is found to be increased by an order of magnitude compared with the photon pressure generated by the same laser light. Lastly, the experiment demonstrates that DM-AFM is a powerful tool for the study of light induced forces and their enhancement in plasmonic nanostructures.« less

  12. Direct Measurement of Optical Force Induced by Near-Field Plasmonic Cavity Using Dynamic Mode AFM.

    PubMed

    Guan, Dongshi; Hang, Zhi Hong; Marcet, Zsolt; Liu, Hui; Kravchenko, I I; Chan, C T; Chan, H B; Tong, Penger

    2015-01-01

    Plasmonic nanostructures have attracted much attention in recent years because of their potential applications in optical manipulation through near-field enhancement. Continuing experimental efforts have been made to develop accurate techniques to directly measure the near-field optical force induced by the plasmonic nanostructures in the visible frequency range. In this work, we report a new application of dynamic mode atomic force microscopy (DM-AFM) in the measurement of the enhanced optical force acting on a nano-structured plasmonic resonant cavity. The plasmonic cavity is made of an upper gold-coated glass sphere and a lower quartz substrate patterned with an array of subwavelength gold disks. In the near-field when the sphere is positioned close to the disk array, plasmonic resonance is excited in the cavity and the induced force by a 1550 nm infrared laser is found to be increased by an order of magnitude compared with the photon pressure generated by the same laser light. The experiment demonstrates that DM-AFM is a powerful tool for the study of light induced forces and their enhancement in plasmonic nanostructures. PMID:26586455

  13. Direct Measurement of Optical Force Induced by Near-Field Plasmonic Cavity Using Dynamic Mode AFM

    PubMed Central

    Guan, Dongshi; Hang, Zhi Hong; Marcet, Zsolt; Liu, Hui; Kravchenko, I. I.; Chan, C. T.; Chan, H. B.; Tong, Penger

    2015-01-01

    Plasmonic nanostructures have attracted much attention in recent years because of their potential applications in optical manipulation through near-field enhancement. Continuing experimental efforts have been made to develop accurate techniques to directly measure the near-field optical force induced by the plasmonic nanostructures in the visible frequency range. In this work, we report a new application of dynamic mode atomic force microscopy (DM-AFM) in the measurement of the enhanced optical force acting on a nano-structured plasmonic resonant cavity. The plasmonic cavity is made of an upper gold-coated glass sphere and a lower quartz substrate patterned with an array of subwavelength gold disks. In the near-field when the sphere is positioned close to the disk array, plasmonic resonance is excited in the cavity and the induced force by a 1550 nm infrared laser is found to be increased by an order of magnitude compared with the photon pressure generated by the same laser light. The experiment demonstrates that DM-AFM is a powerful tool for the study of light induced forces and their enhancement in plasmonic nanostructures. PMID:26586455

  14. Direct Measurement of Optical Force Induced by Near-Field Plasmonic Cavity Using Dynamic Mode AFM

    NASA Astrophysics Data System (ADS)

    Guan, Dongshi; Hang, Zhi Hong; Marcet, Zsolt; Liu, Hui; Kravchenko, I. I.; Chan, C. T.; Chan, H. B.; Tong, Penger

    2015-11-01

    Plasmonic nanostructures have attracted much attention in recent years because of their potential applications in optical manipulation through near-field enhancement. Continuing experimental efforts have been made to develop accurate techniques to directly measure the near-field optical force induced by the plasmonic nanostructures in the visible frequency range. In this work, we report a new application of dynamic mode atomic force microscopy (DM-AFM) in the measurement of the enhanced optical force acting on a nano-structured plasmonic resonant cavity. The plasmonic cavity is made of an upper gold-coated glass sphere and a lower quartz substrate patterned with an array of subwavelength gold disks. In the near-field when the sphere is positioned close to the disk array, plasmonic resonance is excited in the cavity and the induced force by a 1550 nm infrared laser is found to be increased by an order of magnitude compared with the photon pressure generated by the same laser light. The experiment demonstrates that DM-AFM is a powerful tool for the study of light induced forces and their enhancement in plasmonic nanostructures.

  15. Determination of the properties of viscoelastic materials using spherical nanoindentation

    NASA Astrophysics Data System (ADS)

    Martynova, Elena

    2016-02-01

    The article is devoted to determining the properties of linearly viscoelastic isotropic materials from the experiment on the introduction of a spherical indenter at a constant-rate displacement in a viscoelastic sample. The results are based on the Lee-Radok (J. Appl. Mech. 27:438-444, 1960) solution of the viscoelastic contact problem. An exact formula is obtained for calculation of the relaxation function using indentation load-displacement data. To illustrate the application of this formula, it is used to find the relaxation function of polymethyl methacrylate (PMMA). The relaxation function found in the article is compared with data measured in a conventional test to evaluate the suitability of the proposed method.

  16. An approach towards 3D sensitive AFM cantilevers

    NASA Astrophysics Data System (ADS)

    Koops, Richard; Fokkema, Vincent

    2014-04-01

    The atomic force microscope (AFM) tapping mode is a highly sensitive local probing technique that is very useful to study and measure surface properties down to the atomic scale. The tapping mode is mostly implemented using the resonance of the first bending mode of the cantilever and therefore provides sensitivity mainly along the direction of this oscillation. Driven by the semiconductor industry, there is an increasing need for accurate measurements of nanoscale structures for side wall characterization by AFM that requires additional sensitivity in the lateral direction. The conventional tapping mode has been augmented by various authors, for example by tilting the cantilever system (Cho et al 2011 Rev. Sci. Instrum. 82 023707) to access the sidewall or using a torsion mode (Dai et al 2011 Meas. Sci. Technol. 22 094009) of the cantilever to provide additional lateral sensitivity. These approaches however trade lateral sensitivity for vertical sensitivity or still lack sensitivity in the remaining lateral direction. We present an approach towards true 3D sensitivity for AFM cantilevers based on simultaneous excitation and optical detection of multiple cantilever resonance modes along three axes. Tuning the excitation of the cantilever to specific frequencies provides a mechanism to select only those cantilever modes that have the desired characteristics. Additionally, cantilever engineering has been used to design and create a substructure within the cantilever that has been optimized for specific resonance behavior around 4 MHz. In contrast to the conventional approach of using a piezo to actuate the cantilever modulation, we present results on photo-thermal excitation using an intensity modulated low-power laser source. By tightly focusing the excitation spot on the cantilever we were able to attain a deflection efficiency of 0.7 nm µW-1 for the first bending mode. The presented approach results in an efficient all optical excitation and deflection detection

  17. The Advancing State of AF-M315E Technology

    NASA Technical Reports Server (NTRS)

    Masse, Robert; Spores, Ronald A.; McLean, Chris

    2014-01-01

    The culmination of twenty years of applied research in hydroxyl ammonium nitrate (HAN)-based monopropellants, the NASA Space Technology mission Directorate's (STMD) Green Propellant Infusion Mission (GPIM) will achieve the first on-orbit demonstration of an operational AF-M315E green propellant propulsion system by the end of 2015. Following an contextual overview of the completed flight design of the GPIM propellant storage and feed system, results of first operation of a flight-representative heavyweight 20-N engineering model thruster (to be conducted in mid-2014) are presented with performance comparisons to prior lab model (heavyweight) test articles.

  18. Comparison of dynamic lever STM and noncontact AFM

    NASA Astrophysics Data System (ADS)

    Guggisberg, M.; Bammerlin, M.; Lüthi, R.; Loppacher, C.; Battiston, F.; Lü, J.; Baratoff, A.; Meyer, E.; Güntherodt, H.-J.

    We investigate interaction effects which occur in scanning tunneling microscopy (STM) by performing local force spectroscopy with an oscillating tip while imaging Si(111)7×7 terraces in the dynamic lever STM mode (constant time-averaged current). It is found that true atomic resolution is achieved close to the minimum of the resonance frequency vs. distance curve and even closer to the sample. On the other hand true atomic resolution in noncontact AFM (constant frequency shift) is expected several nm away from this minimum, in the range where the frequency shift becomes more negative with decreasing distance.

  19. The Emergence of AFM Applications to Cell Biology: How new technologies are facilitating investigation of human cells in health and disease at the nanoscale

    PubMed Central

    Yang, Ruiguo; Xi, Ning; Fung, Carmen Kar Man; Seiffert-Sinha, Kristina; Lai, King Wai Chiu; Sinha, Animesh A.

    2013-01-01

    Atomic Force Microscopy (AFM) based nanorobotics has been used for building nano devices in semiconductors for almost a decade. Leveraging the unparallel precision localization capabilities of this technology, high resolution imaging and mechanical property characterization is now increasingly being performed in biological settings. AFM also offers the prospect for handling and manipulating biological materials at nanometer scale. It has unique advantages over other methods, permitting experiments in the liquid phase where physiological conditions can be maintained. Taking advantage of these properties, our group has visualized membrane and cytoskeletal structures of live cells by controlling the interaction force of the AFM tip with cellular components at the nN or sub-nN range. Cell stiffness changes were observed by statistically analyzing the Young’s modulus values of human keratinocytes before and after specific antibody treatment. Furthermore, we used the AFM cantilever as a robotic arm for mechanical pushing, pulling and cutting to perform nanoscale manipulations of cell-associated structures. AFM guided nano-dissection, or nanosurgery was enacted on the cell in order to sever intermediate filaments connecting neighboring keratinocytes via sub 100 nm resolution cuts. Finally, we have used a functionalized AFM tip to probe cell surface receptors to obtain binding force measurements. This technique formed the basis for Single Molecule Force Spectroscopy (SMFS). In addition to enhancing our basic understanding of dynamic signaling events in cell biology, these advancements in AFM based biomedical investigations can be expected to facilitate the search for biomarkers related to disease diagnosis progress and treatment. PMID:24416719

  20. Scale effects of nanomechanical properties and deformation behavior of Au nanoparticle and thin film using depth sensing nanoindentation

    PubMed Central

    Maharaj, Dave

    2014-01-01

    Summary Nanoscale research of bulk solid surfaces, thin films and micro- and nano-objects has shown that mechanical properties are enhanced at smaller scales. Experimental studies that directly compare local with global deformation are lacking. In this research, spherical Au nanoparticles, 500 nm in diameter and 100 nm thick Au films were selected. Nanoindentation (local deformation) and compression tests (global deformation) were performed with a nanoindenter using a sharp Berkovich tip and a flat punch, respectively. Data from nanoindentation studies were compared with bulk to study scale effects. Nanoscale hardness of the film was found to be higher than the nanoparticles with both being higher than bulk. Both nanoparticles and film showed increasing hardness for decreasing penetration depth. For the film, creep and strain rate effects were observed. In comparison of nanoindentation and compression tests, more pop-ins during loading were observed during the nanoindentation of nanoparticles. Repeated compression tests of nanoparticles were performed that showed a strain hardening effect and increased pop-ins during subsequent loads. PMID:24991519

  1. Scale effects of nanomechanical properties and deformation behavior of Au nanoparticle and thin film using depth sensing nanoindentation.

    PubMed

    Maharaj, Dave; Bhushan, Bharat

    2014-01-01

    Nanoscale research of bulk solid surfaces, thin films and micro- and nano-objects has shown that mechanical properties are enhanced at smaller scales. Experimental studies that directly compare local with global deformation are lacking. In this research, spherical Au nanoparticles, 500 nm in diameter and 100 nm thick Au films were selected. Nanoindentation (local deformation) and compression tests (global deformation) were performed with a nanoindenter using a sharp Berkovich tip and a flat punch, respectively. Data from nanoindentation studies were compared with bulk to study scale effects. Nanoscale hardness of the film was found to be higher than the nanoparticles with both being higher than bulk. Both nanoparticles and film showed increasing hardness for decreasing penetration depth. For the film, creep and strain rate effects were observed. In comparison of nanoindentation and compression tests, more pop-ins during loading were observed during the nanoindentation of nanoparticles. Repeated compression tests of nanoparticles were performed that showed a strain hardening effect and increased pop-ins during subsequent loads. PMID:24991519

  2. Plastic deformation behaviors of Ni- and Zr-based bulk metallic glasses subjected to nanoindentation

    SciTech Connect

    Weizhong, Liang; Zhiliang, Ning; Zhenqian, Dang; Linzhi, Wu

    2013-12-15

    Plastic deformation behaviors of Ni{sub 42}Ti{sub 20}Zr{sub 21.5}Al{sub 8}Cu{sub 5}Si{sub 3.5} and Zr{sub 51}Ti{sub 5}Ni{sub 10}Cu{sub 25}Al{sub 9} bulk metallic glasses at room temperature were studied by nanoindentation testing and atomic force microscopy under equivalent indentation experimental conditions. The different chemical composition of these two bulk metallic glasses produced variant tendencies for displacement serrated flow to occur during the loading process. The nanoindentation strain rate was calculated as a function of indentation displacement in order to verify the occurrence of displacement serrated flow at different loading rates. Atomic force microscopy revealed decreasing numbers of discrete shear bands around the indentation sites as loading rates increased from 0.025 to 2.5 mNs{sup −1}. Variations in plastic deformation behaviors between Ni and Zr-based glasses materials can be explained by the different metastable microstructures and thermal stabilities of the two materials. The mechanism governing plastic deformation of these metallic glasses was analyzed in terms of an established model of the shear transformation zone. - Highlights: • Plastic deformation of Ni- and Zr-based BMG is studied under identical conditions • Zr-based BMG undergoes a greater extent of plastic deformation than Ni-based BMG • Nanoindentation strain rate is studied to clarify variation in plastic deformation • Metastable microstructure, thermal stability affect BMG plastic deformation.

  3. Physical properties of polyacrylamide gels probed by AFM and rheology

    NASA Astrophysics Data System (ADS)

    Abidine, Yara; Laurent, Valérie M.; Michel, Richard; Duperray, Alain; Iulian Palade, Liviu; Verdier, Claude

    2015-02-01

    Polymer gels have been shown to behave as viscoelastic materials but only a small amount of data is usually provided in the glass transition. In this paper, the dynamic moduli G\\prime and G\\prime\\prime of polyacrylamide hydrogels are investigated using both an AFM in contact force modulation mode and a classical rheometer. The validity is shown by the matching of the two techniques. Measurements are carried out on gels of increasing polymer concentration in a wide frequency range. A model based on fractional derivatives is successfully used, covering the whole frequency range. G\\text{N}0 , the plateau modulus, as well as several other parameters are obtained at low frequencies. The model also predicts the slope a of both moduli in the glass transition, and a transition frequency f\\text{T} is introduced to separate the gel-like behavior with the glassy state. Its variation with polymer content c gives a dependence f\\text{T}∼ c1.6 , in good agreement with previous theories. Therefore, the AFM data provides new information on the physics of polymer gels.

  4. Dual AFM probes alignment based on vision guidance

    NASA Astrophysics Data System (ADS)

    Zhang, Hua-kun; Gao, Si-tian; Lu, Ming-zhen; Wang, Long-long

    2013-10-01

    Atomic force microscope (AFM) with dual probes that operate together can measure both side walls excellently at the same time, which virtually eliminates the prevalent effect of probe width that contributes a large component of uncertainty in measurement results and finally obtains the critical dimension (CD)(e.g. the linewidth) through data synthesis. In calibration process, the dual probes must contact each other in advance, which realizes the alignment in the three dimensions, to establish a zero reference point and ensure the accuracy of measurement. Because nowadays the optical resolution of advanced lens have exceeded micrometer range, and the size of probes is within micro level, it is possible to acquire dual probes images in both horizontal and vertical directions, through which the movement of the probes can be controlled in time. In order to further enhance the alignment precision, sub-pixel edge detection method based on Zernike orthogonal moment is used to obtain relative position between these two probes, which helps the tips alignment attains sub-micron range. Piezoelectric nanopositioning stages calibrated by laser interferometer are used to implement fine movement of the probes to verify the accuracy of the experimental results. To simplify the system, novel self-sensing and self-actuating probe based on a quartz tuning fork combined with a micromachined cantilever is used for dynamic mode AFM. In this case, an external optical detection system is not needed, so the system is simple and small.

  5. Viscoelasticity of gelatin surfaces probed by AFM noise analysis.

    PubMed

    Benmouna, Farida; Johannsmann, Diethelm

    2004-01-01

    The viscoelastic properties of surfaces of swollen gelatin were investigated by analyzing the Brownian motion of an atomic force microscopy (AFM) cantilever in contact with the gel surface. A micron-sized glass sphere attached to the AFM cantilever is used as the dynamic probe. When the sphere approaches the gelatin surface, there is a static repulsive force without a jump into contact. The cantilever's Brownian movement is monitored in parallel, providing access to the dynamic sphere-surface interaction as quantified by the dynamic spring constant, kappa, and the drag coefficient, xi. Gelatin is used as a model substance for a variety of other soft surfaces, where the stiffness of the gel can be varied via the solvent quality, the bloom number, and the pH. The modulus derived from the static force-distance curve is in the kPa range, consistent with the literature. However, the dynamic spring constant as derived from the Brownian motion is much larger than the static differential spring constant dF/dz. On retraction, one observes a rather strong adhesion hysteresis. The strength of the bridge (as given by the dynamic spring constant and the drag coefficient) is very small. PMID:15745019

  6. Analysis of AFM cantilever dynamics close to sample surface

    NASA Astrophysics Data System (ADS)

    Habibnejad Korayem, A.; Habibnejad Korayem, Moharam; Ghaderi, Reza

    2013-07-01

    For imaging and manipulation of biological specimens application of atomic force microscopy (AFM) in liquid is necessary. In this paper, tapping-mode AFM cantilever dynamics in liquid close to sample surface is modeled and simulated by well defining the contact forces. The effect of cantilever tilting angle has been accounted carefully. Contact forces have some differences in liquid in comparison to air or vacuum in magnitude or formulation. Hydrodynamic forces are also applied on the cantilever due to the motion in liquid. A continuous beam model is used with its first mode and forward-time simulation method for simulation of its hybrid dynamics and the frequency response and amplitude versus separation diagrams are extracted. The simulation results show a good agreement with experimental results. The resonance frequency in liquid is so small in comparison to air due to additional mass and also additional damping due to the viscosity of the liquid around. The results show that the effect of separation on free vibration amplitude is great. Its effect on resonance frequency is considerable too.

  7. Iron oxide mineral-water interface reactions studied by AFM

    SciTech Connect

    Hawley, M.E.; Rogers, P.S.Z.

    1994-07-01

    Natural iron mineral surfaces have been examined in air by atomic force (AFM) and scanning tunneling (STM) microscopies. A number of different surface features were found to be characteristic of the native surface. Even surfaces freshly exposed by crushing larger crystals were found to have a pebbly surface texture caused by the presence of thin coatings of what might be surface precipitates. This finding is interpreted as evidence for previous exposure to water, probably through an extensive network of microfractures. Surface reactions on the goethite crystals were studied by AFM at size resolutions ranging from microns to atomic resolution before, during, and after reaction with distilled water and 0.lN HCl. Immediate and extensive surface reconfiguration occurred on contact with water. In one case, after equilibration with water for 3 days, surface reprecipitation, etching and pitting were observed. Atomic resolution images taken under water were found to be disordered. The result of surface reaction was generally to increase the surface area substantially through the extension of surface platelet arrays, present prior to reaction. This work is being done in support of the site characterization project at Yucca Mountain.

  8. Pathogen identification using peptide nanotube biosensors and impedance AFM

    NASA Astrophysics Data System (ADS)

    Maccuspie, Robert I.

    Pathogen identification at highly sensitive levels is crucial to meet urgent needs in fighting the spread of disease or detecting bioterrorism events. Toward that end, a new method for biosensing utilizing fluorescent antibody nanotubes is proposed. Fundamental studies on the self-assembly of these peptide nanotubes are performed, as are applications of aligning these nanotubes on surfaces. As biosensors, these nanotubes incorporate recognition units with antibodies at their ends and fluorescent signaling units at their sidewalls. When viral pathogens were mixed with these antibody nanotubes in solution, the nanotubes rapidly aggregated around the viruses. The size of the aggregates increased as the concentration of viruses increased, as detected by flow cytometry on the order of attomolar concentrations by changes in fluorescence and light scattering intensities. This enabled determination of the concentrations of viruses at trace levels (102 to 106 pfu/mL) within 30 minutes from the receipt of samples to the final quantitative data analysis, as demonstrated on Adenovirus, Herpes Simplex Virus, Influenza, and Vaccinia virus. As another separate approach, impedance AFM is used to study the electrical properties of individual viruses and nanoparticles used as model systems. The design, development, and implementation of the impedance AFM for an Asylum Research platform is described, as well as its application towards studying the impedance of individual nanoparticles as a model system for understanding the fundamental science of how the life cycle of a virus affects its electrical properties. In combination, these approaches fill a pressing need to quantify viruses both rapidly and sensitively.

  9. Comparison of particle sizes determined with impactor, AFM and SEM

    NASA Astrophysics Data System (ADS)

    Gwaze, Patience; Annegarn, Harold J.; Huth, Joachim; Helas, Günter

    2007-11-01

    Particles size comparisons were made between conventional aerodynamic and mobility sizing techniques and physical geometric sizes measured by high resolution microscopes. Atmospheric particles were collected during the wet and dry seasons in the Amazonian ecosystems. Individual particles deposited on four stages of the MOUDI (Micro-Orifice Uniform Deposition Impactor) were characterised for particle volumes, projected surface diameters and morphologies with an Atomic Force Microscope (AFM) and a Scanning Electron Microscope (SEM). AFM and SEM size distributions were verified against distributions derived from response functions of individual MOUDI stages as specified by Winklmayr et al. [Winklmayr, W., Wang, H.-C., John, W., 1990. Adaptation of the Twomey algorithm to the inversion of cascade impactor data. Aerosol Science and Technology 13, 322-331.]. Particles indicated inherent discrepancies in sizing techniques. Particle volumes were systematically lower than expected by factors of up to 3.6. Differences were attributed to loss of mass, presumably water adsorbed on particles. Losses were high and could not be accounted for by measured humidity growth factors suggesting significant losses of other volatile compounds as well, particularly on particles that were collected during the wet season. Microscopy results showed that for hygroscopic particles, microscopy sizes depend on the relative humidity history of particles before and after sampling. Changes in relative humidity significantly altered particle morphologies. Depending on when changes occur, such losses will bias not only microscopy particle sizes but also impactor mass distributions and number concentrations derived from collected particles.

  10. AFM analysis of bleaching effects on dental enamel microtopography

    NASA Astrophysics Data System (ADS)

    Pedreira de Freitas, Ana Carolina; Espejo, Luciana Cardoso; Botta, Sergio Brossi; Teixeira, Fernanda de Sa; Luz, Maria Aparecida A. Cerqueira; Garone-Netto, Narciso; Matos, Adriana Bona; Salvadori, Maria Cecilia Barbosa da Silveira

    2010-02-01

    The purpose of this in vitro study was to test a new methodology to evaluate the effects of 35% hydrogen peroxide agent on the microtopography of sound enamel using an atomic force microscope (AFM). The buccal sound surfaces of three extracted human lower incisors were used, without polishing the surfaces to maintain them with natural morphology. These unpolished surfaces were subjected to bleaching procedure with 35% hydrogen peroxide that consisted of 4 applications of the bleaching agent on enamel surfaces for 10 min each application. Surface images were obtained in a 15 μm × 15 μm area using an AFM. The roughness (Ra and RMS) and the power spectral density (PSD) were obtained before and after the bleaching treatment. As results we could inquire that the PSD analyses were very suitable to identifying the morphological changes on the surfaces, while the Ra and RMS parameters were insufficient to represent the morphological alterations promoted by bleaching procedure on enamel. The morphological wavelength in the range of visible light spectrum (380-750 nm) was analyzed, showing a considerable increase of the PSD with the bleaching treatment.

  11. Discrete drops in the electrical contact resistance during nanoindentation of a bulk metallic glass

    NASA Astrophysics Data System (ADS)

    Singh, Gaurav; Narayan, R. L.; Asiri, A. M.; Ramamurty, U.

    2016-05-01

    Simultaneous measurement of the electrical contact resistance (ECR) during nanoindentation of a Pd-based bulk metallic glass (BMG) shows discontinuities in the current during the loading segment. Through an analysis of the effective change in the contact area that occurs due to the plastic flow via shear banding, we show that the current surges, which are synchronous with the displacement bursts, are associated with shear band nucleation and/or propagation. The potential of nano-ECR measurements for monitoring plastic events in BMGs is discussed.

  12. Atomic force microscopy based nanoindentation study of onion abaxial epidermis walls in aqueous environment

    NASA Astrophysics Data System (ADS)

    Xi, Xiaoning; Kim, Seong H.; Tittmann, Bernhard

    2015-01-01

    An atomic force microscopy based nanoindentation method was employed to study how the structure of cellulose microfibril packing and matrix polymers affect elastic modulus of fully hydrated primary plant cell walls. The isolated, single-layered abaxial epidermis cell wall of an onion bulb was used as a test system since the cellulose microfibril packing in this cell wall is known to vary systematically from inside to outside scales and the most abundant matrix polymer, pectin, can easily be altered through simple chemical treatments such as ethylenediaminetetraacetic acid and calcium ions. Experimental results showed that the pectin network variation has significant impacts on the cell wall modulus, and not the cellulose microfibril packing.

  13. Elastic constants determined by nanoindentation for p-type thermoelectric half-Heusler

    SciTech Connect

    Gahlawat, S.; Wheeler, L.; White, K. W. E-mail: kwwhite@uh.edu; He, R.; Chen, S.; Ren, Z. F. E-mail: kwwhite@uh.edu

    2014-08-28

    This paper presents a study of the elastic properties of the p-type thermoelectric half-Heusler material, Hf{sub 0.44}Zr{sub 0.44}Ti{sub 0.12}CoSb{sub 0.8}Sn{sub 0.2}, using nanoindentation. Large grain-sized polycrystalline specimens were fabricated for these measurements, providing sufficient indentation targets within single grains. Electron Backscatter Diffraction methods indexed the target grains for the correlation needed for our elastic analysis of individual single crystals for this cubic thermoelectric material. Elastic properties, including the Zener ratio and the Poisson ratio, obtained from the elasticity tensor are also reported.

  14. Effect of tip radius on the incipient plasticity of chromium studied by nanoindentation

    DOE PAGESBeta

    Wu, Dong; Morris, James R.; Nieh, T. G.

    2014-10-01

    The onset of plasticity in Cr was investigated by nanoindentation using indenters with tip radii ranging from 60 to 759 nm. The stress for incipient plasticity was found to increase with decreasing tip radius. We find that the cumulative pop-in probability on load could be described successfully by a combined model over the full range of tip radius, indicating that the incipient plasticity might be triggered either by the homogeneous nucleation of dislocation or by the activation of existing dislocations underneath the indenter.

  15. Temperature-dependent mechanical properties of single-layer molybdenum disulphide: Molecular dynamics nanoindentation simulations

    NASA Astrophysics Data System (ADS)

    Zhao, Junhua; Jiang, Jin-Wu; Rabczuk, Timon

    2013-12-01

    The temperature-dependent mechanical properties of single-layer molybdenum disulphide (MoS2) are obtained using molecular dynamics (MD) nanoindentation simulations. The Young's moduli, maximum load stress, and maximum loading strain decrease with increasing temperature from 4.2 K to 500 K. The obtained Young's moduli are in good agreement with those using our MD uniaxial tension simulations and the available experimental results. The tendency of maximum loading strain with different temperature is opposite with that of metal materials due to the short range Stillinger-Weber potentials in MoS2. Furthermore, the indenter tip radius and fitting strain effect on the mechanical properties are also discussed.

  16. Atomic force microscopy based nanoindentation study of onion abaxial epidermis walls in aqueous environment

    SciTech Connect

    Xi, Xiaoning; Tittmann, Bernhard; Kim, Seong H.

    2015-01-14

    An atomic force microscopy based nanoindentation method was employed to study how the structure of cellulose microfibril packing and matrix polymers affect elastic modulus of fully hydrated primary plant cell walls. The isolated, single-layered abaxial epidermis cell wall of an onion bulb was used as a test system since the cellulose microfibril packing in this cell wall is known to vary systematically from inside to outside scales and the most abundant matrix polymer, pectin, can easily be altered through simple chemical treatments such as ethylenediaminetetraacetic acid and calcium ions. Experimental results showed that the pectin network variation has significant impacts on the cell wall modulus, and not the cellulose microfibril packing.

  17. EBSD and Nanoindentation-Correlated Study of Delamination Fracture in Al-Li Alloy 2090

    NASA Technical Reports Server (NTRS)

    Tayon, Wesley A.; Crooks, Roy E.; Domack, Marcia S.; Wagner, John A.; Elmustafa, A. A.

    2008-01-01

    Al-Li alloys offer attractive combinations of high strength and low density. However, a tendency for delamination fracture has limited their use. A better understanding of the delamination mechanisms may identify methods to control delaminations through processing modifications. A combination of new techniques has been used to evaluate delamination fracture in Al-Li alloys. Both high quality electron backscattered diffraction (EBSD) information and valid nanoindentation measurements were obtained from fractured test specimens. Correlations were drawn between nano-scale hardness variations and local texture along delaminating boundaries. Intriguing findings were observed for delamination fracture through the combined analysis of grain orientation, Taylor factor, and kernel average misorientation.

  18. The formation of wrinkles in single-layer graphene sheets under nanoindentation

    NASA Astrophysics Data System (ADS)

    Gil, A. J.; Adhikari, S.; Scarpa, F.; Bonet, J.

    2010-04-01

    We investigate the formation of wrinkles and bulging in single-layer graphene sheets using an equivalent atomistic continuum nonlinear hyperelastic theory for nanoindentation and nanopressurization. We show that nonlinear geometrical effects play a key role in the development of wrinkles. Without abandoning the classical tension field membrane theory, we develop an enhanced model based upon the minimization of a relaxed energy functional in conjunction with nonlinear finite hyperelasticity. Formation of wrinkles are observed in rectangular graphene sheets due to the combination of induced membrane tension and edge effects under external pressure.

  19. Surface Effects on Young's Modulud and Hardness of Fused Silica by Nanoindentation Study

    SciTech Connect

    Zheng, L.; Schmid, A.W.; Lambropoulos, J.C.

    2007-01-24

    The surface Young's modulus (E) and hardness (H) of fused silica samples have been studied by nanoindentation. Two factors strongly affect the results of E and H. One factor is the polishing quality of the fused silica surface. Poor polishing quality produces much smaller E and H than the literature values for bulk fused silica. The second factor is surface flatness. Even for a well-polished silica surface, an "arch bridge effect" may hinder the measurements of the true values of E and H. A correction procedure is proposed to eliminate this effect, and the corrected results show substantial improvements.

  20. Photoinduced stiffening and photoplastic effect of ZnS individual nanobelt in nanoindentation

    SciTech Connect

    Zheng, X. J.; Yu, G. C.; Chen, Y. Q.; Mao, S. X.; Zhang, T.

    2010-11-15

    The photoinduced stiffening (PIS) and photoplastic effect (PPE) of ZnS individual nanobelt (NB) were observed by using a nanoindenter in conjunction with an incident ultraviolet (UV) light source system. The results show that the elastic modulus and hardness of ZnS individual NB under UV illumination are at least 32% and 20% larger than those in darkness. The mechanisms of PIS and PPE are interpreted by the increase in electronic strain and Peierls barrier due to the photogeneration of free carriers in ZnS individual NB. The research may offer useful guidelines to the application of optoelectronic devices based on individual nanostructures.

  1. Hydrodynamic effects of the tip movement on surface nanobubbles: a combined tapping mode, lift mode and force volume mode AFM study.

    PubMed

    Walczyk, Wiktoria; Hain, Nicole; Schönherr, Holger

    2014-08-28

    We report on an Atomic Force Microscopy (AFM) study of AFM tip-nanobubble interactions in experiments conducted on argon surface nanobubbles on HOPG (highly oriented pyrolytic graphite) in water in tapping mode, lift mode and Force Volume (FV) mode AFM. By subsequent data acquisition on the same nanobubbles in these three different AFM modes, we could directly compare the effect of different tip-sample interactions. The tip-bubble interaction strength was found to depend on the vertical and horizontal position of the tip on the bubble with respect to the bubble center. The interaction forces measured experimentally were in good agreement with the forces calculated using the dynamic interaction model. The strength of the hydrodynamic effect was also found to depend on the direction of the tip movement. It was more pronounced in the FV mode, in which the tip approaches the bubble from the top, than in the lift mode, in which the tip approaches the bubble from the side. This result suggests that the direction of tip movement influences the bubble deformation. The effect should be taken into account when nanobubbles are analysed by AFM in various scanning modes. PMID:24988375

  2. The use of nanoindentation for characterizing the properties of mineralized hard tissues: state-of-the art review.

    PubMed

    Lewis, Gladius; Nyman, Jeffry S

    2008-10-01

    The use of nanoindentation to determine nanomechanical properties of mineralized tissues has been investigated extensively. A detailed, critical, and comprehensive review of this literature is the subject of the present work. After stating the motivation for the review, a succinct presentation of the challenges, advantages, and disadvantages of the various quasi-static nanoindentation test methods (to obtain elastic modulus, E, and hardness, H) and dynamic test methods (to obtain storage and loss moduli and/or loss/damping factor) is given in the form of a primer. Explicative summaries of literature reports on various intrinsic and extrinsic factors that significantly influence E and H, followed by 15 suggested topics for future research, are included additionally. This review is designed to present a compact guide to the principles of the nanoindentation technique and to emphasize considerations when determining material properties of mineralized tissues. PMID:18395829

  3. Analysis of In Situ Mechanical Properties of Phases in High-Alloyed White Iron Measured by Grid Nanoindentation

    NASA Astrophysics Data System (ADS)

    Chen, Ling; Ståhl, Jan Eric; Zhou, Jinming

    2015-10-01

    The paper presents an analysis of the in situ mechanical properties (e.g., hardness, elastic modulus, and volume fraction) of phases in high-alloy white iron measured by grid nanoindentation statistically, to reveal the contributions of individual phase properties to the global properties of the material. The in situ mechanical properties of phases measured by grid indentation were validated through targeted indentation. Gaussian and Weibull mixture models were used in analyzing the grid nanoindentation measurements to assess the goodness-of-fit of the indentation data. The nanohardness and indentation modulus measured by grid nanoindentation were directly correlated to the microstructural characteristics of the sample materials. The statistical analysis results were also compared with the mechanical properties and volume fractions obtained using targeted indentation and quantitative metallography based on microstructure analysis to validate the statistical results. The influences of heat treatment on the microstructure, hardness, and elastic modulus of individual phases in the material are also discussed.

  4. Nanoindentation testing and finite element simulations of cortical bone allowing for anisotropic elastic and inelastic mechanical response.

    PubMed

    Carnelli, Davide; Lucchini, Riccardo; Ponzoni, Matteo; Contro, Roberto; Vena, Pasquale

    2011-07-01

    Anisotropy is one of the most peculiar aspects of cortical bone mechanical behaviour, and the numerical approach can be successfully used to investigate aspects of bone tissue mechanics that analytical methods solve in approximate way or do not cover. In this work, nanoindentation experimental tests and finite element simulations were employed to investigate the elastic-inelastic anisotropic mechanical properties of cortical bone. The model allows for anisotropic elastic and post-yield behaviour of the tissue. A tension-compression mismatch and direction-dependent yield stresses are allowed for. Indentation experiments along the axial and transverse directions were simulated with the purpose to predict the indentation moduli and hardnesses along multiple orientations. Results showed that the experimental transverse-to-axial ratio of indentation moduli, equal to 0.74, is predicted with a ∼3% discrepancy regardless the post-yield material behaviour; whereas, the transverse-to-axial hardness ratio, equal to 0.86, can be correctly simulated (discrepancy ∼6% w.r.t. the experimental results) only employing an anisotropic post-elastic constitutive model. Further, direct comparison between the experimental and simulated indentation tests evidenced a good agreement in the loading branch of the indentation curves and in the peak loads for a transverse-to-axial yield stress ratio comparable to the experimentally obtained transverse-to-axial hardness ratio. In perspective, the present work results strongly support the coupling between indentation experiments and FEM simulations to get a deeper knowledge of bone tissue mechanical behaviour at the microstructural level. The present model could be used to assess the effect of variations of constitutive parameters due to age, injury, and/or disease on bone mechanical performance in the context of indentation testing. PMID:21570077

  5. The importance of correcting for variable probe-sample interactions in AFM-IR spectroscopy: AFM-IR of dried bacteria on a polyurethane film.

    PubMed

    Barlow, Daniel E; Biffinger, Justin C; Cockrell-Zugell, Allison L; Lo, Michael; Kjoller, Kevin; Cook, Debra; Lee, Woo Kyung; Pehrsson, Pehr E; Crookes-Goodson, Wendy J; Hung, Chia-Suei; Nadeau, Lloyd J; Russell, John N

    2016-08-01

    AFM-IR is a combined atomic force microscopy-infrared spectroscopy method that shows promise for nanoscale chemical characterization of biological-materials interactions. In an effort to apply this method to quantitatively probe mechanisms of microbiologically induced polyurethane degradation, we have investigated monolayer clusters of ∼200 nm thick Pseudomonas protegens Pf-5 bacteria (Pf) on a 300 nm thick polyether-polyurethane (PU) film. Here, the impact of the different biological and polymer mechanical properties on the thermomechanical AFM-IR detection mechanism was first assessed without the additional complication of polymer degradation. AFM-IR spectra of Pf and PU were compared with FTIR and showed good agreement. Local AFM-IR spectra of Pf on PU (Pf-PU) exhibited bands from both constituents, showing that AFM-IR is sensitive to chemical composition both at and below the surface. One distinct difference in local AFM-IR spectra on Pf-PU was an anomalous ∼4× increase in IR peak intensities for the probe in contact with Pf versus PU. This was attributed to differences in probe-sample interactions. In particular, significantly higher cantilever damping was observed for probe contact with PU, with a ∼10× smaller Q factor. AFM-IR chemical mapping at single wavelengths was also affected. We demonstrate ratioing of mapping data for chemical analysis as a simple method to cancel the extreme effects of the variable probe-sample interactions. PMID:27403761

  6. AFM CHARACTERIZATION OF RAMAN LASER INDUCED DAMAGE ON CDZNTECRYSTAL SURFACES

    SciTech Connect

    Teague, L.; Duff, M.

    2008-10-07

    High quality CdZnTe (or CZT) crystals have the potential for use in room temperature gamma-ray and X-ray spectrometers. Over the last decade, the methods for growing high quality CZT have improved the quality of the produced crystals however there are material features that can influence the performance of these materials as radiation detectors. The presence of structural heterogeneities within the crystals, such as twinning, pipes, grain boundaries (polycrystallinity), and secondary phases (SPs) can have an impact on the detector performance. There is considerable need for reliable and reproducible characterization methods for the measurement of crystal quality. With improvements in material characterization and synthesis, these crystals may become suitable for widespread use in gamma radiation detection. Characterization techniques currently utilized to test for quality and/or to predict performance of the crystal as a gamma-ray detector include infrared (IR) transmission imaging, synchrotron X-ray topography, photoluminescence spectroscopy, transmission electron microscopy (TEM), atomic force microscopy (AFM) and Raman spectroscopy. In some cases, damage caused by characterization methods can have deleterious effects on the crystal performance. The availability of non-destructive analysis techniques is essential to validate a crystal's quality and its ability to be used for either qualitative or quantitative gamma-ray or X-ray detection. The work presented herein discusses the damage that occurs during characterization of the CZT surface by a laser during Raman spectroscopy, even at minimal laser powers. Previous Raman studies have shown that the localized annealing from tightly focused, low powered lasers results in areas of higher Te concentration on the CZT surface. This type of laser damage on the surface resulted in decreased detector performance which was most likely due to increased leakage current caused by areas of higher Te concentration. In this study

  7. Device level 3D characterization using PeakForce AFM

    NASA Astrophysics Data System (ADS)

    Timoney, Padraig; Zhang, Xiaoxiao; Vaid, Alok; Hand, Sean; Osborne, Jason; Milligan, Eric; Feinstein, Adam

    2016-03-01

    Traditional metrology solutions face a range of challenges at the 1X node such as three dimensional (3D) measurement capabilities, shrinking overlay and critical dimension (CD) error budgets driven by multi-patterning and via in trench CD measurements. With advent of advanced technology nodes and 3D processing, an increasing need is emerging for in-die metrology including across-structure and structure-to-structure characterization. A myriad of work has emerged in the past few years intending to address these challenges from various aspects; in-die OCD with reduced spot size and tilt beam on traditional critical dimension scanning electron microscopy (CDSEM) for height measurements. This paper explores the latest capability offered by PeakForceTM Tapping Atomic Force Microscopy (PFT-AFM). The use of traditional harmonic tapping mode for scanning high aspect ratio, and complex "3D" wafer structures, results in limited depth probing capability as well as excessive tip wear. These limitations arise due to the large tip-sample interaction volume in such confined spaces. PeakForce Tapping eliminates these limitations through direct real time control of the tip-sample interaction contact force. The ability of PeakForce to measure, and respond directly to tip- sample interaction forces results in more detailed feature resolution, reduced tip wear, and improved depth capability. In this work, the PFT-AFM tool was applied for multiple applications, including the 14nm fin and replacement metal gate (RMG) applications outlined below. Results from DOE wafers, detailed measurement precision studies and correlation to reference metrology are presented for validation of this methodology. With the fin application, precision of 0.3nm is demonstrated by measuring 5 dies with 10 consecutive runs. Capability to resolve within-die and localized within-macro height variation is also demonstrated. Results obtained from the fin measurements support the increasing trend that measurements

  8. 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

  9. Conductive-probe AFM characterization of graphene sheets bonded to gold surfaces

    NASA Astrophysics Data System (ADS)

    Hauquier, Fanny; Alamarguy, David; Viel, Pascal; Noël, Sophie; Filoramo, Arianna; Huc, Vincent; Houzé, Frédéric; Palacin, Serge

    2012-01-01

    Conducting probe atomic force microscopy (CP-AFM) has been used to perform mechanical and electrical experiments on graphene layers bonded to polyaminophenylene (PAP) films grafted on gold substrates. This technique is a new approach for the characterization of graphene sheets and represents a complementary tool to Raman spectroscopy. The combination of friction and electrical imaging reveals that different stacked graphene sheets have been successfully distinguished from each other and from the underlying PAP films. Lateral force microscopy has shown that the friction is greatly reduced on graphene sheets in comparison with the organic coating. The electrical resistance images show very different local conduction properties which can be linked to the number of underlying graphene sheets. The resistance decreases very slowly when the normal load increases. Current-voltage curves display characteristics of metal-molecule-metal junctions.

  10. Nanoindentation study of the superlattice hardening effect at TiC(110)/NbC(110) interfaces

    SciTech Connect

    Sekkal, W.; Zaoui, A.; Schmauder, S.

    2005-04-18

    We present an atomistic calculation using the embedded atom method in order to investigate nanoindentation in superlattices based on carbide materials. The purpose is to conduct a nanoindentation simulation study in order to evaluate the hardness of TiC and the one of TiC/NbC. Results clearly show that this calculated quantity increases considerably from the carbide alone to the carbide in sandwich with another one like NbC. This mainly highlights the possibility to increase the hardness of carbide materials and confirms theoretically the previous experimental deductions.

  11. Effect of tip mass on frequency response and sensitivity of AFM cantilever in liquid.

    PubMed

    Farokh Payam, Amir; Fathipour, Morteza

    2015-03-01

    The effect of tip mass on the frequency response and sensitivity of atomic force microscope (AFM) cantilever in the liquid environment is investigated. For this purpose, using Euler-Bernoulli beam theory and considering tip mass and hydrodynamic functions in a liquid environment, an expression for the resonance frequencies of AFM cantilever in liquid is derived. Then, based on this expression, the effect of the surface contact stiffness on the flexural mode of a rectangular AFM cantilever in fluid is investigated and compared with the case where the AFM cantilever operates in the air. The results show that in contrast with an air environment, the tip mass has no significant impact on the resonance frequency and sensitivity of the AFM cantilever in the liquid. Hence, analysis of AFM behaviour in liquid environment by neglecting the tip mass is logical. PMID:25562584

  12. Measuring the elastic modulus and residual stress of freestanding thin films using nanoindentation techniques

    SciTech Connect

    Herbert, E.; Oliver, W. C.; De Boer, Maarten P.; Pharr, George Mathews

    2009-01-01

    A new method is proposed to determine the elastic modulus and residual stress of freestanding thin films based on nanoindentation techniques. The experimentally measured stiffness-displacement response is applied to a simple membrane model that assumes the film deformation is dominated by stretching as opposed to bending. Dimensional analysis is used to identify appropriate limitations of the proposed model. Experimental verification of the method is demonstrated for Al/0.5 wt% Cu films nominally 22 {micro}m wide, 0.55 {micro}m thick, and 150, 300, and 500 {micro}m long. The estimated modulus for the four freestanding films match the value measured by electrostatic techniques to within 2%, and the residual stress to within 19.1%. The difference in residual stress can be completely accounted for by thermal expansion and a modest change in temperature of 3 C. Numerous experimental pitfalls are identified and discussed. Collectively, these data and the technique used to generate them should help future investigators make more accurate and precise measurements of the mechanical properties of freestanding thin films using nanoindentation.

  13. Mechanical properties of laser-deposited composite boride coating using nanoindentation

    SciTech Connect

    Agarwal, A.; Dahotre, N.B.

    2000-02-01

    Nanoindentation proves to be an effective technique to measure mechanical properties of composite materials, as it has high spatial resolution that enables estimation of properties even from fine grains, particles, and precipitates. The elastic modulus, E, of the composite boride coating deposited on AISI 1010 steel using the laser surface engineering (LSE) process has been computed using the nanoindentation technique. The highest E value of 477.3 GPa was achieved for coating in a sample that contained 0.69 volume fraction of TiB{sub 2} particles in the coating after processing with the highest laser traverse speed of 33 mm/s. A comparison between the theoretical and experimental computation of the elastic modulus suggests that theoretical elastic modulus values are lower than computed elastic modulus, as the latter includes the effect of dissolution of fine TiB{sub 2} particles in Fe matrix and metastable phase formation such as Fe{sub a}B{sub b} and Ti{sub m}B{sub n}. Dissolution of fine TiB{sub 2} particles in the Fe matrix in the coating region has been corroborated by transmission electron microscope (TEM) micrographs and corresponding energy-dispersive spectroscope (EDS) analysis and selected area diffraction (SAD) pattern.

  14. In Situ TEM Nanoindentation Studies on Stress-Induced Phase Transformations in Metallic Materials

    NASA Astrophysics Data System (ADS)

    Liu, Y.; Wang, H.; Zhang, X.

    2016-01-01

    Although abundant phase transformations are in general thermally driven processes, there are many examples wherein stresses can induce phase transformations. Numerous in situ techniques, such as in situ x-ray diffraction and neutron diffraction, have been applied to reveal phase transformations. Recently, an in situ nanoindentation technique coupled with transmission electron microscopy demonstrated the capability to directly correlating stresses with phase transformations and microstructural evolutions at a submicron length scale. Here we briefly review in situ studies on stress-induced diffusional and diffusionless phase transformations in amorphous CuZrAl alloy and NiFeGa shape memory alloy. In the amorphous CuZrAl, in situ nanoindentation studies show that the nucleation of nanocrystals (a diffusional process) occurs at ultra-low stresses manifested by a prominent stress drop. In the NiFeGa shape memory alloy, two distinctive types of martensitic (diffusionless) phase transformations accompanied by stress plateaus are observed, including a reversible gradual phase transformation at low stress levels, and an irreversible abrupt phase transition at higher stress levels.

  15. Deformation mechanisms during nanoindentation of sodium borosilicate glasses of nuclear interest

    SciTech Connect

    Kilymis, D. A.; Delaye, J.-M.

    2014-07-07

    In this paper we analyze results of Molecular Dynamics simulations of Vickers nanoindentation, performed for sodium borosilicate glasses of interest in the nuclear industry. Three glasses have been studied in their pristine form, as well as a disordered one that is analogous to the real irradiated glass. We focused in the behavior of the glass during the nanoindentation in order to reveal the mechanisms of deformation and how they are affected by microstructural characteristics. Results have shown a strong dependence on the SiO{sub 2} content of the glass, which promotes densification due to the open structure of SiO{sub 4} tetrahedra and also due to the strength of Si-O bonds. Densification for the glasses is primarily expressed by the relative decrease of the Si-O-Si and Si-O-B angles, indicating rotation of the structural units and decrease of free volume. The increase of alkali content on the other hand results to higher plasticity of the matrix and increased shear flow. The most important effect on the deformation mechanism of the disordered glasses is that of the highly depolymerized network that will also induce shear flow and, in combination with the increased free volume, will result in the decreased hardness of these glasses, as has been previously observed.

  16. Recent advances in small-scale mechanical property measurement by nanoindentation

    SciTech Connect

    Pharr, George Mathews

    2015-08-25

    Since its initial development in the early 1980’s [1], nanoindentation has matured into one of the premier testing techniques for measuring mechanical properties at the micrometer and sub-micrometer scales and has emerged as a critical tool that has helped to shape the nanotechnology revolution. At the heart of the technique are testing systems with simple but precise force actuators and displacement measuring devices that record the force–displacement record as a diamond indenter, usually the form of a pyramid or a sphere, is pressed into and withdrawn from a small region in the surface of a material of interest. The nano-scale force–displacement data, which can be obtained with a spatial resolution as small as a few nanometers, contains a wealth of information about the local mechanical properties [2], [3] and [4]. This enables the mechanical characterization of very thin films, like those used in the semiconductor, magnetic storage, and hard coatings industries, as well as very small precipitates, particles and second phases, many of which may not exist in bulk form and cannot be characterized by traditional mechanical testing methods. Here, computer automation of nanoindentation testing systems now routinely provides for complete two-dimensional mapping of properties over regions stretching from sub-micron to millimeters in scale.

  17. Measurement of residual stress in quenched 1045 steel by the nanoindentation method

    SciTech Connect

    Zhu Lina; Xu Binshi; Wang Haidou; Wang Chengbiao

    2010-12-15

    In this paper, the residual stress in quenched AISI 1045 steel was measured by a recently developed nanoindentation technique. Depth control mode was adopted to measure the residual stress. It was found that residual compressive stress was generated in the quenched steel. The material around nanoindents exhibits significant pile-up deformation. A new method was proposed to determine the real contact area for pile-up material on the basis of invariant pile-up morphology of the loaded or unloaded states. The results obtained by the new method were in good agreement with the residual stresses measured by the classical X-ray diffraction (XRD) method. - Research Highlights: {yields} A new method was proposed to measure the real contact area for pile-up materials. {yields} The real contact depth is defined as the sum of h{sub max} and the pile-up height h{sub p}. {yields} The value of residual stress measured by the nanoindentation method was in good agreement with that by the XRD method.

  18. Recent advances in small-scale mechanical property measurement by nanoindentation

    DOE PAGESBeta

    Pharr, George Mathews

    2015-08-25

    Since its initial development in the early 1980’s [1], nanoindentation has matured into one of the premier testing techniques for measuring mechanical properties at the micrometer and sub-micrometer scales and has emerged as a critical tool that has helped to shape the nanotechnology revolution. At the heart of the technique are testing systems with simple but precise force actuators and displacement measuring devices that record the force–displacement record as a diamond indenter, usually the form of a pyramid or a sphere, is pressed into and withdrawn from a small region in the surface of a material of interest. The nano-scalemore » force–displacement data, which can be obtained with a spatial resolution as small as a few nanometers, contains a wealth of information about the local mechanical properties [2], [3] and [4]. This enables the mechanical characterization of very thin films, like those used in the semiconductor, magnetic storage, and hard coatings industries, as well as very small precipitates, particles and second phases, many of which may not exist in bulk form and cannot be characterized by traditional mechanical testing methods. Here, computer automation of nanoindentation testing systems now routinely provides for complete two-dimensional mapping of properties over regions stretching from sub-micron to millimeters in scale.« less

  19. In Situ TEM Nanoindentation Studies on Stress-Induced Phase Transformations in Metallic Materials

    SciTech Connect

    Liu, Y.; Wang, H.; Zhang, X.

    2015-11-30

    Though abundant phase transformations are in general thermally driven processes, there are many examples wherein stresses can induce phase transformations. We applied numerous in situ techniques, such as in situ x-ray diffraction and neutron diffraction in order to reveal phase transformations. Recently, an in situ nanoindentation technique coupled with transmission electron microscopy demonstrated the capability to directly correlating stresses with phase transformations and microstructural evolutions at a submicron length scale. We briefly review in situ studies on stress-induced diffusional and diffusionless phase transformations in amorphous CuZrAl alloy and NiFeGa shape memory alloy. Moreover, in the amorphous CuZrAl, in situ nanoindentation studies show that the nucleation of nanocrystals (a diffusional process) occurs at ultra-low stresses manifested by a prominent stress drop. In the NiFeGa shape memory alloy, two distinctive types of martensitic (diffusionless) phase transformations accompanied by stress plateaus are observed, including a reversible gradual phase transformation at low stress levels, and an irreversible abrupt phase transition at higher stress levels.

  20. Defect Dependent Elasticity: Nanoindentation as a Probe of Stress-State

    SciTech Connect

    JARAUSCH,K.F.; KIELY,J.D.; HOUSTON,JACK E.; RUSSELL,P.E.

    2000-01-18

    Nanoindentation studies reveal that the measured elastic properties of materials can be strongly dependent upon their stress-state and defect structure. Using an interfacial force microscope (IFM), the measured elastic response of 100 nm thick Au films was found to be strongly correlated with the films' stress state and thermal history. Indentation elasticity was also found to vary in close proximity to grain boundaries in thin films and near surface steps on single crystal surfaces. Molecular dynamics simulations suggest that these results cannot be explained by elasticity due only to bond stretching. Instead, the measured elastic properties appear to be a combination of bond and defect compliance representing a composite modulus. We propose that stress concentration arising from the structure of grains, voids and grain boundaries is the source of an additional compliance which is sensitive to the stress state and thermal history of a material. The elastic properties of thin metallic films appear to reflect the collective elastic response of the grains, voids and grain boundaries. These results demonstrate that nanoindentation can be useful as a highly localized probe of stress-state and defect structures.

  1. Selection of the implant and coating materials for optimized performance by means of nanoindentation.

    PubMed

    Saber-Samandari, Saeed; Berndt, Christopher C; Gross, Karlis A

    2011-02-01

    Mechanical compatibility between a coating and a substrate is important for the longevity of implant materials. While previous studies have utilized the entire coating for analysis of mechanical compatibility of the surface, this study focuses on the nanoindentation of a uniformly thermally sprayed splat. Hydroxyapatite was thermally sprayed to create a homogeneous deposit density, as confirmed by microRaman spectroscopy, of amorphous calcium phosphate. Substrates were commercially pure Ti, Ti-6Al-4V, Co-Cr alloy and stainless steel. Nanoindentation revealed that splats deposited on the different metals have similar hardness and elastic modulus values of 4.2 ± 0.2 GPa and 80 ± 3 GPa, respectively. The mechanical properties were affected by the substrate type more than residual stresses, which were found to be low. It is recommended that amorphous calcium phosphate is annealed to relieve the quenching stress or that appropriate temperature histories are chosen to relax the stress created in cooling the coating assembly. PMID:20883836

  2. Depth-sensing nano-indentation on a myelinated axon at various stages

    NASA Astrophysics Data System (ADS)

    Huang, Wei-Chin; Liao, Jiunn-Der; Lin, Chou-Ching K.; Ju, Ming-Shaung

    2011-07-01

    A nano-mechanical characterization of a multi-layered myelin sheath structure, which enfolds an axon and plays a critical role in the transmission of nerve impulses, is conducted. Schwann cells co-cultured in vitro with PC12 cells for various co-culture times are differentiated to form a myelinated axon, which is then observed using a transmission electron microscope. Three major myelination stages, with distinct structural characteristics and thicknesses around the axon, can be produced by varying the co-culture time. A dynamic contact module and continuous depth-sensing nano-indentation are used on the myelinated structure to obtain the load-on-sample versus measured displacement curve of a multi-layered myelin sheath, which is used to determine the work required for the nano-indentation tip to penetrate the myelin sheath. By analyzing the harmonic contact stiffness versus the measured displacement profile, the results can be used to estimate the three stages of the multi-layered structure on a myelinated axon. The method can also be used to evaluate the development stages of myelination or demyelination during nerve regeneration.

  3. The influence of sputtering procedure on nanoindentation and nanoscratch behaviour of W-S-C film

    NASA Astrophysics Data System (ADS)

    Roy, Manish; Koch, T.; Pauschitz, A.

    2010-09-01

    Sulphides of tungsten with its lamellar structure - whereby weak van der Waals forces act between the layers - are commonly believed to be responsible for their excellent self-lubricating properties. The present investigation is undertaken in order to explore the possibility of using this film for MEMS application. In order to achieve this objective, W-S-C films are deposited on 100Cr6 steel using radio frequency magnetron sputtering. Carbon was incorporated in the films via three different ways: (1) using a reactive gas (CH 4), (2) by co-sputtering from separate targets (WS 2 and C targets) and, (3) by co-sputtering from a C target embedded with WS 2 pellets. Microstructural features and mechanical properties of these films are evaluated with the help of scanning electron microscopy and nanoindentation. The topography, structural features and scratch behaviour are analysed using atomic force microscopy, X-ray diffraction and nanoindenter. It is noted that the film deposited by sputtering two targets exhibits the highest hardness due to high oxygen content. The highest elastic modulus pertains to the film deposited from the carbon target containing WS 2 pellets as this film has amorphous structure and the minimum porosity. The friction coefficient under scratching is the highest for reactively sputtered film whereas it is the minimum for the film deposited from the carbon target containing WS 2 pellets as this film has amorphous structure and the minimum roughness.

  4. Nanoindentation of plasma-deposited nitrogen-rich silicon nitride thin films

    NASA Astrophysics Data System (ADS)

    Soh, Martin T. K.; Fischer-Cripps, A. C.; Savvides, N.; Musca, C. A.; Faraone, L.

    2006-07-01

    Nanoindentation was performed on plasma-deposited nitrogen-rich silicon nitride thin films deposited on various substrates between 150 and 300°C. A very simple and effective depth-profiling method is introduced, which involves indentation of thin films deposited on substrates with different mechanical properties. The primary advantage of this method is that it avoids the complications associated with many of the complex mathematical models available to deconvolve thin film mechanical properties, while nevertheless allowing the user to visually identify thin film properties. This method is demonstrated on our thin films, which have a hardness between 14 and 21GPa, and reduced modulus between 120 and 160GPa. The initial rise in hardness at low contact depths, commonly attributed to an indentation-size effect, is shown to be due to elastic contact between the indenter and thin film surface. This demonstrates the perils of blindly following the 10% rule for hardness calculation. The contribution of elastic and plastic deformations from nanoindentation is used to clarify the physical meaning of hardness and reduced modulus.

  5. Characterization of mineral-associated organic matter: a combined approach of AFM and NanoSIMS

    NASA Astrophysics Data System (ADS)

    Pohl, Lydia; Schurig, Christian; Eusterhues, Karin; Mueller, Carsten W.; Höschen, Carmen; Totsche, Kai-Uwe; Kögel-Knabner, Ingrid

    2016-04-01

    The heterogeneous spatial distribution and amount of organic matter (OM) in soils, especially at the micro- or submicron-scale, has major consequences for the soil microstructure and for the accessibility of OM to decomposing microbial communities. Processes occurring at the microscale control soil properties and processes at larger scales, such as macro-aggregation and carbon turnover. Since OM acts as substrate and most important driver for biogeochemical processes, particular attention should be paid to its spatial interaction with soil minerals. In contrast to bulk analysis, Nanoscale Secondary Ion Mass Spectrometry (NanoSIMS) offers the possibility to examine the composition and spatial distribution of OM within the intact organo-mineral matrix. Nevertheless, the yield of secondary electrons is influenced by the individual topography of the analysed particles, which aggravated the quantitative interpretation of the data. A combination of NanoSIMS and Atomic Force Microscopy (AFM), enabled us to visualize and quantify the topographical features of individual particles and correct the NanoSIMS data for this effect. We performed adsorption experiments with water-soluble soil OM in 6 concentration steps, which was extracted from forest floor layer of a Podzol, and adsorbed to illite. Upon the end of the sorption experiments the liquid phase and the solid phase were separated and the carbon content was analysed with TOC- and C/N-measurement, respectively. For the spatially resolved analyses, the samples were applied as thin layers onto silicon wafers and individual particles were chosen by means of the AFM. Subsequently, the identical particles were analysed with NanoSIMS to investigate the distribution of C, N, O, Si, P and Al. The recorded data were analysed for differences in elemental distribution between the different concentration steps. Additionally, we performed a correlation of the detectable counts with the topography of the particle within one

  6. NC-AFM identification of different aluminum atoms on Al2O3/NiAl(110) surface

    NASA Astrophysics Data System (ADS)

    Stich, Ivan; Brndiar, Jan; Li, Yan Jun; Sugawara, Yasuhiro

    2015-03-01

    Ultrathin alumina film formed by oxidation of NiAl(110) is widely used as a system for technologically important oxide-supported catalysts. Using small amplitude NC-AFM we have obtained images of this system with unprecedented resolution, significantly surpassing the previous STM and NC-AFM images. In particular, we are able to resolve aluminum atoms with different coordination, such as five-, and four-fold coordinated Al atoms. Experiments are supported by extensive density functional theory modeling. Starting from the previous atomic model, we have been able to describe the gross image features such as the dark oxygen sites. We find that the system is strongly ionic with the oxygen sites strongly negatively charged and aluminum sites positively charged. Hence, the NC-AFM images can reliably be understood from electrostatic potentials. These finding also suggest an oxygen terminated apex. Resolving finer contrast features of the differently coordinated Al atoms required construction of better and more realistic approximants to the ultra-thin incommensurable alumina interface. Supported by APVV-0207-11 and VEGA (2/0007/12) projects.

  7. AFM surface investigation of polyethylene modified by ion bombardment

    NASA Astrophysics Data System (ADS)

    Švorčík, V.; Arenholz, E.; Hnatowicz, V.; Rybka, V.; Öchsner, R.; Ryssel, H.

    1998-07-01

    Polyethylene (PE) was irradiated with 63 keV Ar + and 155 keV Xe + ions to fluences of 1 × 10 13 to 3 × 10 15 cm -2 with ion energies being chosen in order to achieve approximately the same penetration depth for both species. The PE surface morphology was examined by means of atomic force microscopy (AFM), whereas the concentration of free radicals and conjugated double bonds, both created by the ion irradiation, were determined using electron paramagnetic resonance (EPR) and UV-VIS spectroscopy, respectively. As expected, the degradation of PE was higher after irradiation with heavier Xe + ions but the changes in the PE surface morphology were more pronounced for Ar + ions. This newly observed effect can be explained by stronger compaction of the PE surface layer in the case of the Xe + irradiation, connected with a reduction of free volume available.

  8. FM-AFM crossover in vanadium oxide nanomaterials

    NASA Astrophysics Data System (ADS)

    Demishev, S. V.; Chernobrovkin, A. L.; Glushkov, V. V.; Grigorieva, A. V.; Goodilin, E. A.; Sluchanko, N. E.; Samarin, N. A.; Semeno, A. V.

    2010-01-01

    The magnetic properties of nanomaterials based on vanadium oxide (multiwall nanotubes, nanorods, and nanolayers) have been investigated in the temperature range of 1.8-220 K by high-frequency (60-GHz) EPR. A transition from a ferromagnetic temperature dependence to an antiferromagnetic temperature dependence has been observed in nanorods and nanotubes with a decrease in the temperature. The FM-AFM crossover observed near T C ˜ 110 K is accompanied by a low-temperature increase in the Curie constant by a factor of 2.7-7. The comparison of the experimental data for various VO x nanoparticles indicates that the most probable cause of the change in the type of magnetic interaction is a change in the concentration of V4+ magnetic ions.

  9. Adhesion forces between AFM tips and superficial dentin surfaces.

    PubMed

    Pelin, I M; Piednoir, A; Machon, D; Farge, P; Pirat, C; Ramos, S M M

    2012-06-15

    In this work, we study the adhesion forces between atomic force microscopy (AFM) tips and superficial dentin etched with phosphoric acid. Initially, we quantitatively analyze the effect of acid etching on the surface heterogeneity and the surface roughness, two parameters that play a key role in the adhesion phenomenon. From a statistical study of the force-distance curves, we determine the average adhesion forces on the processed substrates. Our results show that the average adhesion forces, measured in water, increase linearly with the acid exposure time. The highest values of such forces are ascribed to the high density of collagen fibers on the etched surfaces. The individual contribution of exposed collagen fibrils to the adhesion force is highlighted. We also discuss in this paper the influence of the environmental medium (water/air) in the adhesion measurements. We show that the weak forces involved require working in the aqueous medium. PMID:22472512

  10. BOREAS AFM-04 Twin Otter Aircraft Sounding Data

    NASA Technical Reports Server (NTRS)

    MacPherson, J. Ian; Desjardins, Raymond L.; Hall, Forrest G. (Editor); Knapp, David E. (Editor); Smith, David E. (Technical Monitor)

    2000-01-01

    The Boreal Ecosystem-Atmosphere Study (BOREAS) Airborne Fluxes and Meteorology (AFM)-4 team used the National Research Council, Canada (NRC) Twin Otter aircraft to make sounding measurements through the boundary layer. These measurements included concentrations of carbon dioxide and ozone, atmospheric pressure, dry bulb temperature, potential temperature, dewpoint temperature, calculated mixing ratio, and wind speed and direction. Aircraft position, heading, and altitude were also recorded. Data were collected at both the Northern Study Area (NSA) and the Southern Study Area (SSA) in 1994 and 1996. These data are stored in tabular ASCII files. The Twin Otter aircraft sounding data are available from the Earth Observing System Data and Information System (EOSDIS) Oak Ridge National Laboratory (ORNL) Distributed Active Archive Center (DAAC). The data files also are available on a CD-ROM (see document number 20010000884).

  11. Visualization of internal structure of banana starch granule through AFM.

    PubMed

    Peroni-Okita, Fernanda H G; Gunning, A Patrick; Kirby, Andrew; Simão, Renata A; Soares, Claudinéia A; Cordenunsi, Beatriz R

    2015-09-01

    Atomic force microscopy (AFM) is a high resolution technique for studying the external and internal structures of starch granules. For this purpose granules were isolated from bananas and embedded in a non-penetrating resin. To achieve image contrast of the ultrastructure, the face of the cut blocks were wetted in steam and force modulation mode imaging was used. Images of starch from green bananas showed large variation of height across the granule due to a locational specific absorption of water and swelling of amorphous regions; the data reveal that the center of the granules are structurally different and have different viscoelastic properties. Images of starches from ripe bananas showed an even greater different level of organization: absence of growth rings around the hilum; the central region of the granule is richer in amylose; very porous surface with round shaped dark structures; the size of blocklets are larger than the green fruits. PMID:26005137

  12. AFM of self-assembled lambda DNA-histone networks.

    PubMed

    Liu, YuYing; Guthold, Martin; Snyder, Matthew J; Lu, HongFeng

    2015-10-01

    Atomic force microscopy (AFM) was used to investigate the self-assembly behavior of λ-DNA and histones at varying histone:DNA ratios. Without histones and at the lowest histone:DNA ratio (less than one histone per 1000 base pairs of DNA), the DNA appeared as individual (uncomplexed), double-stranded DNA molecules. At increasing histone concentrations (one histone per 500, 250 and 167 base pairs of DNA), the DNA molecules started to form extensive polygonal networks of mostly pentagons and hexagons. The observed networks might be one of the naturally occurring, stable DNA-histone structures. The condensing effects of the divalent cations Mg(2+) and Ca(2+) on the DNA-histone complexes were also investigated. The networks persisted at high Mg(2+) concentration (20mM) and the highest histone concentration. At high Ca(2+) concentration and the highest histone concentration, the polygonal network disappeared and, instead, individual, tightly condensed aggregates were formed. PMID:26141439

  13. Recent advances in exchange bias of layered magnetic FM/AFM systems

    NASA Astrophysics Data System (ADS)

    Liu, ZhongYuan

    2013-01-01

    The exchange bias (EB) has been investigated in magnetic materials with the ferromagnetic (FM)/antiferromagnetic (AFM) contacting interfaces for more than half a century. To date, the significant progress has been made in the layered magnetic FM/AFM thin film systems. EB mechanisms have shown substantive research advances. Here some of the new advances are introduced and discussed with the emphasis on the influence of AFM layer, the interlayer EB coupling across nonmagnetic spacer, and the interlayer coupling across AFM layer, as well as EB related to multiferrioc materials and electrical control.

  14. Evaluation of critical depth ratio for soft V2O5 film on hard Si substrate by finite element modeling of experimentally measured nanoindentation response

    NASA Astrophysics Data System (ADS)

    Gupta, A. K.; Porwal, Deeksha; Dey, Arjun; Mukhopadhyay, Anoop Kumar; Sharma, Anand Kumar

    2016-04-01

    A combined nanoindentation experiment and finite element modeling (FEM) approach was utilized in the present work to evaluate the effects of variations in the ratio (h/t) of indentation depth (h) to film thickness (t) on the nanomechanical behavior of 2.3-6.2 μm vanadium pentoxide (V2O5) films. The soft V2O5 films were deposited by pulsed radio frequency magnetron sputtering on a relatively hard silicon (Si) substrate. The elasto-plastic properties of the V2O5 films as well as the Si substrate were evaluated using a power law-based nonlinear material model. Based on the present nanoindentation and FEM results the critical penetration depth to film thickness ratio (h /t)c, i.e. critical depth ratio (CDR) was predicted as 7.9%,,confirming thereby that there is no universal critical penetration depth beyond which the mechanical properties of the substrate start to affect the evaluated nanomechanical properties (e.g. nanohardness H, Young’s modulus E, etc) of a given soft film on a given hard substrate. The experimental data showed that at h ~ 0.5t the magnitudes of E and H were approximately two times the values measured at h  ⩽  0.1t. The FEM results obtained in the present work successfully predicted the effects of variations in the h /t ratio on the indenter displacements as well as the distributions of the von Mises stress for the soft V2O5 films on the hard Si substrate system.

  15. Strain rate sensitivity of nanoindentation creep in an AlCoCrFeNi high-entropy alloy

    NASA Astrophysics Data System (ADS)

    Jiao, Z. M.; Wang, Z. H.; Wu, R. F.; Qiao, J. W.

    2016-09-01

    Creep behaviors of an AlCoCrFeNi high-entropy alloy with the body-centered cubic structure were investigated by nanoindentation. The enhanced strain gradient induced by higher strain rate leads to decreased strain rate sensitivity during creep process. The present alloy exhibits excellent creep resistance, mainly due to its large entropy of mixing and highly distorted lattice structure.

  16. Measurement of ultra thin film fracture toughness by nano-indentation: A numerical study

    NASA Astrophysics Data System (ADS)

    Burke, Benjamin

    As the individual layers of interconnect structures decrease in size, it becomes increasingly difficult to determine the fracture toughness, and hence the reliability, of these layers. After a layer is thinner than ˜500nm, it becomes difficult to determine the fracture toughness directly with traditional methods. Using nano-indentation, it is possible to extract the cohesive and adhesive fracture energies of these films without elaborate experimental setups. There are, however, several issues with this approach. Nano-indentation creates cracks both within the film (the cohesive cracks) and between the film and the substrate (the adhesive cracks) as well as significant plastic deformation of the film and substrate. Using SIMULA Abaqus Standard, a commercial finite element analysis tool, 2D and 3D models were created to examine the deformation characteristics associated with the nano-indentation process. The models either have pre-existing stationary cracks, or simulated by cohesive zone surfaces to account for crack nucleation and growth. The 2D model is axi-symmetric and only accounts for the adhesive crack. It is used primarily as a test the cohesive zone model and to begin to determine experimental testing limits. The 3D model is a one sixth slice of the area indented. Both cohesive and adhesive cracks are modeled and the interaction between the two cracks is investigated. While there are many parameters controlling the crack initiation and propagation process, several trends were identified. The domain of practical testing should be between one and three film thickness, so as to avoid the confluence of the indenter plastic process zone on the propagating crack front. When excursion on the load-indentation depth happens, the fracture energy is about 20% of the associated work done by the indenter (or the area under the excursion segment). The FEM simulation showed the general role of film thickness, toughness and modulus on the initiation and propagation of both

  17. Structure and Dynamics of Four-way DNA Junctions Dynamics Revealed by Single-Molecule AFM

    NASA Astrophysics Data System (ADS)

    Lyubchenko, Yuri

    2004-03-01

    For-way DNA junctions (Holliday junctions) are critical intermediates for homologous, site-specific recombination, DNA repair and replication. A wealth of structural information is available for immobile four-way junctions. However, these data cannot give the answer on the mechanism of branch migration, the major property of the Holliday junction. Two models for the mechanism of branch migration were suggested. According to the early model of Alberts-Meselson-Sigal, exchanging DNA strands around the junction remain parallel during branch migration. Kinetic studies of branch migration suggest an alternative model in which the junction adopts an extended conformation. We tested these models using a Holliday junction undergoing branch migration. Note that it was the first time when the dynamics of the four-way DNA junction capable of branch migration had been analyzed. We applied time-lapse atomic force microscopy (single molecule dynamics AFM) to image directly loosely bound DNA at liquid-surface interface. These experiments show that mobile Holliday junctions adopt an unfolded conformation during branch migration. This conformation of the junction remains unchanged until strand separation. The data obtained support the model for branch migration having the extended conformation of the Holliday junction. The analysis of the Holliday junctions dynamics at conditions limiting branch migration revealed a broad movement of the arms suggesting that the range of mobility of these junctions is much wider than detected before. Further applications of the time-lapse AFM approach in attempt to resolve the subpopulations of the junctions conformers and the prospects for analyses of dynamics of complex biological systems will be discussed.

  18. Probing of miniPEGγ-PNA-DNA Hybrid Duplex Stability with AFM Force Spectroscopy

    PubMed Central

    Dutta, Samrat; Armitage, Bruce A.; Lyubchenko, Yuri L.

    2016-01-01

    Peptide nucleic acids (PNA) are synthetic polymers, the neutral peptide backbone of which provides elevated stability to PNA-PNA and PNA-DNA hybrid duplex. It was demonstrated that incorporation of diethylene glycol (miniPEG) at the γ position of the peptide backbone increased the thermal stability of the hybrid duplexes (Sahu, B. et al. (2011) Journal of Organic Chemistry 76, 5614-5627). Here, we applied atomic force microscopy (AFM) based single molecule force spectroscopy (SMFS) and dynamic force spectroscopy (DFS) to test the strength and stability of the hybrid 10 bp duplex. This hybrid duplex consisted of miniPEGγ-PNA and DNA of the same length (γMPPNA-DNA), which we compared to a DNA duplex with a homologous sequence. AFM force spectroscopy data obtained at the same conditions showed that γMPPNA-DNA hybrid is more stable than the DNA counterpart, 65 ± 15 pN vs 47 ± 15 pN, respectively. The DFS measurements performed in a range of pulling speeds analyzed in the framework of the Bell-Evans approach yielded a dissociation constant, koff ∼ 0.030 ± 0.01 sec-1 for γMPPNA-DNA hybrid duplex vs. 0.375 ± 0.18 sec-1 for the DNA-DNA duplex suggesting that the hybrid duplex is much more stable. Correlating the high affinity of γMPPNA-DNA to slow dissociation kinetics is consistent with prior bulk characterization by surface plasmon resonance. Given the growing interest in γMPPNA as well as other synthetic DNA analogues, the use of single molecule experiments along with computational analysis of force spectroscopy data will provide direct characterization of various modifications as well as higher order structures such as triplexes and quadruplexes. PMID:26898903

  19. Oscillatory structural forces due to nonionic surfactant micelles: data by colloidal-probe AFM vs theory.

    PubMed

    Christov, Nikolay C; Danov, Krassimir D; Zeng, Yan; Kralchevsky, Peter A; von Klitzing, Regine

    2010-01-19

    Micellar solutions of nonionic surfactants Brij 35 and Tween 20 are confined between two surfaces in a colloidal-probe atomic-force microscope (CP-AFM). The experimentally detected oscillatory forces due to the layer-by-layer expulsion of the micelles agree very well with the theoretical predictions for hard-sphere fluids. While the experiment gives parts of the stable branches of the force curve, the theoretical model allows reconstruction of the full oscillatory curve. Therewith, the strength and range of the ordering could be determined. The resulting aggregation number from the fits of the force curves for Brij 35 is close to 70 and exhibits a slight tendency to increase with the surfactant concentration. The last layer of micelles cannot be pressed out. The measured force-vs-distance curve has nonequilibrium portions, which represent "jumps" from one to another branch of the respective equilibrium oscillatory curve. In the case of Brij 35, at concentrations <150 mM spherical micelles are present and the oscillation period is close to the micelle diameter, slightly decreasing with the rise of concentration. For elongated micelles (at concentration 200 mM), no harmonic oscillations are observed anymore; instead, the period increases with the decrease of film thickness. In the case of Tween 20, the force oscillations are almost suppressed, which implies that the micelles of this surfactant are labile and are demolished by the hydrodynamic shear stresses due to the colloidal-probe motion. The comparison of the results for the two surfactants demonstrates that in some cases the micelles can be destroyed by the CP-AFM, but in other cases they can be stable and behave as rigid particles. This behavior correlates with the characteristic times of the slow micellar relaxation process for these surfactants. PMID:20067306

  20. Probing of miniPEGγ-PNA-DNA Hybrid Duplex Stability with AFM Force Spectroscopy.

    PubMed

    Dutta, Samrat; Armitage, Bruce A; Lyubchenko, Yuri L

    2016-03-15

    Peptide nucleic acids (PNA) are synthetic polymers, the neutral peptide backbone of which provides elevated stability to PNA-PNA and PNA-DNA hybrid duplexes. It was demonstrated that incorporation of diethylene glycol (miniPEG) at the γ position of the peptide backbone increased the thermal stability of the hybrid duplexes (Sahu, B. et al. J. Org. Chem. 2011, 76, 5614-5627). Here, we applied atomic force microscopy (AFM) based single molecule force spectroscopy and dynamic force spectroscopy (DFS) to test the strength and stability of the hybrid 10 bp duplex. This hybrid duplex consisted of miniPEGγ-PNA and DNA of the same length (γ(MP)PNA-DNA), which we compared to a DNA duplex with a homologous sequence. AFM force spectroscopy data obtained at the same conditions showed that the γ(MP)PNA-DNA hybrid is more stable than the DNA counterpart, 65 ± 15 pN vs 47 ± 15 pN, respectively. The DFS measurements performed in a range of pulling speeds analyzed in the framework of the Bell-Evans approach yielded a dissociation constant, koff ≈ 0.030 ± 0.01 s⁻¹ for γ(MP)PNA-DNA hybrid duplex vs 0.375 ± 0.18 s⁻¹ for the DNA-DNA duplex suggesting that the hybrid duplex is much more stable. Correlating the high affinity of γ(MP)PNA-DNA to slow dissociation kinetics is consistent with prior bulk characterization by surface plasmon resonance. Given the growing interest in γ(MP)PNA as well as other synthetic DNA analogues, the use of single molecule experiments along with computational analysis of force spectroscopy data will provide direct characterization of various modifications as well as higher order structures such as triplexes and quadruplexes. PMID:26898903

  1. BOREAS AFM-12 1-km AVHRR Seasonal Land Cover Classification

    NASA Technical Reports Server (NTRS)

    Steyaert, Lou; Hall, Forrest G.; Newcomer, Jeffrey A. (Editor); Knapp, David E. (Editor); Loveland, Thomas R.; Smith, David E. (Technical Monitor)

    2000-01-01

    The Boreal Ecosystem-Atmosphere Study (BOREAS) Airborne Fluxes and Meteorology (AFM)-12 team's efforts focused on regional scale Surface Vegetation and Atmosphere (SVAT) modeling to improve parameterization of the heterogeneous BOREAS landscape for use in larger scale Global Circulation Models (GCMs). This regional land cover data set was developed as part of a multitemporal one-kilometer Advanced Very High Resolution Radiometer (AVHRR) land cover analysis approach that was used as the basis for regional land cover mapping, fire disturbance-regeneration, and multiresolution land cover scaling studies in the boreal forest ecosystem of central Canada. This land cover classification was derived by using regional field observations from ground and low-level aircraft transits to analyze spectral-temporal clusters that were derived from an unsupervised cluster analysis of monthly Normalized Difference Vegetation Index (NDVI) image composites (April-September 1992). This regional data set was developed for use by BOREAS investigators, especially those involved in simulation modeling, remote sensing algorithm development, and aircraft flux studies. Based on regional field data verification, this multitemporal one-kilometer AVHRR land cover mapping approach was effective in characterizing the biome-level land cover structure, embedded spatially heterogeneous landscape patterns, and other types of key land cover information of interest to BOREAS modelers.The land cover mosaics in this classification include: (1) wet conifer mosaic (low, medium, and high tree stand density), (2) mixed coniferous-deciduous forest (80% coniferous, codominant, and 80% deciduous), (3) recent visible bum, vegetation regeneration, or rock outcrops-bare ground-sparsely vegetated slow regeneration bum (four classes), (4) open water and grassland marshes, and (5) general agricultural land use/ grasslands (three classes). This land cover mapping approach did not detect small subpixel-scale landscape

  2. Nano-Wilhelmy investigation of dynamic wetting properties of AFM tips through tip-nanobubble interaction.

    PubMed

    Wang, Yuliang; Wang, Huimin; Bi, Shusheng; Guo, Bin

    2016-01-01

    The dynamic wetting properties of atomic force microscopy (AFM) tips are of much concern in many AFM-related measurement, fabrication, and manipulation applications. In this study, the wetting properties of silicon and silicon nitride AFM tips are investigated through dynamic contact angle measurement using a nano-Wilhelmy balance based method. This is done by capillary force measurement during extension and retraction motion of AFM tips relative to interfacial nanobubbles. The working principle of the proposed method and mathematic models for dynamic contact angle measurement are presented. Geometric models of AFM tips were constructed using scanning electronic microscopy (SEM) images taken from different view directions. The detailed process of tip-nanobubble interaction was investigated using force-distance curves of AFM on nanobubbles. Several parameters including nanobubble height, adhesion and capillary force between tip and nanobubbles are extracted. The variation of these parameters was studied over nanobubble surfaces. The dynamic contact angles of the AFM tips were calculated from the capillary force measurements. The proposed method provides direct measurement of dynamic contact angles for AFM tips and can also be taken as a general approach for nanoscale dynamic wetting property investigation. PMID:27452115

  3. Nano-Wilhelmy investigation of dynamic wetting properties of AFM tips through tip-nanobubble interaction

    PubMed Central

    Wang, Yuliang; Wang, Huimin; Bi, Shusheng; Guo, Bin

    2016-01-01

    The dynamic wetting properties of atomic force microscopy (AFM) tips are of much concern in many AFM-related measurement, fabrication, and manipulation applications. In this study, the wetting properties of silicon and silicon nitride AFM tips are investigated through dynamic contact angle measurement using a nano-Wilhelmy balance based method. This is done by capillary force measurement during extension and retraction motion of AFM tips relative to interfacial nanobubbles. The working principle of the proposed method and mathematic models for dynamic contact angle measurement are presented. Geometric models of AFM tips were constructed using scanning electronic microscopy (SEM) images taken from different view directions. The detailed process of tip-nanobubble interaction was investigated using force-distance curves of AFM on nanobubbles. Several parameters including nanobubble height, adhesion and capillary force between tip and nanobubbles are extracted. The variation of these parameters was studied over nanobubble surfaces. The dynamic contact angles of the AFM tips were calculated from the capillary force measurements. The proposed method provides direct measurement of dynamic contact angles for AFM tips and can also be taken as a general approach for nanoscale dynamic wetting property investigation. PMID:27452115

  4. Beyond topography - enhanced imaging of cometary dust with the MIDAS AFM

    NASA Astrophysics Data System (ADS)

    Bentley, M. S.; Torkar, K.; Jeszenszky, H.; Romstedt, J.

    2013-09-01

    The MIDAS atomic force microscope (AFM) onboard the Rosetta spacecraft is primarily designed to return the 3D shape and structure of cometary dust particles collected at comet 67P/Churyumov-Gerasimenko [1]. Commercial AFMs have, however, been further developed to measure many other sample properties. The possibilities to make such measurements with MIDAS are explored here.

  5. Nano-Wilhelmy investigation of dynamic wetting properties of AFM tips through tip-nanobubble interaction

    NASA Astrophysics Data System (ADS)

    Wang, Yuliang; Wang, Huimin; Bi, Shusheng; Guo, Bin

    2016-07-01

    The dynamic wetting properties of atomic force microscopy (AFM) tips are of much concern in many AFM-related measurement, fabrication, and manipulation applications. In this study, the wetting properties of silicon and silicon nitride AFM tips are investigated through dynamic contact angle measurement using a nano-Wilhelmy balance based method. This is done by capillary force measurement during extension and retraction motion of AFM tips relative to interfacial nanobubbles. The working principle of the proposed method and mathematic models for dynamic contact angle measurement are presented. Geometric models of AFM tips were constructed using scanning electronic microscopy (SEM) images taken from different view directions. The detailed process of tip-nanobubble interaction was investigated using force-distance curves of AFM on nanobubbles. Several parameters including nanobubble height, adhesion and capillary force between tip and nanobubbles are extracted. The variation of these parameters was studied over nanobubble surfaces. The dynamic contact angles of the AFM tips were calculated from the capillary force measurements. The proposed method provides direct measurement of dynamic contact angles for AFM tips and can also be taken as a general approach for nanoscale dynamic wetting property investigation.

  6. Mechano-rheological properties of the murine thrombus determined via nanoindentation and finite element modeling.

    PubMed

    Slaboch, Constance L; Alber, Mark S; Rosen, Elliot D; Ovaert, Timothy C

    2012-06-01

    Deep vein thrombosis, pulmonary embolism, and abdominal aortic aneurysms are blood-related diseases that represent a major public health problem. These diseases are characterized by the formation of a thrombus (i.e., blood clot) that either blocks a major artery or causes an aortic rupture. Identifying the mechanical properties of thrombi can help determine when these incidents will occur. In this investigation, a murine thrombus, formed from platelet-rich plasma, calcium, and thrombin, was nanoindented and the elastic modulus was estimated via elastic contact theory. This information was used as input to an inverse finite element simulation, which determined optimal values for the elastic modulus and viscosity of the thrombus using a viscoelastic material model. A sensitivity analysis was also performed to determine which material parameters have the greatest affect on the simulation. Results from this investigation demonstrate the feasibility of the mechanical characterization of a murine thrombus using nanoindentation. PMID:22520420

  7. In situ nanoindentation study on plasticity and work hardening in aluminium with incoherent twin boundaries

    NASA Astrophysics Data System (ADS)

    Bufford, D.; Liu, Y.; Wang, J.; Wang, H.; Zhang, X.

    2014-09-01

    Nanotwinned metals have been the focus of intense research recently, as twin boundaries may greatly enhance mechanical strength, while maintaining good ductility, electrical conductivity and thermal stability. Most prior studies have focused on low stacking-fault energy nanotwinned metals with coherent twin boundaries. In contrast, the plasticity of twinned high stacking-fault energy metals, such as aluminium with incoherent twin boundaries, has not been investigated. Here we report high work hardening capacity and plasticity in highly twinned aluminium containing abundant Σ3{112} incoherent twin boundaries based on in situ nanoindentation studies in a transmission electron microscope and corresponding molecular dynamics simulations. The simulations also reveal drastic differences in deformation mechanisms between nanotwinned copper and twinned aluminium ascribed to stacking-fault energy controlled dislocation-incoherent twin boundary interactions. This study provides new insight into incoherent twin boundary-dominated plasticity in high stacking-fault energy twinned metals.

  8. Effects of sequential tungsten and helium ion implantation on nano-indentation hardness of tungsten

    SciTech Connect

    Armstrong, D. E. J.; Edmondson, P. D.; Roberts, S. G.

    2013-06-24

    To simulate neutron and helium damage in a fusion reactor first wall sequential self-ion implantation up to 13 dpa followed by helium-ion implantation up to 3000 appm was performed to produce damaged layers of {approx}2 {mu}m depth in pure tungsten. The hardness of these layers was measured using nanoindentation and was studied using transmission electron microscopy. Substantial hardness increases were seen in helium implanted regions, with smaller hardness increases in regions which had already been self-ion implanted, thus, containing pre-existing dislocation loops. This suggests that, for the same helium content, helium trapped in distributed vacancies gives stronger hardening than helium trapped in vacancies condensed into dislocation loops.

  9. Nanoindentation response of a single micrometer-sized GaAs wall

    NASA Astrophysics Data System (ADS)

    Le Bourhis, E.; Patriarche, G.

    2005-04-01

    Wall-patterned GaAs surfaces have been elaborated by photolithography and dry etching. The mechanical response of individual μm-sized walls was tested at different positions on the wall by nanoindentation. Overall results show that contact stiffness remains constant across the wall while total penetration drastically increases at the proximity of the free sides of the wall. Transmission electron microscopy was used to get further insight into the plastic deformation of the walls and reveals that the central-plastic zone governs the mechanical response instead of the rosette arms. The application of substrate patterning with enhanced plastic compliance is suggested in order to eliminate residual dislocations appearing in mismatched structures grown for optoelectronic devices.

  10. In Situ Nanoindentation Studies on Detwinning and Work Hardening in Nanotwinned Monolithic Metals

    DOE PAGESBeta

    Liu, Y.; Li, N.; Bufford, D.; Lee, J. H.; Wang, J.; Wang, H.; Zhang, X.

    2015-07-14

    Certain nanotwinned (nt) metals have rare combinations of high mechanical strength and ductility. Here, we review recent in situ nanoindentation studies (using transmission electron microscopes) on the deformation mechanisms of nt face-centered cubic metals including Cu, Ni, and Al with a wide range of stacking fault energy (SFE). Moreover, in nt Cu with low-to-intermediate SFE, detwinning (accompanied by rapid twin boundary migration) occurs at ultralow stress. In Ni with relatively high SFE, coherent {111} twin boundaries lead to substantial work hardening. Twinned Al has abundant {112} incoherent twin boundaries, which induce significant work-hardening capability and plasticity in Al. Finally, twinmore » boundaries in Al also migrate but at very high stresses. Furthermore, molecular dynamics simulations reveal the influence of SFE on deformation mechanisms in twinned metals.« less

  11. Nanoindentation study of irradiation and temperature effects in yttria-stabilized zirconia

    NASA Astrophysics Data System (ADS)

    Kurpaska, L.; Jagielski, J.; Nowakowska-Langier, K.

    2016-07-01

    In the present study, the detailed evaluation of nanomechanical properties in terms of hardness and Young's modulus of irradiated polycrystalline YSZ pellets were studied using the nanoindentation technique. The samples were irradiated at room temperature with 150 keV Ar-ions to a fluences of 1 × 1014 and 1 × 1015 ions/cm2 (i.e. before bubble formation), which correspond to a peak damage of 0.12 and 1.2 dpa respectively. Substantial improvement of mechanical properties related to the creation of both radiation defects and residual stress in the implanted surface layer were observed. Additionally, in-situ high temperature nanomechanical investigation of pristine YSZ pellet was conducted. A significant decrease of nanomechanical properties was observed with increasing temperature.

  12. Investigation of the Anisotropic Mechanical Behaviors of Copper Single Crystals Through Nanoindentation Modeling

    NASA Astrophysics Data System (ADS)

    Liu, Mao; Tieu, Kiet Anh; Zhou, Kun; Peng, Ching-Tun

    2016-03-01

    A crystal plasticity finite element method constitutive model was developed to investigate the anisotropic mechanical behaviors of (001), (011), and (111) initially orientated copper (Cu) single crystals during nanoindentation deformation. The numerical load-indentation depth curve and hardness-indentation depth curve were compared with experimental observations to validate the established three-dimensional (3D) CPFEM model. The difference of indentation loads between (111) crystal and (001) crystal is ~10.68 pct, and the difference of indentation modulus between (111) surface and (001) surface is ~10.80 pct. The numerical results show the noticeable indentation size effect for three crystals, and slightly different hardness values on different crystallographic planes. The equivalent plastic strain and lattice rotation angles were also analyzed on three through-thickness cross sections to study the plastic deformation-induced texture anisotropy.

  13. In Situ Nanoindentation Studies on Detwinning and Work Hardening in Nanotwinned Monolithic Metals

    NASA Astrophysics Data System (ADS)

    Liu, Y.; Li, N.; Bufford, D.; Lee, J. H.; Wang, J.; Wang, H.; Zhang, X.

    2016-01-01

    Certain nanotwinned (nt) metals have rare combinations of high mechanical strength and ductility. In this article, we review recent in situ nanoindentation studies (using transmission electron microscopes) on the deformation mechanisms of nt face-centered cubic metals including Cu, Ni, and Al with a wide range of stacking fault energy (SFE). In nt Cu with low-to-intermediate SFE, detwinning (accompanied by rapid twin boundary migration) occurs at ultralow stress. In Ni with relatively high SFE, coherent {111} twin boundaries lead to substantial work hardening. Twinned Al has abundant {112} incoherent twin boundaries, which induce significant work-hardening capability and plasticity in Al. Twin boundaries in Al also migrate but at very high stresses. Furthermore, molecular dynamics simulations reveal the influence of SFE on deformation mechanisms in twinned metals.

  14. Nanoindentation of hcp metals: a comparative simulation study of the evolution of dislocation networks.

    PubMed

    Alhafez, Iyad Alabd; Ruestes, Carlos J; Gao, Yu; Urbassek, Herbert M

    2016-01-29

    Using molecular dynamics simulation, we study the nanoindentation of three hcp metals: Mg, Ti, and Zr. Both the basal and two prismatic surface planes are considered. We focus on the characterization of the plasticity generated in the crystal. The similarities to, and the differences from, the behavior of the more commonly investigated fcc and bcc metals are highlighted. We find that hcp metals show a larger variety than the fcc and bcc metals studied up until now. The prolific emission of prismatic loops can lead to extended plastic zones. The size of the plastic zone is quantified by the ratio f of the plastic zone radius to the radius of the contact area. We find values of between 1.6 (an almost collapsed zone) and >5; in the latter case, complex dislocation networks build up which are extended in the direction of easy glide. PMID:26655887

  15. Influence of crystal orientation on hardness and nanoindentation deformation in ion-irradiated stainless steels

    NASA Astrophysics Data System (ADS)

    Miura, Terumitsu; Fujii, Katsuhiko; Fukuya, Koji; Takashima, Keisuke

    2011-10-01

    The influence of crystal orientation on hardness and the range of plastic deformation caused by nanoindentation was investigated in a solution annealed type 316 stainless steel irradiated with Fe 2+ ions. The hardness was a function of grain orientation and was correlated with the Taylor factor averaged over three normal directions of the contact surface of the Berkovich indenter. The transmission electron microscope observations of the deformation microstructure under the indentations showed that the range of plastic deformation reached up to 10 times the indent depth for unirradiated material and depended on the orientation relation between the contact surface of the indenter and the slip directions. The range of plastic deformation decreased as the damage structure developed in ion irradiation.

  16. Magnetic Field Tunable Small-scale Mechanical Properties of Nickel Single Crystals Measured by Nanoindentation Technique

    PubMed Central

    Zhou, Hao; Pei, Yongmao; Fang, Daining

    2014-01-01

    Nano- and micromagnetic materials have been extensively employed in micro-functional devices. However, measuring small-scale mechanical and magnetomechanical properties is challenging, which restricts the design of new products and the performance of smart devices. A new magnetomechanical nanoindentation technique is developed and tested on a nickel single crystal in the absence and presence of a saturated magnetic field. Small-scale parameters such as Young's modulus, indentation hardness, and plastic index are dependent on the applied magnetic field, which differ greatly from their macroscale counterparts. Possible mechanisms that induced 31% increase in modulus and 7% reduction in hardness (i.e., the flexomagnetic effect and the interaction between dislocations and magnetic field, respectively) are analyzed and discussed. Results could be useful in the microminiaturization of applications, such as tunable mechanical resonators and magnetic field sensors. PMID:24695002

  17. Temperature Dependent Mechanical Property of PZT Film: An Investigation by Nanoindentation

    PubMed Central

    Li, Yingwei; Feng, Shangming; Wu, Wenping; Li, Faxin

    2015-01-01

    Load-depth curves of an unpoled Lead Zirconate Titanate (PZT) film composite as a function of temperature were measured by nanoindentation technique. Its reduce modulus and hardness were calculated by the typical Oliver-Pharr method. Then the true modulus and hardness of the PZT film were assessed by decoupling the influence of substrate using methods proposed by Zhou et al. and Korsunsky et al., respectively. Results show that the indentation depth and modulus increase, but the hardness decreases at elevated temperature. The increasing of indentation depth and the decreasing of hardness are thought to be caused by the decreasing of the critical stress needed to excite dislocation initiation at high temperature. The increasing of true modulus is attributed to the reducing of recoverable indentation depth induced by back-switched domains. The influence of residual stress on the indentation behavior of PZT film composite was also investigated by measuring its load-depth curves with pre-load strains. PMID:25768957

  18. Phase Identification of Dual-Phase (DP980) Steels by Electron Backscatter Diffraction and Nanoindentation Techniques.

    PubMed

    Zhang, Fan; Ruimi, Annie; Field, David P

    2016-02-01

    Phase identification of multi-phase materials provides essential information relating the material to its mechanical properties. In this study we selected DP980, a type of dual-phase steel, to investigate the content of martensite and ferrite grains. A combination of advanced techniques was used to provide detailed and precise information of the microstructure. Scanning and transmission electron microscopy were used to provide observations of the sample surface at different scales. Martensite and ferrite phases of DP980 were further identified and characterized using electron backscatter diffraction and scanning probe microscopy. Results obtained with nanoindentation tests confirmed that the differences in nanohardness values in single-phase grains are martensite and ferrite with different surface heights shown by scanning probe microscopy. The similarity shown in the image quality map and scanning probe microscopy proves that a large fraction of martensite can be distinguished in this undeformed material using image quality parameters obtained during electron backscatter diffraction imaging. PMID:26781200

  19. Investigation of the Anisotropic Mechanical Behaviors of Copper Single Crystals Through Nanoindentation Modeling

    NASA Astrophysics Data System (ADS)

    Liu, Mao; Tieu, Kiet Anh; Zhou, Kun; Peng, Ching-Tun

    2016-06-01

    A crystal plasticity finite element method constitutive model was developed to investigate the anisotropic mechanical behaviors of (001), (011), and (111) initially orientated copper (Cu) single crystals during nanoindentation deformation. The numerical load-indentation depth curve and hardness-indentation depth curve were compared with experimental observations to validate the established three-dimensional (3D) CPFEM model. The difference of indentation loads between (111) crystal and (001) crystal is ~10.68 pct, and the difference of indentation modulus between (111) surface and (001) surface is ~10.80 pct. The numerical results show the noticeable indentation size effect for three crystals, and slightly different hardness values on different crystallographic planes. The equivalent plastic strain and lattice rotation angles were also analyzed on three through-thickness cross sections to study the plastic deformation-induced texture anisotropy.

  20. TEM, XRD and nanoindentation characterization of Xenon ion irradiation damage in austenitic stainless steels

    NASA Astrophysics Data System (ADS)

    Huang, H. F.; Li, J. J.; Li, D. H.; Liu, R. D.; Lei, G. H.; Huang, Q.; Yan, L.

    2014-11-01

    Cross-sectional and bulk specimens of a 20% cold-worked 316 austenitic stainless steel (CW 316 SS) has been characterized by TEM, XRD and nanoindentation to determine the microstructural evolution and mechanical property changes of 316 SS after irradiation with 7 MeV Xe26+ ions. TEM results reveal the presence of dislocation loops with a number density of approximately 3 × 1022 m-3 and sizes between 3 to 10 nm due to the collapse of vacancy rich cores inside displacement cascades. Peak broadening observed in XRD diffraction patters reveal systematic changes to lattice parameters due to irradiation. The calculated indentation values in irradiated 316 SS were found to be much higher in comparison to the unirradiated specimen, indicating the dose dependent effect of irradiation on hardness. The relationship between irradiation induced microstructural evolution and the changes to the mechanical properties of CW 316 SS are discussed in the context of fluence and irradiation temperature.

  1. Molecular dynamics simulation of nano-indentation of (111) cubic boron nitride with optimized Tersoff potential

    NASA Astrophysics Data System (ADS)

    Zhao, Yinbo; Peng, Xianghe; Fu, Tao; Huang, Cheng; Feng, Chao; Yin, Deqiang; Wang, Zhongchang

    2016-09-01

    We conduct molecular dynamics simulation of nanoindentation on (111) surface of cubic boron nitride and find that shuffle-set dislocations slip along <112> direction on {111} plane at the initial stage of the indentation. The shuffle-set dislocations are then found to meet together, forming surfaces of a tetrahedron. We also find that the surfaces are stacking-fault zones, which intersect with each other, forming edges of stair-rod dislocations along <110> direction. Moreover, we also calculate the generalized stacking fault (GSF) energies along various gliding directions on several planes and find that the GSF energies of the <112>{111} and <110>{111} systems are relatively smaller, indicating that dislocations slip more easily along <110> and <112> directions on the {111} plane.

  2. Temperature-dependent mechanical properties of single-layer molybdenum disulphide: Molecular dynamics nanoindentation simulations

    SciTech Connect

    Zhao, Junhua; Jiang, Jin-Wu; Rabczuk, Timon

    2013-12-02

    The temperature-dependent mechanical properties of single-layer molybdenum disulphide (MoS{sub 2}) are obtained using molecular dynamics (MD) nanoindentation simulations. The Young's moduli, maximum load stress, and maximum loading strain decrease with increasing temperature from 4.2 K to 500 K. The obtained Young's moduli are in good agreement with those using our MD uniaxial tension simulations and the available experimental results. The tendency of maximum loading strain with different temperature is opposite with that of metal materials due to the short range Stillinger-Weber potentials in MoS{sub 2}. Furthermore, the indenter tip radius and fitting strain effect on the mechanical properties are also discussed.

  3. Dislocation structure in AlN films induced by in situ transmission electron microscope nanoindentation

    NASA Astrophysics Data System (ADS)

    Tokumoto, Yuki; Kutsukake, Kentaro; Ohno, Yutaka; Yonenaga, Ichiro

    2012-11-01

    To elucidate dislocation generation and propagation processes in AlN films containing a high density of grown-in threading dislocations (TDs), in situ nanoindentation (NI) was performed in a transmission electron microscope at room temperature. Dislocations with the Burgers vector b = 1/3<12¯10> were introduced not only on the primary slip plane, i.e., the (0001) basal planes, but also on the {101¯1} and {101¯2} pyramidal planes. The results are explained by considering the distribution of the resolved shear stress. It was found that the dislocations induced by NI interact with grown-in TDs: (1) for the NI-induced dislocations on pyramidal planes, edge grown-in TDs induce cross slip to basal planes, and (2) for the NI-induced dislocations on basal planes, screw grown-in TDs prevent their propagation, while edge grown-in TDs do not.

  4. Nanoindentation of hcp metals: a comparative simulation study of the evolution of dislocation networks

    NASA Astrophysics Data System (ADS)

    Alabd Alhafez, Iyad; Ruestes, Carlos J.; Gao, Yu; Urbassek, Herbert M.

    2016-01-01

    Using molecular dynamics simulation, we study the nanoindentation of three hcp metals: Mg, Ti, and Zr. Both the basal and two prismatic surface planes are considered. We focus on the characterization of the plasticity generated in the crystal. The similarities to, and the differences from, the behavior of the more commonly investigated fcc and bcc metals are highlighted. We find that hcp metals show a larger variety than the fcc and bcc metals studied up until now. The prolific emission of prismatic loops can lead to extended plastic zones. The size of the plastic zone is quantified by the ratio f of the plastic zone radius to the radius of the contact area. We find values of between 1.6 (an almost collapsed zone) and >5 in the latter case, complex dislocation networks build up which are extended in the direction of easy glide.

  5. Influence of crystallographic orientation on the response of copper crystallites to nanoindentation

    SciTech Connect

    Korchuganov, Aleksandr V.; Kryzhevich, Dmitrij S. E-mail: kost@ispms.tsc.ru; Zolnikov, Konstantin P. E-mail: kost@ispms.tsc.ru; Psakhie, Sergey G.

    2014-11-14

    Molecular dynamics simulation was performed to study the features of nucleation and development of plastic deformation in copper crystallites in nanoindentation with different crystallographic orientations of their loaded surface: (011), (001), and (111). Atomic interaction was described by a potential constructed in terms of the embedded atom method. It is shown that behavior of the crystallite reaction force correlates well with a change in the fraction of atoms involved in local structural rearrangements. The generation of local structural changes decreases the slope of the crystallite reaction force curve or results in an extremum due to internal stress relaxation. Analysis of structural changes in the material being indented demonstrates that the orientation of its loaded surface greatly affects the features of nucleation and development of plastic deformation.

  6. Microstructure and Nanoindentation Characterization of Low Temperature Hybrid Treated layer on Austenitic Stainless Steel

    NASA Astrophysics Data System (ADS)

    Triwiyanto, Askar; Hussain, Patthi; Che Ismail, Mokhtar

    2013-06-01

    In this work, the hybrid treated layer on austenitic AISI 316L stainless steels were characterized to investigate the improvement on its surface properties. Characterization of this resulting layer was performed by FESEM (Field Emission Scanning Electron Microscope), USPM (Universal Scanning Probe Microscope) and nanoindentation. By using these methods, changes in the mechanical properties due to the diffusion of carbon and nitrogen at low temperature treatments have been traced. This hybrid treated sample has confirmed a considerable increase in hardness and a small rise in the elastic modulus compared to the untreated sample. It is found that all treated samples have enhance E/H ratio which exhibited the decreasing tendency to plastic deformation and reduced the mismatch of properties, while keeping deformation within the elastic range.

  7. Temperature dependent mechanical property of PZT film: an investigation by nanoindentation.

    PubMed

    Li, Yingwei; Feng, Shangming; Wu, Wenping; Li, Faxin

    2015-01-01

    Load-depth curves of an unpoled Lead Zirconate Titanate (PZT) film composite as a function of temperature were measured by nanoindentation technique. Its reduce modulus and hardness were calculated by the typical Oliver-Pharr method. Then the true modulus and hardness of the PZT film were assessed by decoupling the influence of substrate using methods proposed by Zhou et al. and Korsunsky et al., respectively. Results show that the indentation depth and modulus increase, but the hardness decreases at elevated temperature. The increasing of indentation depth and the decreasing of hardness are thought to be caused by the decreasing of the critical stress needed to excite dislocation initiation at high temperature. The increasing of true modulus is attributed to the reducing of recoverable indentation depth induced by back-switched domains. The influence of residual stress on the indentation behavior of PZT film composite was also investigated by measuring its load-depth curves with pre-load strains. PMID:25768957

  8. In Situ Nanoindentation Studies on Detwinning and Work Hardening in Nanotwinned Monolithic Metals

    SciTech Connect

    Liu, Y.; Li, N.; Bufford, D.; Lee, J. H.; Wang, J.; Wang, H.; Zhang, X.

    2015-07-14

    Certain nanotwinned (nt) metals have rare combinations of high mechanical strength and ductility. Here, we review recent in situ nanoindentation studies (using transmission electron microscopes) on the deformation mechanisms of nt face-centered cubic metals including Cu, Ni, and Al with a wide range of stacking fault energy (SFE). Moreover, in nt Cu with low-to-intermediate SFE, detwinning (accompanied by rapid twin boundary migration) occurs at ultralow stress. In Ni with relatively high SFE, coherent {111} twin boundaries lead to substantial work hardening. Twinned Al has abundant {112} incoherent twin boundaries, which induce significant work-hardening capability and plasticity in Al. Finally, twin boundaries in Al also migrate but at very high stresses. Furthermore, molecular dynamics simulations reveal the influence of SFE on deformation mechanisms in twinned metals.

  9. He and H irradiation effects on the nanoindentation hardness of CLAM steel

    NASA Astrophysics Data System (ADS)

    Jiang, Siben; Peng, Lei; Ge, Hongen; Huang, Qunying; Xin, Jingping; Zhao, Ziqiang

    2014-12-01

    In this study, He and H ion irradiation induced hardening behavior of China Low Activation Martensitic (CLAM) steel was investigated, and the influence of Si on irradiation hardening was also examined. CLAM steel with different Si contents, Heat 0912 and Heat 0408D, were irradiated with single He (He concentration range from 0 to 2150 appm) ion beam and He/H dual ion beams. Then nanoindentation tests were applied to evaluate the ion irradiation induced hardening effect. The result of Heat 0912 showed hardening effect would be more serious with higher He concentration, and the trend saturated when He concentration reach 1000 appm. Comparing the result of Heat 0912 and Heat 0408D, higher Si content might improve the resistance to hardening.

  10. Microtexture and Nanoindentation Study of Delamination Cracking in Al-Cu-Li-X Alloys

    NASA Technical Reports Server (NTRS)

    Crooks, R.; Domack, M. S.; Wagner, J. A.

    2005-01-01

    Commercial Al-Li alloys have strength and weight advantages over non-Li aluminum alloys. The fracture behavior of these alloys is unusual and has limited their use. The fracture mode, described as delamination, is intergranular, along the broad grain boundaries parallel to the rolling plane of the plate. Microtexture analyses have shown that delaminations occur along boundaries with greater than 30 misorientation. However, it was observed that relatively few of the high angle boundaries exhibited this behavior. Some grains of the retained deformation texture show high internal misorientation, which is a measure of stored strain energy. Delamination tends to occur between these grains and adjacent, recrystallized grains. Nanoindentation studies indicate a higher hardness for the high internal misorientation grains. These results suggest that the delamination could be reduced by processing the alloys to minimize grain-to-grain property disparities.

  11. High speed AFM studies of 193 nm immersion photoresists during TMAH development

    NASA Astrophysics Data System (ADS)

    Ngunjiri, Johnpeter; Meyers, Greg; Cameron, Jim; Suzuki, Yasuhiro; Jeon, Hyun; Lee, Dave; Choi, Kwang Mo; Kim, Jung Woo; Im, Kwang-Hwyi; Lim, Hae-Jin

    2016-03-01

    In this paper we report on our studies of the dynamic process of resist development in real time. Using High Speed - Atomic Force Microscopy (HS-AFM) in dilute developer solution, changes in morphology and nanomechanical properties of patterned resist were monitored. The Bruker Dimension FastScan AFMTM was applied to analyze 193 nm acrylic-based immersion resists in developer. HS-AFM operated in Peak Force mapping mode allowed for concurrent measurements of image topography resist stiffness, adhesion to AFM probe and deformation during development. In our studies we focused on HS-AFM topography data as it readily revealed detailed information about initial resist morphology, followed by a resist swelling process and eventual dissolution of the exposed resist areas. HS-AFM showed potential for tracking and understanding development of patterned resist films and can be useful in evaluating the dissolution properties of different resist designs.

  12. A review of design concepts for the Advanced Fluids Module (AFM) project

    NASA Technical Reports Server (NTRS)

    Hill, Myron E.; Tschen, Peter S.

    1993-01-01

    This paper reviews preliminary fluid module design concepts for the Advanced Fluids Module (AFM) project. The objective of this effort is to provide a facility that can handle a wide variety of fluids experiments. Sample science requirements were written and conceptual designs were subsequently generated during the last year. Experiments from the following fluid physics subject areas were used as conceptual design drivers: static and dynamic interfacial phenomena; bubble/droplet thermocapillary migration; surface tension convection and instabilities; thermal/solutal convection; pool boiling; and multiphase flow. After the conceptual designs were completed, the next phase attempted to combine experiments capabilities into a multipurpose, multiuser apparatus configured for the Space Station Freedom. It was found that all the fluid subject areas considered could be accommodated by three basic types of fluids modules. These modules are the Static Fluid Cell Module, the Dynamic Fluid Cell Module, and the Multiphase Flow Module. Descriptions of these preliminary modules designs and their particular sub-systems (e.g., fluid and thermal systems) are discussed. These designs will be refined as the nature of the flight program becomes clearer over the next six to twelve months.

  13. Diabetes increases stiffness of live cardiomyocytes measured by atomic force microscopy nanoindentation.

    PubMed

    Benech, Juan C; Benech, Nicolás; Zambrana, Ana I; Rauschert, Inés; Bervejillo, Verónica; Oddone, Natalia; Damián, Juan P

    2014-11-15

    Stiffness of live cardiomyocytes isolated from control and diabetic mice was measured using the atomic force microscopy nanoindentation method. Type 1 diabetes was induced in mice by streptozotocin administration. Histological images of myocardium from mice that were diabetic for 3 mo showed disorderly lineup of myocardial cells, irregularly sized cell nuclei, and fragmented and disordered myocardial fibers with interstitial collagen accumulation. Phalloidin-stained cardiomyocytes isolated from diabetic mice showed altered (i.e., more irregular and diffuse) actin filament organization compared with cardiomyocytes from control mice. Sarco/endoplasmic reticulum Ca(2+)-ATPase (SERCA2a) pump expression was reduced in homogenates obtained from the left ventricle of diabetic animals compared with age-matched controls. The apparent elastic modulus (AEM) for live control or diabetic isolated cardiomyocytes was measured using the atomic force microscopy nanoindentation method in Tyrode buffer solution containing 1.8 mM Ca(2+) and 5.4 mM KCl (physiological condition), 100 nM Ca(2+) and 5.4 mM KCl (low extracellular Ca(2+) condition), or 1.8 mM Ca(2+) and 140 mM KCl (contraction condition). In the physiological condition, the mean AEM was 112% higher for live diabetic than control isolated cardiomyocytes (91 ± 14 vs. 43 ± 7 kPa). The AEM was also significantly higher in diabetic than control cardiomyocytes in the low extracellular Ca(2+) and contraction conditions. These findings suggest that the material properties of live cardiomyocytes were affected by diabetes, resulting in stiffer cells, which very likely contribute to high diastolic LV stiffness, which has been observed in vivo in some diabetes mellitus patients. PMID:25163520

  14. NANOINDENTATION OF THE INSERTIONAL ZONES OF HUMAN MENISCAL ATTACHMENTS INTO UNDERLYING BONE

    PubMed Central

    Hauch, K.N.; Oyen, M.L.; Odegard, G.M.; Haut Donahue, T. L.

    2009-01-01

    The fibrocartilagenous knee menisci are situated between the femoral condyles and tibia plateau and are primarily anchored to the tibia by means of four attachments at the anterior and posterior horns. Strong fixation of meniscal attachments to the tibial plateau provide resistance to extruding forces of the meniscal body, allowing the menisci to assist in load transmission from the femur to the tibia. Clinically, tears and ruptures of the meniscal attachments and insertion to bone are rare. While it has been suggested that the success of a meniscal replacement is dependent on several factors, one of which is the secure fixation and firm attachment of the replacement to the tibial plateau, little is known about the material properties of meniscal attachments and the transition in material properties from the meniscus to subchondral bone. The objective of this study was to use nanoindentation to investigate the transition from meniscal attachment into underlying subchondral bone through uncalcified and calcified fibrocartilage. Nanoindentation tests were performed on both the anterior and posterior meniscal insertions to measure the instantaneous elastic modulus and elastic modulus at infinite time. The elastic moduli were found to increase in a bi-linear fashion from the external ligamentous attachment to the subchondral bone. The elastic moduli for the anterior attachments were consistently larger than those for the matching posterior attachments at similar indentation locations. These results show that there is a gradient of stiffness from the superficial zones of the insertion close to the ligamentous attachment into the deeper zones of the bone. This information will be useful in the continued development of successful meniscal replacements and understanding of fixation of the replacements to the tibial plateau. PMID:19627840

  15. Tubulin Bond Energies and Microtubule Biomechanics Determined from Nanoindentation in Silico

    PubMed Central

    2015-01-01

    Microtubules, the primary components of the chromosome segregation machinery, are stabilized by longitudinal and lateral noncovalent bonds between the tubulin subunits. However, the thermodynamics of these bonds and the microtubule physicochemical properties are poorly understood. Here, we explore the biomechanics of microtubule polymers using multiscale computational modeling and nanoindentations in silico of a contiguous microtubule fragment. A close match between the simulated and experimental force–deformation spectra enabled us to correlate the microtubule biomechanics with dynamic structural transitions at the nanoscale. Our mechanical testing revealed that the compressed MT behaves as a system of rigid elements interconnected through a network of lateral and longitudinal elastic bonds. The initial regime of continuous elastic deformation of the microtubule is followed by the transition regime, during which the microtubule lattice undergoes discrete structural changes, which include first the reversible dissociation of lateral bonds followed by irreversible dissociation of the longitudinal bonds. We have determined the free energies of dissociation of the lateral (6.9 ± 0.4 kcal/mol) and longitudinal (14.9 ± 1.5 kcal/mol) tubulin–tubulin bonds. These values in conjunction with the large flexural rigidity of tubulin protofilaments obtained (18,000–26,000 pN·nm2) support the idea that the disassembling microtubule is capable of generating a large mechanical force to move chromosomes during cell division. Our computational modeling offers a comprehensive quantitative platform to link molecular tubulin characteristics with the physiological behavior of microtubules. The developed in silico nanoindentation method provides a powerful tool for the exploration of biomechanical properties of other cytoskeletal and multiprotein assemblies. PMID:25389565

  16. Influences of spherical tip radius, contact depth, and contact area on nanoindentation properties of bone.

    PubMed

    Paietta, Rachel C; Campbell, Sara E; Ferguson, Virginia L

    2011-01-11

    Nanoindentation has been widely used as a means to measure the micro-mechanical properties of bone and to predict the macroscopic properties. The role of indent depth and indenter tip geometry in measuring the hierarchical properties of bone tissue was explored experimentally using a range of spherical indenter tips of R=5, 25, 65, and 200 μm. Nanoindentation arrays, not targeted to fall on specific structures or locations, enabled statistical sampling of osteons within PMMA-embedded, bovine, cortical bone on a single sample to a range of maximum displacements (minimum of 100 nm and maximum of 2000 nm). Elastic finite element models were then utilized to isolate the contributions of indenter tip radius, contact area, and position within the lamellar structure in comparison to the experimental results. For a small, R=5 μm indenter tip, indentation modulus consistently increased with contact depth and increased plastic deformation, resulting in an artificial increase in elastic properties. While larger radius tips (R=25, 65, and 200 μm) did not enable evaluation of a high spatial resolution on the surface, they produced data that was representative of the lower load and contact depth measurements with the smaller tip. However the sensitivity to mechanical property variations across the 2-D surface of the material was lost with increase in indenter tip size. Correspondingly, measurement variance was also decreased as the volume contributing to the indent response represented an average of surface roughness, varying mineral content, defects, and underlying tissue type and structure. PMID:21092970

  17. BOREAS AFM-2 Wyoming King Air 1994 Aircraft Sounding Data

    NASA Technical Reports Server (NTRS)

    Kelly, Robert D.; Hall, Forrest G. (Editor); Knapp, David E. (Editor); Smith, David E. (Technical Monitor)

    2000-01-01

    The BOREAS AFM-2 team used the University of Wyoming King Air aircraft during IFCs 1, 2, and 3 in 1994 to collected pass-by-pass fluxes (and many other statistics) for the large number of level (constant altitude), straight-line passes used in a variety of flight patterns over the SSA and NSA and areas along the transect between these study areas. The data described here form a second set, namely soundings that were incorporated into nearly every research flight by the King Air in 1994. These soundings generally went from near the surface to above the inversion layer. Most were flown immediately after takeoff or immediately after finishing the last flux pattern of that particular day's flights. The parameters that were measured include wind direction, wind speed, west wind component (u), south wind component (v), static pressure, air dry bulb temperature, potential temperature, dewpoint, temperature, water vapor mixing ratio, and CO2 concentration. Data on the aircraft's location, attitude, and altitude during data collection are also provided. These data are stored in tabular ASCH files. The data files are available on a CD-ROM (see document number 20010000884) or from the Oak Ridge National Laboratory (ORNL) Distributed Active Archive Center (DAAC).

  18. BOREAS AFM-03-NCAR Electra 1994 Aircraft Sounding Data

    NASA Technical Reports Server (NTRS)

    Lenschow, Donald H.; Oncley, Steven P.; Hall, Forrest G. (Editor); Knapp, David E. (Editor); Smith, David E. (Technical Monitor)

    2000-01-01

    The Boreal Ecosystem-Atmosphere Study (BOREAS) Airborne Fluxes and Meteorology (AFM)-3 team used the National Center for Atmospheric Research's (NCAR) Electra aircraft to make sounding measurements to study the planetary boundary layer using in situ and remote-sensing measurements. Measurements were made of wind speed and direction, air pressure and temperature, potential temperature, dewpoint, mixing ratio of H, O, CO, concentration, and ozone concentration. Twenty-five research missions were flown over the Northern Study Area (NSA), Southern Study Area (SSA), and the transect during BOREAS Intensive Field Campaigns (IFCs) 1, 2, and 3 during 1994. All missions had from four to ten soundings through the top of the planetary boundary layer. This sounding data set contains all of the in situ vertical profiles through the boundary layer top that were made (with the exception of 'porpoise' maneuvers). Data were recorded in one-second time intervals. These data are stored in tabular ASCII files. The NCAR Electra 1994 aircraft sounding data are available from the Earth Observing System Data and Information System (EOSDIS) Oak Ridge National Laboratory (ORNL) Distributed Active Archive Center (DAAC). The data files are available on a CD-ROM (see document number 20010000884).

  19. AFM-based force microsensor for a microrobot

    NASA Astrophysics Data System (ADS)

    Fatikow, Sergej; Fahlbusch, Stephan

    2001-10-01

    Microrobots are the result of increasing research activities at the border between microsystem technology and robotics. Today already, robots with dimensions of a few cubic- centimeters can be developed. Like conventional robots, microrobots represent a complex system that usually contains several different types of actuators and sensors. The measurement of gripping forces is the most important sensor application in micromanipulation besides visual servoing to protect the parts from too high surface pressures and thereby damage during the assembly process. Very small forces in the range of 200 (mu) N down to 0.1 (mu) N or even less have to be sensed. Thus, the aim of our current research activities is the development of a high-resolution integrated force microsensor for measuring gripping forces in a microhandling robot. On the one hand, the sensor should be a device for teleoperated manipulation tasks in a flexible microhandling station. On the other hand, typical microhandling operations should to a large extend be automated with the aid of computer-based signal processing of sensor information. The user should be provided with an interface for teleoperated manipulation and an interface for partially automated manipulation of microobjects. In this paper, a concept for the measurement of gripping forces in microrobotics using piezoresistive AFM (atomic force microscope) cantilevers is introduced. Further on, the concept of a microrobot-based SEM station and its applications are presented.

  20. AFM Investigation of Liquid-Filled Polymer Microcapsules Elasticity.

    PubMed

    Sarrazin, Baptiste; Tsapis, Nicolas; Mousnier, Ludivine; Taulier, Nicolas; Urbach, Wladimir; Guenoun, Patrick

    2016-05-10

    Elasticity of polymer microcapsules (MCs) filled with a liquid fluorinated core is studied by atomic force microscopy (AFM). Accurately characterized spherical tips are employed to obtain the Young's moduli of MCs having four different shell thicknesses. We show that those moduli are effective ones because the samples are composites. The strong decrease of the effective MC elasticity (from 3.0 to 0.1 GPa) as the shell thickness decreases (from 200 to 10 nm) is analyzed using a novel numerical approach. This model describes the evolution of the elasticity of a coated half-space according to the contact radius, the thickness of the film, and the elastic moduli of bulk materials. This numerical model is consistent with the experimental data and allows simulating the elastic behavior of MCs at high frequencies (5 MHz). While the quasi-static elasticity of the MCs is found to be very dependent on the shell thickness, the high frequency (5 MHz) elastic behavior of the core leads to a stable behavior of the MCs (from 2.5 to 3 GPa according to the shell thickness). Finally, the effect of thermal annealing on the MCs elasticity is investigated. The Young's modulus is found to decrease because of the reduction of the shell thickness due to the loss of the polymer. PMID:27058449

  1. In situ AFM crystal growth and dissolution study of calcite in the presence of aqueous fluoride

    NASA Astrophysics Data System (ADS)

    Vavouraki, A.; Putnis, C. V.; Putnis, A.; Koutsoukos, P. G.

    2009-04-01

    Fluoride is naturally abundant, encountered in rocks, soil and fresh and ocean water. Calcite crystals, during crystal growth may incorporate fluoride ions into their lattice (Okumura et al., 1983). In situ atomic force microscopy (AFM) has been used to study the growth and dissolution of calcite {104} surfaces in aqueous solutions in the presence of fluoride, using a fluid cell in which the supersaturated and the understaturated solutions respectively, flow over a freshly cleaved calcite crystal. For growth experiments, supersaturation index (S.I.) with respect to calcite was equal to 0.89 and the initial solution pH 10.2. The crystal growth rates were measured from the closure of the rhombohedral etch pits along the [010] direction induced by an initial dissolution step using pure water. The spreading rate of 2-dimensional nuclei was also measured along the same direction. In the presence of low fluoride concentrations (≤0.33 mM), the crystal growth rate of calcite was unaffected. At higher concentrations (up to 5 mM) growth rate decreased substantially to 50% of the rate in the absence of fluoride. Potential fluoride sorption over the calcite surface may ascribe the decrease of growth rates. Dissolution experiments were conducted at pH= 7.2 and dissolution rates of calcite were measured from the spreading of rhombohedral etch pits along both [010] and [42] directions. The presence of low concentrations of fluoride (≤1.1 mM) in the undersaturated solutions enhanced the dissolution rate along the [42] direction by 50% in comparison with pure water. The morphology of rhombohedral etch pits changed to hexagonal in the presence of fluoride in the undersaturated solutions. The AFM dissolution experiments suggested that the fluoride ions adsorbed onto the calcite surface. Further increase of fluoride concentrations (up to 1.6 mM) resulted in the decrease of the calcite dissolution rate by 60% in both [010] and [42] directions. Reference: Okumura, M, Kitano, Y

  2. PREFACE: NC-AFM 2005: Proceedings of the 8th International Conference on Non-Contact Atomic Force Microscopy

    NASA Astrophysics Data System (ADS)

    Reichling, M.; Mikosch, W.

    2006-04-01

    The 8th International Conference on Non-Contact Atomic Force Microscopy, held in Bad Essen, Germany, from 15 18th August 2005, attracted a record breaking number of participants presenting excellent contributions from a variety of scientific fields. This clearly demonstrated the high level of activity and innovation present in the community of NC-AFM researchers and the continuous growth of the field. The strongest ever participation of companies for a NC-AFM meeting is a sign for the emergence of new markets for the growing NC-AFM community; and the high standard of the products presented at the exhibition, many of them brand-new developments, reflected the unbroken progress in technology. The development of novel technologies and the sophistication of known techniques in research laboratories and their subsequent commercialization is still a major driving force for progress in this area of nanoscience. The conference was a perfect demonstration of how progress in the development of enabling technologies can readily be transcribed into basic research yielding fundamental insight with an impact across disciplines. The NC-AFM 2005 scientific programme was based on five cornerstones, each representing an area of vivid research and scientific progress. Atomic resolution imaging on oxide surfaces, which has long been a vision for the catalysis community, appears to be routine in several laboratories and after a period of demonstrative experiments NC-AFM now makes unique contributions to the understanding of processes in surface chemistry. These capabilities also open up new routes for the analysis of clusters and molecules deposited on dielectric surfaces where resolution limits are pushed towards the single atom level. Atomic precision manipulation with the dynamic AFM left the cradle of its infancy and flourishes in the family of bottom-up fabrication nanotechnologies. The systematic development of established and the introduction of new concepts of contrast

  3. XPS and AFM Study of GaAs Surface Treatment

    SciTech Connect

    Contreras-Guerrero, R.; Wallace, R. M.; Aguirre-Francisco, S.; Herrera-Gomez, A.; Lopez-Lopez, M.

    2008-11-13

    Obtaining smooth and atomically clean surfaces is an important step in the preparation of a surface for device manufacturing. In this work different processes are evaluated for cleaning a GaAs surface. A good surface cleaning treatment is that which provides a high level of uniformity and controllability of the surface. Different techniques are useful as cleaning treatments depending on the growth process to be used. The goal is to remove the oxygen and carbon contaminants and then form a thin oxide film to protect the surface, which is easy to remove later with thermal desorption mechanism like molecular beam epitaxy (MBE) with minimal impact to the surface. In this study, atomic force microscopy (AFM), x-ray photoelectron spectroscopy (XPS) and secondary ion mass spectrometry (SIMS) were used to characterize the structure of the surface, the composition, as well as detect oxygen and carbon contaminant on the GaAs surface. This study consists in two parts. The first part the surface was subjected to different chemical treatments. The chemical solutions were: (a)H{sub 2}SO{sub 4}:H{sub 2}O{sub 2}:H{sub 2}O(4:1:100), (b) HCl: H{sub 2}O(1:3), (c)NH{sub 4}OH 29%. The treatments (a) and (b) reduced the oxygen on the surface. Treatment (c) reduces carbon contamination. In the second part we made MOS devices on the surfaces treated. They were characterized by CV and IV electrical measurements. They show frequency dispersion.

  4. AFM nanoscale indentation in air of polymeric and hybrid materials with highly different stiffness

    NASA Astrophysics Data System (ADS)

    Suriano, Raffaella; Credi, Caterina; Levi, Marinella; Turri, Stefano

    2014-08-01

    In this study, nanomechanical properties of a variety of polymeric materials was investigated by means of AFM. In particular, selecting different AFM probes, poly(methyl methacrylate) (PMMA), polydimethylsiloxane (PDMS) bulk samples, sol-gel hybrid thin films and hydrated hyaluronic acid hydrogels were indented in air to determine the elastic modulus. The force-distance curves and the indentation data were found to be greatly affected by the cantilever stiffness and by tip geometry. AFM indentation tests show that the choice of the cantilever spring constant and of tip shape is crucially influenced by elastic properties of samples. When adhesion-dominated interactions occur between the tip and the surface of samples, force-displacement curves reveal that a suitable functionalization of AFM probes allows the control of such interactions and the extraction of Young' modulus from AFM curves that would be otherwise unfeasible. By applying different mathematical models depending on AFM probes and materials under investigation, the values of Young's modulus were obtained and compared to those measured by rheological and dynamic mechanical analysis or to literature data. Our results show that a wide range of elastic moduli (10 kPa-10 GPa) can be determined by AFM in good agreement with those measured by conventional macroscopic measurements.

  5. Photoresponse from single upright-standing ZnO nanorods explored by photoconductive AFM

    PubMed Central

    Beinik, Igor; Kratzer, Markus; Wachauer, Astrid; Wang, Lin; Piryatinski, Yuri P; Brauer, Gerhard; Chen, Xin Yi; Hsu, Yuk Fan; Djurišić, Aleksandra B

    2013-01-01

    Summary Background: ZnO nanostructures are promising candidates for the development of novel electronic devices due to their unique electrical and optical properties. Here, photoconductive atomic force microscopy (PC-AFM) has been applied to investigate transient photoconductivity and photocurrent spectra of upright-standing ZnO nanorods (NRs). With a view to evaluate the electronic properties of the NRs and to get information on recombination kinetics, we have also performed time-resolved photoluminescence measurements macroscopically. Results: Persistent photoconductivity from single ZnO NRs was observed for about 1800 s and was studied with the help of photocurrent spectroscopy, which was recorded locally. The photocurrent spectra recorded from single ZnO NRs revealed that the minimum photon energy sufficient for photocurrent excitation is 3.1 eV. This value is at least 100 meV lower than the band-gap energy determined from the photoluminescence experiments. Conclusion: The obtained results suggest that the photoresponse in ZnO NRs under ambient conditions originates preferentially from photoexcitation of charge carriers localized at defect states and dominates over the oxygen photodesorption mechanism. Our findings are in agreement with previous theoretical predictions based on density functional theory calculations as well as with earlier experiments carried out at variable oxygen pressure. PMID:23616940

  6. Tuning the resonance of a photonic crystal microcavity with an AFM probe.

    PubMed

    Märki, Iwan; Salt, Martin; Herzig, Hans Peter

    2006-04-01

    We present theoretical and experimental results on switching and tuning of a two-dimensional photonic crystal resonant microcavity by means of a silicon AFM tip, probing the highly localized optical field in the vicinity of the cavity. On-off switching and modulation of the transmission signal in the kHz range is achieved by bringing an AFM tip onto the center of the microcavity, inducing a damping effect on the transmission resonance. Tuning of the resonant wavelength in the order of several nanometers becomes possible by inserting the AFM tip into one of the holes of the Bragg mirror forming the microcavity in the propagation direction. PMID:19516436

  7. Development of portable experimental set-up for AFM to work at cryogenic temperature

    NASA Astrophysics Data System (ADS)

    Agarwal, D. H.; Bhatt, P. M.; Pathan, A. M.; Patel, Hitarthi; Joshi, U. S.

    2012-06-01

    We report on the designing aspects and fabrication of low temperature atomic force microscope (AFM) to study the surface structures of nanomaterials. Several key features of design including liquid nitrogen reservoir, vacuum chamber, vibration isolation table etc. have been presented. The whole set up was assembled in-house at a fairly low cost to be used with any commercial AFM system. The surface morphology of important oxide (In0.94Sn0.04)2O3 (ITO) thin film nanostructures has been investigated using the cryogenic AFM set up.

  8. The formation of liquid bridge in different operating modes of AFM

    NASA Astrophysics Data System (ADS)

    Wei, Zheng; Sun, Yan; Ding, WenXuan; Wang, ZaiRan

    2016-09-01

    The liquid bridge is one of the principal factors that cause artifacts in ambient-pressure atomic force microscope (AFM) images. Additionally, it is the main component of the adhesion force in ambient conditions. To understand the AFM imaging mechanism and the sample characteristics, it is essential to study the liquid bridge. This study interprets the physical mechanism involved in liquid bridge formation, which is composed of three different physical processes: the squeezing process, capillary condensation, and liquid film flow. We discuss the contributions of these three mechanisms to the volume and the capillary force of the liquid bridge in different AFM operation modes.

  9. MetaRep, an extended CMAS 3D program to visualize mafic (CMAS, ACF-S, ACF-N) and pelitic (AFM-K, AFM-S, AKF-S) projections

    NASA Astrophysics Data System (ADS)

    France, Lydéric; Nicollet, Christian

    2010-06-01

    MetaRep is a program based on our earlier program CMAS 3D. It is developed in MATLAB ® script. MetaRep objectives are to visualize and project major element compositions of mafic and pelitic rocks and their minerals in the pseudo-quaternary projections of the ACF-S, ACF-N, CMAS, AFM-K, AFM-S and AKF-S systems. These six systems are commonly used to describe metamorphic mineral assemblages and magmatic evolutions. Each system, made of four apices, can be represented in a tetrahedron that can be visualized in three dimensions with MetaRep; the four tetrahedron apices represent oxides or combination of oxides that define the composition of the projected rock or mineral. The three-dimensional representation allows one to obtain a better understanding of the topology of the relationships between the rocks and minerals and relations. From these systems, MetaRep can also project data in ternary plots (for example, the ACF, AFM and AKF ternary projections can be generated). A functional interface makes it easy to use and does not require any knowledge of MATLAB ® programming. To facilitate the use, MetaRep loads, from the main interface, data compiled in a Microsoft Excel ™ spreadsheet. Although useful for scientific research, the program is also a powerful tool for teaching. We propose an application example that, by using two combined systems (ACF-S and ACF-N), provides strong confirmation in the petrological interpretation.

  10. Molecular shape and binding force of Mycoplasma mobile's leg protein Gli349 revealed by an AFM study

    SciTech Connect

    Lesoil, Charles; Nonaka, Takahiro; Sekiguchi, Hiroshi; Osada, Toshiya; Miyata, Makoto; Afrin, Rehana; Ikai, Atsushi

    2010-01-15

    Recent studies of the gliding bacteria Mycoplasma mobile have identified a family of proteins called the Gli family which was considered to be involved in this novel and yet fairly unknown motility system. The 349 kDa protein called Gli349 was successfully isolated and purified from the bacteria, and electron microscopy imaging and antibody experiments led to the hypothesis that it acts as the 'leg' of M. mobile, responsible for attachment to the substrate as well as for gliding motility. However, more precise evidence of the molecular shape and function of this protein was required to asses this theory any further. In this study, an atomic force microscope (AFM) was used both as an imaging and a force measurement device to provide new information about Gli349 and its role in gliding motility. AFM images of the protein were obtained revealing a complex structure with both rigid and flexible parts, consistent with previous electron micrographs of the protein. Single-molecular force spectroscopy experiments were also performed, revealing that Gli349 is able to specifically bind to sialyllactose molecules and withstand unbinding forces around 70 pN. These findings strongly support the idea that Gli349 is the 'leg' protein of M. mobile, responsible for binding and also most probably force generation during gliding motility.

  11. Correction of the post -- necking true stress -- strain data using instrumented nanoindentation

    NASA Astrophysics Data System (ADS)

    Romero Fonseca, Ivan Dario

    The study of large plastic deformations has been the focus of numerous studies particularly in the metal forming processes and fracture mechanics fields. A good understanding of the plastic flow properties of metallic alloys and the true stresses and true strains induced during plastic deformation is crucial to optimize the aforementioned processes, and to predict ductile failure in fracture mechanics analyzes. Knowledge of stresses and strains is extracted from the true stress-strain curve of the material from the uniaxial tensile test. In addition, stress triaxiality is manifested by the neck developed during the last stage of a tensile test performed on a ductile material. This necking phenomenon is the factor responsible for deviating from uniaxial state into a triaxial one, then, providing an inaccurate description of the material's behavior after the onset of necking. The research of this dissertation is aimed at the development of a correction method for the nonuniform plastic deformation (post-necking) portion of the true stress-strain curve. The correction proposed is based on the well-known relationship between hardness and flow (yield) stress, except that instrumented nanoindentation hardness is utilized rather than conventional macro or micro hardness. Three metals with different combinations of strain hardening behavior and crystal structure were subjected to quasi-static tensile tests: power-law strain hardening low carbon G10180 steel (BCC) and electrolytic tough pitch copper C11000 (FCC), and linear strain hardening austenitic stainless steel S30400 (FCC). Nanoindentation hardness values, measured on the broken tensile specimen, were converted into flow stress values by means of the constraint factor C from Tabor's, the representative plastic strainepsilonr and the post-test true plastic strains measured. Micro Vickers hardness testing was carried out on the sample as well. The constraint factors were 5.5, 4.5 and 4.5 and the representative plastic

  12. Characterization Of Multi-layered Fish Scales (Atractosteus spatula) Using Nanoindentation, X-ray CT, FTIR, and SEM

    PubMed Central

    Allison, Paul G.; Rodriguez, Rogie I.; Moser, Robert D.; Williams, Brett A.; Poda, Aimee R.; Seiter, Jennifer M.; Lafferty, Brandon J.; Kennedy, Alan J.; Chandler, Mei Q.

    2014-01-01

    The hierarchical architecture of protective biological materials such as mineralized fish scales, gastropod shells, ram’s horn, antlers, and turtle shells provides unique design principles with potentials for guiding the design of protective materials and systems in the future. Understanding the structure-property relationships for these material systems at the microscale and nanoscale where failure initiates is essential. Currently, experimental techniques such as nanoindentation, X-ray CT, and SEM provide researchers with a way to correlate the mechanical behavior with hierarchical microstructures of these material systems1-6. However, a well-defined standard procedure for specimen preparation of mineralized biomaterials is not currently available. In this study, the methods for probing spatially correlated chemical, structural, and mechanical properties of the multilayered scale of A. spatula using nanoindentation, FTIR, SEM, with energy-dispersive X-ray (EDX) microanalysis, and X-ray CT are presented. PMID:25046233

  13. Effect of Strain Rate on Deformation Behavior of AlCoCrFeNi High-Entropy Alloy by Nanoindentation

    NASA Astrophysics Data System (ADS)

    Tian, L.; Jiao, Z. M.; Yuan, G. Z.; Ma, S. G.; Wang, Z. H.; Yang, H. J.; Zhang, Y.; Qiao, J. W.

    2016-05-01

    In this study, nanoindentation tests with continuous stiffness measurement technique were measured to investigate the deformation behavior of a high-entropy alloy AlCoCrFeNi under different indentation strain rates at room temperature. Results suggest that the creep behavior exhibits remarkable strain rate dependence. In-situ scanning images showed a conspicuous pileup around the indents, indicating that an extremely localized plastic deformation occurred during the nanoindentation. Under different strain rates, elastic modulus basically remains unchanged, while the hardness decreases with increasing indentation depth due to the indentation size effect. Furthermore, the modulus and hardness of AlCoCrFeNi HEAs are greater than that of the Al x CoCrFeNi (x = 0.3,0.5) at the strain rate of 0.2 s-1 due to its higher negative enthalpy of mixing related to the atomic binding force, and the solid solution strengthening induced by the lattice distortion, respectively.

  14. Effects of brushing timing after erosive challenge on enamel loss in situ: White light interferometer and nanoindentation study.

    PubMed

    Tsuda, Yuka; Kitasako, Yuichi; Sadr, Alireza; Nakashima, Syozi; Tagami, Junji

    2016-01-01

    This in situ study aimed to evaluate effects of waiting periods after erosive challenge before toothbrushing on enamel abrasion and nanoindentation hardness. Ten subjects wore intraoral appliances each with a set of 4 bovine enamel blocks. The enamel blocks were subjected to 2 cycles a day for 3 days as follows; intraoral exposure to form acquired pellicle and extraoral erosion followed by either 0, 3, 30 or 60 min intraoral exposure and then brushing, which was performed using an automatic brushing machine. Abrasive loss was assessed by white light interferometry. Nanoindentation was performed to calculate relative hardness. Abrasion and relative hardness were statistically analyzed by ANOVA. Abrasive loss was significantly less in groups exposed to saliva compared with 0 min (p<0.05); there was no significant difference between 30 and 60 min (p>0.05). Relative hardness was statistically higher after intraoral exposure, but no differences existed among any intraoral exposure periods (p>0.05). PMID:27477227

  15. Nano-indentation of single-layer optical oxide thin films grown by electron-beam deposition

    SciTech Connect

    Mehrotra, K.; Oliver, J. B.; Lambropoulos, J. C.

    2015-01-01

    Mechanical characterization of optical oxide thin films is performed using nano-indentation, and the results are explained based on the deposition conditions used. These oxide films are generally deposited to have a porous microstructure that optimizes laser induced damage thresholds, but changes in deposition conditions lead to varying degrees of porosity, density, and possibly the microstructure of the thin film. This can directly explain the differences in the mechanical properties of the film studied here and those reported in literature. Of the four single-layer thin films tested, alumina was observed to demonstrate the highest values of nano-indentation hardness and elastic modulus. This is likely a result of the dense microstructure of the thin film arising from the particular deposition conditions used.

  16. Characterization of multi-layered fish scales (Atractosteus spatula) using nanoindentation, X-ray CT, FTIR, and SEM.

    PubMed

    Allison, Paul G; Rodriguez, Rogie I; Moser, Robert D; Williams, Brett A; Poda, Aimee R; Seiter, Jennifer M; Lafferty, Brandon J; Kennedy, Alan J; Chandler, Mei Q

    2014-01-01

    The hierarchical architecture of protective biological materials such as mineralized fish scales, gastropod shells, ram's horn, antlers, and turtle shells provides unique design principles with potentials for guiding the design of protective materials and systems in the future. Understanding the structure-property relationships for these material systems at the microscale and nanoscale where failure initiates is essential. Currently, experimental techniques such as nanoindentation, X-ray CT, and SEM provide researchers with a way to correlate the mechanical behavior with hierarchical microstructures of these material systems1-6. However, a well-defined standard procedure for specimen preparation of mineralized biomaterials is not currently available. In this study, the methods for probing spatially correlated chemical, structural, and mechanical properties of the multilayered scale of A. spatula using nanoindentation, FTIR, SEM, with energy-dispersive X-ray (EDX) microanalysis, and X-ray CT are presented. PMID:25046233

  17. Deformation behaviour and 6H-LPSO structure formation at nanoindentation in lamellar high Nb containing TiAl alloy

    NASA Astrophysics Data System (ADS)

    Song, L.; Xu, X. J.; Peng, C.; Wang, Y. L.; Liang, Y. F.; Shang, S. L.; Liu, Z. K.; Lin, J. P.

    2015-02-01

    Microstructure and deformation mechanisms at a nanoindentation in the lamellar colony of high Nb containing TiAl alloy have been studied using the focused ion beam and the transmission electron microscopy. Considerable deformation twins are observed around the nanoindentation, and a strain gradient is generated. A continuous change in the bending angle of the lamellar structure can be derived, and a strain-induced grain refinement process is observed as various active deformations split the γ grains into subgrains. In addition to all possible deformation mechanisms (ordinary dislocation, super-dislocation and deformation twining) activated due to the heavy plastic deformation, a 6-layer hexagonal (6H) long-period stacking ordered structure is identified for the first time near the contact zone and is thought to be closely related to the glide of partial dislocations.

  18. Effect of Strain Rate on Deformation Behavior of AlCoCrFeNi High-Entropy Alloy by Nanoindentation

    NASA Astrophysics Data System (ADS)

    Tian, L.; Jiao, Z. M.; Yuan, G. Z.; Ma, S. G.; Wang, Z. H.; Yang, H. J.; Zhang, Y.; Qiao, J. W.

    2016-06-01

    In this study, nanoindentation tests with continuous stiffness measurement technique were measured to investigate the deformation behavior of a high-entropy alloy AlCoCrFeNi under different indentation strain rates at room temperature. Results suggest that the creep behavior exhibits remarkable strain rate dependence. In-situ scanning images showed a conspicuous pileup around the indents, indicating that an extremely localized plastic deformation occurred during the nanoindentation. Under different strain rates, elastic modulus basically remains unchanged, while the hardness decreases with increasing indentation depth due to the indentation size effect. Furthermore, the modulus and hardness of AlCoCrFeNi HEAs are greater than that of the Al x CoCrFeNi ( x = 0.3,0.5) at the strain rate of 0.2 s-1 due to its higher negative enthalpy of mixing related to the atomic binding force, and the solid solution strengthening induced by the lattice distortion, respectively.

  19. Plasticity and ultra-low stress induced twin boundary migration in nanotwinned Cu by in situ nanoindentation studies

    SciTech Connect

    Liu, Y.; Chen, Y.; Jian, J.; Wang, H.; Zhang, X.

    2014-06-09

    Nanotwinned metals have rare combinations of mechanical strength and ductility. Previous studies have shown that detwinning occurs in plastically deformed nanotwinned metals. Although molecular dynamics simulations have predicted that fine nanotwins can migrate at low stress, there is little in situ evidence to validate such predictions. Also it is unclear if detwinning occurs prior to or succeeding plastic yielding. Here, by using in situ nanoindentation in a transmission electron microscope, we show that a non-elastic detwinning process in nanotwinned Cu occurred at ultra-low indentation stress (0.1 GPa), well before the stress necessary for plastic yielding. Furthermore, the in situ nanoindentation technique allows us to differentiate dislocation-nucleation dominated microscopic yielding preceding macroscopic yielding manifested by dislocation-transmission through twin boundaries. This study thus provides further insights for understanding plasticity in nanotwinned metals at microscopic levels.

  20. An in vitro study of the microstructure, composition and nanoindentation mechanical properties of remineralizing human dental enamel

    NASA Astrophysics Data System (ADS)

    Arsecularatne, J. A.; Hoffman, M.

    2014-08-01

    This paper describes the results of an in vitro investigation on the interrelations among microstructure, composition and mechanical properties of remineralizing human dental enamel. Polished enamel samples have been demineralized for 10 min in an acetic acid solution (at pH 3) followed by remineralization in human saliva for 30 and 120 min. Microstructure variations of sound, demineralized and remineralized enamel samples have been analysed using focused ion beam, scanning electron microscopy and transmission electron microscopy, while their compositions have been analysed using energy dispersive x-ray. Variations in the mechanical properties of enamel samples have been assessed using nanoindentation. The results reveal that, under the selected conditions, only partial remineralization of the softened enamel surface layer occurs where some pores remain unrepaired. As a result, while the nanoindentation elastic modulus shows an improvement following remineralization, hardness does not.

  1. Hierarchical super-structure identified by polarized light microscopy, electron microscopy and nanoindentation: Implications for the limits of biological control over the growth mode of abalone sea shells

    PubMed Central

    2012-01-01

    Background Mollusc shells are commonly investigated using high-resolution imaging techniques based on cryo-fixation. Less detailed information is available regarding the light-optical properties. Sea shells of Haliotis pulcherina were embedded for polishing in defined orientations in order to investigate the interface between prismatic calcite and nacreous aragonite by standard materialographic methods. A polished thin section of the interface was prepared with a defined thickness of 60 μm for quantitative birefringence analysis using polarized light and LC-PolScope microscopy. Scanning electron microscopy images were obtained for comparison. In order to study structural-mechanical relationships, nanoindentation experiments were performed. Results Incident light microscopy revealed a super-structure in semi-transparent regions of the polished cross-section under a defined angle. This super-structure is not visible in transmitted birefringence analysis due to the blurred polarization of small nacre platelets and numerous organic interfaces. The relative orientation and homogeneity of calcite prisms was directly identified, some of them with their optical axes exactly normal to the imaging plane. Co-oriented "prism colonies" were identified by polarized light analyses. The nacreous super-structure was also visualized by secondary electron imaging under defined angles. The domains of the super-structure were interpreted to consist of crystallographically aligned platelet stacks. Nanoindentation experiments showed that mechanical properties changed with the same periodicity as the domain size. Conclusions In this study, we have demonstrated that insights into the growth mechanisms of nacre can be obtained by conventional light-optical methods. For example, we observed super-structures formed by co-oriented nacre platelets as previously identified using X-ray Photo-electron Emission Microscopy (X-PEEM) [Gilbert et al., Journal of the American Chemical Society 2008, 130

  2. Grain Growth Orientation and Anisotropy in Cu6Sn5 Intermetallic: Nanoindentation and Electron Backscatter Diffraction Analysis

    NASA Astrophysics Data System (ADS)

    Choudhury, Soud Farhan; Ladani, Leila

    2014-04-01

    As the size of joints in micro/nano-electronics diminishes, the role of intermetallic (IMC) layers becomes more significant. It was shown that solder joint strength is controlled largely by IMC strength at higher strain rates. Additionally, there is a possibility that very small joints are completely composed of IMCs. Further miniaturization of joints may result in statistical grain size effects. Therefore, it is essential to characterize IMC materials and understand their anisotropic mechanical properties. One of the most common types of IMCs in microelectronic joints is Cu6Sn5, which is formed in a variety of bonding materials with different compositions of Sn, Cu, and Ag. This work studies through nanoindentation elastic-plastic properties of a single grain of Cu6Sn5 IMC in a Sn-3.5Ag/Cu system with reflow soldering. Elastic properties such as elastic modulus and hardness were determined from the nanoindentation load-depth curve. The reverse analysis model described by Dao et al. was used to extract plastic properties such as yield strength and strain hardening exponent from nanoindentation data. Care was taken to achieve indentation of single grains with sufficient accuracy and repeatability. Electron backscatter diffraction (EBSD) mapping was used to determine orientation of Cu6Sn5 grains and to relate the orientation with the load-depth curve results of nanoindentation and the corresponding elastic and plastic properties. The EBSD results indicated that the Cu6Sn5 crystal structure is hexagonal. Columnar growth of the Cu6Sn5 grains was observed as the grains mostly grew along the c-axis of the crystal. Indentation of different grains parallel to the basal plane showed no significant difference in mechanical properties.

  3. 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

  4. Fabrication of cone-shaped boron doped diamond and gold nanoelectrodes for AFM-SECM.

    PubMed

    Avdic, A; Lugstein, A; Wu, M; Gollas, B; Pobelov, I; Wandlowski, T; Leonhardt, K; Denuault, G; Bertagnolli, E

    2011-04-01

    We demonstrate a reliable microfabrication process for a combined atomic force microscopy (AFM) and scanning electrochemical microscopy (SECM) measurement tool. Integrated cone-shaped sensors with boron doped diamond (BDD) or gold (Au) electrodes were fabricated from commercially available AFM probes. The sensor formation process is based on mature semiconductor processing techniques, including focused ion beam (FIB) machining, and highly selective reactive ion etching (RIE). The fabrication approach preserves the geometry of the original AFM tips resulting in well reproducible nanoscaled sensors. The feasibility and functionality of the fully featured tips are demonstrated by cyclic voltammetry, showing good agreement between the measured and calculated currents of the cone-shaped AFM-SECM electrodes. PMID:21368355

  5. Fabrication of cone-shaped boron doped diamond and gold nanoelectrodes for AFM-SECM

    NASA Astrophysics Data System (ADS)

    Avdic, A.; Lugstein, A.; Wu, M.; Gollas, B.; Pobelov, I.; Wandlowski, T.; Leonhardt, K.; Denuault, G.; Bertagnolli, E.

    2011-04-01

    We demonstrate a reliable microfabrication process for a combined atomic force microscopy (AFM) and scanning electrochemical microscopy (SECM) measurement tool. Integrated cone-shaped sensors with boron doped diamond (BDD) or gold (Au) electrodes were fabricated from commercially available AFM probes. The sensor formation process is based on mature semiconductor processing techniques, including focused ion beam (FIB) machining, and highly selective reactive ion etching (RIE). The fabrication approach preserves the geometry of the original AFM tips resulting in well reproducible nanoscaled sensors. The feasibility and functionality of the fully featured tips are demonstrated by cyclic voltammetry, showing good agreement between the measured and calculated currents of the cone-shaped AFM-SECM electrodes.

  6. Cyclic nanoindentation studies on CrN thin films prepared by RF sputtering on Zr-based metallic glass

    SciTech Connect

    Jellad, A.; Benameur, T.; Labdi, S.

    2011-01-17

    Cyclic nanoindentation tests were carried out to study the influence of the chromium nitride thin films on the mechanical properties of Zr-based metallic glass. Chromium nitride thin coatings have been deposited on Zr{sub 50}Cu{sub 40}Al{sub 10} metallic glass substrate by RF sputtering. The deposition process was done at room temperature under nitrogen reactive gas using a metallic chromium target. The CrN films have a thickness of 300 nm. Several cyclic nanoindentation measurements were conducted on CrN films and Zr{sub 50}Cu{sub 40}Al{sub 10} metallic glass substrate samples at various loading rate values. We have found that the coated metallic glass sample shows high mechanical properties such as hardness and reduced elastic modulus. Cyclic nanoindentation results show a hardening behaviour for these CrN coatings. Moreover, the CrN coated on Zr-based metallic glass was found to have a high value of resistance to crack propagation, as being analysed through the SEM pictures of the residual Vickers indentation impressions.

  7. Comparative study of helium effects on EU-ODS EUROFER and EUROFER97 by nanoindentation and TEM

    NASA Astrophysics Data System (ADS)

    Roldán, M.; Fernández, P.; Rams, J.; Jiménez-Rey, D.; Materna-Morris, E.; Klimenkov, M.

    2015-05-01

    Helium effects on EU-ODS EUROFER were studied by means of nanoindentation and TEM. The results were compared with those of EUROFER97. Both steels were implanted in a stair-like profile configuration using energies from 2 MeV (maximum He content ∼750 appm He) to 15 MeV (minimum He ∼350 appm He) at room temperature. The nanoindentation tests on He implanted samples showed a hardness increase that depended on the He concentration. The maximum hardness increase observed at 5 mN was 21% in EU-ODS EUROFER and 41% in EUROFER97; it corresponded with the zone with the highest He concentration which was around 750 appm, according to MARLOWE simulation. In addition, FIB lamellae were prepared from EUROFER97 and EU-ODS EUROFER containing the aforementioned zones with maximum (750 appm) and minimum (300 appm) He. TEM investigations carried out showed small and homogeneously distributed He nanobubbles on both alloys in the zone corresponding with maximum He content. These microstructural features seem to be the cause of the hardness increase measured by nanoindentation.

  8. Effects of water molecules on tribological behavior and property measurements in nano-indentation processes - a numerical analysis

    PubMed Central

    2013-01-01

    Nano/micro-manufacturing under wet condition is an important consideration for various tool-based processes such as indentation, scratching, and machining. The existence of liquids adds complexity to the system, changes the tool/work interfacial condition, and affects material behaviors. For indentation, it may also affect material property measurements. However, little effort has been made to study this challenging issue at nano- or atomistic scale. In this study, we tackle this challenge by investigating nano-indentation processes submerged in water using the molecular dynamics (MD) simulation approach. Compared with dry indentation in which no water molecules are present, the existence of water molecules causes the increase of indentation force in initial penetration, but the decrease of indentation force in full penetration. It also reduces the sticking phenomenon between the work and tool atoms during indenter retraction, such that the indentation geometry can be better retained. Meanwhile, nano-indentation under wet condition exhibits the indentation size effect, while dry nano-indentation exhibits the reverse indentation size effect. The existence of water leads to higher computed hardness values at low indentation loads and a smaller value of Young's modulus. In addition, the friction along the tool/work interface is significantly reduced under wet indentation. PMID:24044504

  9. Using XAFS, EDAX and AFM in comparative study of various natural and synthetic emeralds

    NASA Astrophysics Data System (ADS)

    Parikh, P.; Saini, N. L.; Dalela, S.; Bhardwaj, D. M.; Fernandes, S.; Gupta, R. P.; Garg, K. B.

    2003-01-01

    We have performed XAFS, EDAX and AFM studies on some natural and synthetic emeralds. While the XAFS results yield information on changes in the valence of the Cr ion and the n-n distance the AFM is used to determine the areal atomic density on surface of the crystals. It is a pilot study to explore if the three techniques can offer a possible way of distinguishing between the natural and synthetic emeralds and the results are promising.

  10. Reconciling measurements in AFM reference metrology when using different probing techniques

    NASA Astrophysics Data System (ADS)

    Rana, Narender; Archie, Charles; Foucher, Johann

    2011-03-01

    CD-AFM can report CD measurements to several nanometer differences when different probing techniques including probe types, scan methods, or data analyses are employed on the same sample despite using standard calibration techniques. This potentially weakens the assertion that this instrument is inherently accurate. It is particularly important to resolve these discrepancies given the measurement challenges where multiple probing techniques need to be employed to get complete CD information. Probe type refers to tip construction methods that can significantly affect geometrical aspects of probe such as effective length, width, and edge height as well as material composition and coating. Scan code refers to CD or DT mode of tool operation. Analysis includes probe geometry deconvolution and measurement algorithms. These challenges in measurement accuracy are especially significant for the foot or bottom CD metrology of 3D structures. This paper explores the impact of these different probing techniques on the measurement accuracy. In one series of experiments, measurements for different probing techniques are compared when the test and the referencing structures are composed of similar material and possess smooth vertical profiles. The investigation is then extended to explore the accuracy of bottom CD measurement of non vertical profiles encountered in actual process development. A hybrid method using CD and DT modes has been tested to measure the bottom CD of challenging pitch structures. The limited space for the probe is particularly problematic for CD mode but the accuracy of DT mode for CD measurement is a concern. Other challenges will also be discussed along with possible solutions. CD-AFM has increased uncertainty when it comes to measuring within 15 nm of the bottom of a structure. In this regime details of the shape of the probe and the method by which this shape is extracted from the raw data become important. Measured CDs can vary by a few nanometers

  11. Photoconductivity, High-resolution AFM, and Scanning Conductance Microscopy of Porphyrin Nanorods

    NASA Astrophysics Data System (ADS)

    Schwab, Alexander D.; Smith, Deirdre E.; Hone, James

    2005-03-01

    We have shown^1 that the diacid form of the porphyrin tetrakis(4-sulfonatophenyl) porphine (TPPS4) self assembles into nanorods with well-defined height and width. Upon illumination, their conductivity grows over hundreds of seconds. They also produce a zero-bias photocurrent with trainable polarity.^2 We present measurements as a function of illumination wavelength and intensity, which support a model of charge hopping along paths of previously photoionized porphyrin molecules. We also give results from Scanning Conductance Microscopy experiments; these are designed to clarify the role of the contacts in the DC measurements. Our high-resolution AFM images support the model of a hollow tube^3, which collapses on contact with the substrate. ^1A.D. Schwab et al., J. Phys. Chem. B 107, 11339 (2003). ^2A.D. Schwab et al., Nano Letters 4, 1261 (2004). ^3S.C.M. Gandini, E.L. Gelamo, R. Itri, and M. Tabak, Biophys. J. 85, 1259 (2003).

  12. Molecular dynamics simulation of dextran extension by constant force in single molecule AFM.

    PubMed

    Neelov, Igor M; Adolf, David B; McLeish, Tom C B; Paci, Emanuele

    2006-11-15

    The extension of 1-6 polysaccharides has been studied in a series of recent single molecule AFM experiments. For dextran, a key finding was the existence of a plateau in the force-extension curve at forces between 700 and 1000 pN. We studied the extension of the dextran 10-mer under constant force using atomistic simulation with various force fields. All the force fields reproduce the experimental plateau on the force-extension curve. With AMBER94 and AMBER-GLYCAM04 force fields the plateau can be explained by a transition of the glucopyranose rings in the dextran monomers from the chair ((4)C(1)) to the inverted chair ((1)C(4)) conformation while other processes occur at smaller (rotation around C5-C6 bond) or higher (chairs to boat transitions) forces. The CHARMM force field provides a different picture which associates the occurrence of the plateau to chair-boat transitions of the glucopyranose rings. PMID:16950842

  13. Combined quantitative ultrasonic and time-resolved interaction force AFM imaging

    SciTech Connect

    Parlak, Z.; Degertekin, F. L.

    2011-01-15

    The authors describe a method where quantitative ultrasonic atomic force microscopy (UAFM) is achieved during time-resolved interaction force (TRIF) imaging in intermittent contact mode. The method uses a calibration procedure for quantitative UAFM. It improves elasticity measurements of stiff regions of surfaces while retaining the capabilities of the TRIF mode for topography, adhesion, dissipation, and elasticity measurements on soft regions of sample surfaces. This combination is especially advantageous when measuring and imaging samples with broad stiffness range in a nondestructive manner. The experiments utilize an active AFM probe with high bandwidth and the UAFM calibration is performed by measuring the magnitude of the time-resolved UAFM signal at a judiciously chosen frequency for different contact stiffness values during individual taps. Improved sensitivity to stiff surface elasticity is demonstrated on a special sample. The results show that combining UAFM with TRIF provides 2.5 GPa (5%) standard deviation on the silicon surface reduced Young's modulus, representing 5x improvement over using only TRIF mode imaging.

  14. Novel micro-machining method basing on AFM and high-accuracy stage

    NASA Astrophysics Data System (ADS)

    Yan, Yongda; Sun, Tao; Dong, Shen; Cheng, Kai

    2003-01-01

    This paper presents an easy and novel mechanical micro-machining method. Combining the commercial AFM and the high accuracy stage and using a diamond tip as the cutting tool which acts as a single asperity, a mechanical micro-machining system is developed. Some experiments are carried out basing on this system. Influence of the diamond tip"s shape on micro machining is considered. And different machining techniques are compared in this paper. Using this method the intricate patterns (circle, flat, polygon flat and a gear geometry) are successfully fabricated. So the novel approach"s strength are as follows: It can machine several tens of microns micro-parts more easier and cheaper then the conventional technology. And it can image the micro-structure just after it is machined. Generally this technique can be used to machine the mask of other micro-machining process, the mold of micro-parts, or to machine on the micro-part which is fabricated by other ways.

  15. Size and orientation of the lipid II headgroup as revealed by AFM imaging.

    PubMed

    Ganchev, D N; Hasper, H E; Breukink, E; de Kruijff, B

    2006-05-16

    In this study, we investigated the size and orientation of the bacterial Lipid II (L II) headgroup when the L II molecule is present in liquid-crystalline domains of DOPC in a supported DPPC bilayer. Using atomic force microscopy, we detected that L II causes the appearance of a 1.9 nm thick layer, situated over the DOPC headgroup region. With an increased scanning force, this layer can be penetrated by the AFM tip down to the level of the DOPC bilayer. Using different L II precursor molecules, we demonstrated that the detected layer consists of the headgroups of L II and that the MurNAc-pentapeptide unit of the headgroup is responsible for the measured 1.9 nm height of that layer. Monolayer experiments provided information about the in-plane dimensions of the L II headgroup. On the basis of these results and considerations of the molecular dimensions of L II headgroup constituents, we propose a model for the orientation of the L II headgroup in the membrane. In this model, the pentapeptide of the L II headgroup is rather extended and points away from the bilayer surface, which could be important for biological processes, in which L II is involved. PMID:16681392

  16. In situ QCM and TM-AFM investigations of the early stages of degradation of silver and copper surfaces

    NASA Astrophysics Data System (ADS)

    Kleber, Ch.; Hilfrich, U.; Schreiner, M.

    2007-01-01

    The early stages of atmospheric corrosion of pure copper and pure silver specimens were investigated performing in situ tapping mode atomic force microscopy (TM-AFM), in situ quartz crystal microbalance (QCM) and X-ray photoelectron spectroscopy (XPS). The information obtained by TM-AFM is the change of the topography of the sample surfaces with emphasis on the shape and lateral distribution of the corrosion products grown within the first hours of weathering. The simultaneously performed in situ QCM measurements are indicating the mass changes due to possibly occurring corrosive processes on the surface during weathering and are therefore a valuable tool for the determination of corrosion rates. Investigations were carried out in synthetic air at different levels of relative humidity (RH) with and without addition of 250 ppb SO 2 as acidifying agent. On a polished copper surface the growth of corrosion products could be observed by TM-AFM analysis at 60% RH without any addition of acidifying gases [M. Wadsak, M. Schreiner, T. Aastrup, C. Leygraf, Surf. Sci. 454-456 (2000) 246-250]. On a weathered copper surface the addition of SO 2 to the moist air stream leads to the formation of additional features as already described in the literature [M. Wadsak, M. Schreiner, T. Aastrup, C. Leygraf, Surf. Sci. 454-456 (2000) 246-250; Ch. Kleber, J. Weissenrieder, M. Schreiner, C. Leygraf, Appl. Surf. Sci. 193 (2002) 245-253]. Exposing a silver specimen to humidity leads to the degradation of the surface structure as well as to a formation of corrosion products, which could be detected by in situ QCM measurements. After addition of 250 ppb SO 2 to the moist gas stream an increase of the formed feature's volume on the silver surface could be observed by TM-AFM measurements. The results obtained additionally from the in situ QCM measurements confirm the influence of SO 2 due to a further increase of the mass of the formed corrosion layer (and therefore an increase of the

  17. Insight into mechanics of AFM tip-based nanomachining: bending of cantilevers and machined grooves.

    PubMed

    Al-Musawi, R S J; Brousseau, E B; Geng, Y; Borodich, F M

    2016-09-23

    Atomic force microscope (AFM) tip-based nanomachining is currently the object of intense research investigations. Values of the load applied to the tip at the free end of the AFM cantilever probe used for nanomachining are always large enough to induce plastic deformation on the specimen surface contrary to the small load values used for the conventional contact mode AFM imaging. This study describes an important phenomenon specific for AFM nanomachining in the forward direction: under certain processing conditions, the deformed shape of the cantilever probe may change from a convex to a concave orientation. The phenomenon can principally change the depth and width of grooves machined, e.g. the grooves machined on a single crystal copper specimen may increase by 50% on average following such a change in the deformed shape of the cantilever. It is argued that this phenomenon can take place even when the AFM-based tool is operated in the so-called force-controlled mode. The study involves the refined theoretical analysis of cantilever probe bending, the analysis of experimental signals monitored during the backward and forward AFM tip-based machining and the inspection of the topography of produced grooves. PMID:27532247

  18. AFM/CLSM data visualization and comparison using an open-source toolkit.

    PubMed

    Rajwa, Bartek; McNally, Helen A; Varadharajan, Padma; Sturgis, Jennifer; Robinson, J Paul

    2004-06-01

    There is a vast difference in the traditional presentation of AFM data and confocal data. AFM data are presented as surface contours while confocal data are usually visualized using either surface- or volume-rendering techniques. Finding a common meaningful visualization platform is not an easy task. AFM and CLSM technologies are complementary and are more frequently being used to image common biological systems. In order to provide a presentation method that would assist us in evaluating cellular morphology, we propose a simple visualization strategy that is comparative, intuitive, and operates within an open-source environment of ImageJ, SurfaceJ, and VolumeJ applications. In order to find some common ground for AFM-CLSM image comparison, we have developed a plug-in for ImageJ, which allows us to import proprietary image data sets into this application. We propose to represent both AFM and CLSM image data sets as shaded elevation maps with color-coded height. This simple technique utilizes the open source VolumeJ and SurfaceJ plug-ins. To provide an example of this visualization technique, we evaluated the three-dimensional architecture of living chick dorsal root ganglia and sympathetic ganglia measured independently with AFM and CLSM. PMID:15352089

  19. Probing ternary solvent effect in high Voc polymer solar cells using advanced AFM techniques

    DOE PAGESBeta

    Li, Chao; Soleman, Mikhael; Lorenzo, Josie; Dhasmana, Nitesh; Chantharasupawong, Panit; Ievlev, Anton; Gesquiere, Andre; Tetard, Laurene; Thomas, Jayan

    2016-01-25

    This work describes a simple method to develop a high Voc low band gap PSCs. In addition, two new atomic force microscopy (AFM)-based nanoscale characterization techniques to study the surface morphology and physical properties of the structured active layer are introduced. With the help of ternary solvent processing of the active layer and C60 buffer layer, a bulk heterojunction PSC with Voc more than 0.9 V and conversion efficiency 7.5% is developed. In order to understand the fundamental properties of the materials ruling the performance of the PSCs tested, AFM-based nanoscale characterization techniques including Pulsed-Force-Mode AFM (PFM-AFM) and Mode-Synthesizing AFMmore » (MSAFM) are introduced. Interestingly, MSAFM exhibits high sensitivity for direct visualization of the donor–acceptor phases in the active layer of the PSCs. Lastly, conductive-AFM (cAFM) studies reveal local variations in conductivity in the donor and acceptor phases as well as a significant increase in photocurrent in the PTB7:ICBA sample obtained with the ternary solvent processing.« less

  20. In Situ TEM Nanoindentation Studies on Stress-Induced Phase Transformations in Metallic Materials

    DOE PAGESBeta

    Liu, Y.; Wang, H.; Zhang, X.

    2015-11-30

    Though abundant phase transformations are in general thermally driven processes, there are many examples wherein stresses can induce phase transformations. We applied numerous in situ techniques, such as in situ x-ray diffraction and neutron diffraction in order to reveal phase transformations. Recently, an in situ nanoindentation technique coupled with transmission electron microscopy demonstrated the capability to directly correlating stresses with phase transformations and microstructural evolutions at a submicron length scale. We briefly review in situ studies on stress-induced diffusional and diffusionless phase transformations in amorphous CuZrAl alloy and NiFeGa shape memory alloy. Moreover, in the amorphous CuZrAl, in situ nanoindentationmore » studies show that the nucleation of nanocrystals (a diffusional process) occurs at ultra-low stresses manifested by a prominent stress drop. In the NiFeGa shape memory alloy, two distinctive types of martensitic (diffusionless) phase transformations accompanied by stress plateaus are observed, including a reversible gradual phase transformation at low stress levels, and an irreversible abrupt phase transition at higher stress levels.« less

  1. Characterization of Microstructure and Mechanical Properties of High Chromium Cast Irons Using SEM and Nanoindentation

    NASA Astrophysics Data System (ADS)

    Chen, Ling; Iyengar, Srinivasan; Zhou, Jinming; Turba, Krystof; Ståhl, Jan-Eric

    2015-01-01

    The effects of composition changes and heat treatment on the microstructure and mechanical properties of high-chromium white cast irons were studied in order to characterize possible improvements in product performance and machinability. Materials characterization was performed using nanoindentation, SEM, and EDS techniques. Present results show that changes in carbon and silicon contents as well as heat treatment strongly affect the mechanical properties and their variation in the material. In the as-cast condition, the sample with relatively lower carbon and silicon contents has an austenite-martensite matrix and is much harder than the sample with relatively higher carbon and silicon contents having more eutectic carbides in a bainite matrix. Annealing leads to softening of the materials relative to the as-cast condition, with the relatively higher carbon-silicon material being marginally harder due to the presence of more eutectic carbides. A similar trend is seen after the hardening treatment, and the presence of primary carbide can restrict the extent of hardening due to the loss of alloying elements from the matrix.

  2. Influence of roughness and tilt on nanoindentation measurements: A quantitative model.

    PubMed

    Laurent-Brocq, Mathilde; Béjanin, Estelle; Champion, Yannick

    2015-01-01

    A model, which takes into account the indentation size effect, was proposed to relate hardness and its standard deviation to the quality of the sample surface, i.e., the roughness and the tilt. Stainless steel samples were mechanically polished so as to obtain various roughness and tilt. Then the quality of the surface and the hardness were measured respectively by scanning probe microscopy and by nanoindentation. The model was fitted according to those experimental data. It was shown that the standard deviation only depends on the ratio of the arithmetic roughness over the contact depth of the indent while the average hardness also depends on the contact depth and on the tilt. It was deduced that hardness measurements are performed with an uncertainty lower than 10% if: (i) the ratio of the arithmetic roughness over the contact depth of the indent is lower than 0.05, (ii) the tilt of the sample is lower than 2° and (iii) the difference of roughness between samples is lower than 50%. PMID:25931233

  3. Application of nanoindentation testing to study of the interfacial transition zone in steel fiber reinforced mortar

    SciTech Connect

    Wang Xiaohui Jacobsen, Stefan; He Jianying; Zhang Zhiliang; Lee, Siaw Foon; Lein, Hilde Lea

    2009-08-15

    The characteristics of the profiles of elastic modulus and hardness of the steel fiber-matrix and fiber-matrix-aggregate interfacial zones in steel fiber reinforced mortars have been investigated by using nanoindentation and Scanning Electron Microscopy (SEM), where two sets of parameters, i.e. water/binder ratio and content of silica fume were considered. Different interfacial bond conditions in the interfacial transition zones (ITZ) are discussed. For sample without silica fume, efficient interfacial bonds across the steel fiber-matrix and fiber-matrix-aggregate interfaces are shown in low water/binder ratio mortar; while in high water/binder ratio mortar, due to the discontinuous bleeding voids underneath the fiber, the fiber-matrix bond is not very good. On the other hand, for sample with silica fume, the addition of 10% silica fume leads to no distinct presence of weak ITZ in the steel fiber-matrix interface; but the effect of the silica fume on the steel fiber-matrix-aggregate interfacial zone is not obvious due to voids in the vicinity of steel fiber.

  4. Nanoindentations on conch shells of Gastropoda and Bivalvia molluscs reveal anisotropic evolution against external attacks.

    PubMed

    Bignardi, Cristina; Petraroli, Michele; Pugno, Nicola M

    2010-10-01

    Nanoindentation method has been used to explore, at the nanoscale, the mechanical properties of four different representative types of conch shells belonging to the two biggest classes of molluscs, Gastropoda and Bivalvia, in order to compare nanohardness and Young's modulus with respect to the microstructural anisotropic architectures. For the experimental tests a Nano Indenter XP (MTS Nano Instruments, Oak Ridge TN) has been used. The mechanical tests have been carried out on the inner and outer surfaces of the shells, as well as on their cross-section, near to the inner/outer surfaces and in the middle layer. The results confirm the three layered anisotropic architecture of the investigated conchs. On each of these 5 surfaces, 2 x 5 indentations have been performed at different maximum depth: from 250 nm to 4 microm, with a step of 250 nm, for a total of 3200 tests. The numerous observations have been analysed applying an ad hoc modification of the Weibull Statistics, suggesting a natural evolution of the shells against external attacks. PMID:21137746

  5. Evaluating fundamental position-dependent differences in wood cell wall adhesion using nanoindentation

    PubMed Central

    Obersriebnig, Michael; Konnerth, Johannes; Gindl-Altmutter, Wolfgang

    2013-01-01

    Spruce wood specimens were bonded with one-component polyurethane (PUR) and urea-formaldehyde (UF) adhesive, respectively. The adhesion of the adhesives to the wood cell wall was evaluated at two different locations by means of a new micromechanical assay based on nanoindentation. One location tested corresponded to the interface between the adhesive and the natural inner cell wall surface of the secondary cell wall layer 3 (S3), whereas the second location corresponded to the interface between the adhesive and the freshly cut secondary cell wall layer 2 (S2). Overall, a trend towards reduced cell wall adhesion was found for PUR compared to UF. Position-resolved examination revealed excellent adhesion of UF to freshly cut cell walls (S2) but significantly diminished adhesion to the inner cell wall surface (S3). In contrast, PUR showed better adhesion to the inner cell wall surface and less adhesion to freshly cut cell walls. Atomic force microscopy revealed a less polar character for the inner cell wall surface (S3) compared to freshly cut cell walls (S2). It is proposed that differences in the polarity of the used adhesives and the surface chemistry of the two cell wall surfaces examined account for the observed trends.

  6. Serrated flow behaviors of a Zr-based bulk metallic glass by nanoindentation

    SciTech Connect

    Cheng, L.; Jiao, Z. M.; Ma, S. G.; Wang, Z. H. E-mail: wangzhihua@tyut.edu.cn; Qiao, J. W. E-mail: wangzhihua@tyut.edu.cn

    2014-02-28

    Instrumented nanoindentation tests were used to investigate the mechanical properties of Zr{sub 52.5}Cu{sub 17.9}Ni{sub 14.6}Al{sub 10}Ti{sub 5} bulk metallic glass. The corresponding loading strain rates were ranged from 0.002 s{sup −1}, 0.02 s{sup −1} to 0.2 s{sup −1}. Plastic flow of this material exhibited remarkable serrations at low strain rates and increasingly became weakening until disappearance with increasing indentation strain rate, implying strong rate sensitivity. A significant pile-up around the indents was observed through atomic force microscopy, which suggested a highly localized plastic deformation. Mechanism governing the deformation was tentatively discussed in terms of the increasing process of free volume with a negligible temperature rise under low strain rate, which well explained the declining trend of elastic modulus and hardness with an increase of indentation depth.

  7. Mechanical characterization of several ion-implanted alloys: nanoindentation testing, wear testing and finite element modeling

    NASA Astrophysics Data System (ADS)

    Bourcier, R. J.; Follstaedt, D. M.; Dugger, M. T.; Myers, S. M.

    1991-07-01

    The influence of ion implantation on the mechanical properties of metal alloys has been examined using a variety of experimental and numerical techniques. Ultralow load indentation testing and finite element modeling has been used for the aluminum/oxygen to extract fundamental mechanical properties. Aluminum implanted with 20 at.% O exhibits extraordinary strength, as high as 3300 MPa. The degree of strengthening expected for this Al(O) alloy on the basis of the observed microstructure of fine (1.5-3.5 nm) oxide precipitates was estimated using several micromechanical models, and the results agree with our experimental findings. Pin-on-disk tribological characterization of aluminum implanted with 10 at.% oxygen revealed that the ion-beam treatment reduced the average friction coefficient from greater than 1.0 (for pure Al) to approximately 0.25 (for Al(O)). Large-amplitude stick-slip oscillations, which occur within the first two cycles for pure aluminum, were postponed to 30-50 cycles for the ion-implanted material. Two stainless steels which have been amorphized by implantation, 304 implanted with C and 440C implanted with Ti + C, show measurable hardening with implantation, of the order of 40 and 15%, respectively. In addition, nanoindentation within pin-on-disk wear tracks on 440C reveals that the mechanical state of the extensively deformed implanted layer is apparently unchanged from its initial state.

  8. Slow positron beam and nanoindentation study of irradiation-related defects in reactor vessel steels

    NASA Astrophysics Data System (ADS)

    Liu, Xiangbing; Wang, Rongshan; Jiang, Jing; Wu, Yichu; Zhang, Chonghong; Ren, Ai; Xu, Chaoliang; Qian, Wangjie

    2014-08-01

    In order to understand the nature of the hardening after radiation in reactor vessel steels, China A508-3 steels were implanted by proton with an energy of 240 keV up to 2.5 × 1016, 5.5 × 1016, 1.1 × 1017, and 2.5 × 1017 ions cm-2, respectively. Vacancy type defects were detected by energy-variable positron beam Doppler broadening technique and then nanoindentation measurements were performed to investigate proton-induced hardening effects. The results showed that S-parameter increased as a function of positron incident energy after irradiation, and the increasing rate of the S-parameter near the surface was larger than that in the bulk due to radiation damage. The size of vacancy type defects increased with dose. Irradiation induced hardening was shown that the average hardness increased with dose. Moreover a direct correlation between positron annihilation parameter and hardness was found based on Kasada method.

  9. Nanoindentation investigation of heavy ion irradiated Ti 3(Si,Al)C 2

    NASA Astrophysics Data System (ADS)

    Liu, X. M.; Le Flem, M.; Béchade, J. L.; Monnet, I.

    2010-06-01

    Because of good damage tolerance, thermal stability and interesting mechanical properties, Ti 3SiC 2, belonging to M n+1AX n phases, has been considered as a potential candidate material for applications in the future Gas Fast nuclear Reactors (GFR) such as components of fuel cladding working between 500 °C and 800 °C. However, the outstanding mechanical properties of Ti 3SiC 2 related to a layered microstructure could be impacted by irradiation. In this work, high energy Kr and Xe ion irradiated Ti 3Si 0.95Al 0.05C 2 and Ti 3Si 0.90Al 0.10C 2 samples, provided by IMR Shenyang, Chinese Academy of Science, were characterized by nanoindentation technique. After irradiation at room temperature, an increase in hardness with irradiation dose was highlighted. Nevertheless, some damage tolerance remained because of preservation of the typical MAX layered structure. Irradiations at 300 °C and 500 °C lead to less significant increase suggesting irradiation defect annealing. A complete recovery of the properties at 800 °C seems to be obtained.

  10. Mechanical Deformation Behavior of Nonpolar GaN Thick Films by Berkovich Nanoindentation

    PubMed Central

    2009-01-01

    In this study, the deformation mechanisms of nonpolar GaN thick films grown on m-sapphire by hydride vapor phase epitaxy (HVPE) are investigated using nanoindentation with a Berkovich indenter, cathodoluminescence (CL), and Raman microscopy. Results show that nonpolar GaN is more susceptible to plastic deformation and has lower hardness thanc-plane GaN. After indentation, lateral cracks emerge on the nonpolar GaN surface and preferentially propagate parallel to the orientation due to anisotropic defect-related stresses. Moreover, the quenching of CL luminescence can be observed to extend exclusively out from the center of the indentations along the orientation, a trend which is consistent with the evolution of cracks. The recrystallization process happens in the indented regions for the load of 500 mN. Raman area mapping indicates that the distribution of strain field coincides well with the profile of defect-expanded dark regions, while the enhanced compressive stress mainly concentrates in the facets of the indentation. PMID:20596453

  11. Nanoindentation hardness and adhesion investigations of vapor deposited nanostructured diamond films

    NASA Astrophysics Data System (ADS)

    Catledge, Shane A.; Borham, James; Vohra, Yogesh K.; Lacefield, William R.; Lemons, Jack E.

    2002-04-01

    The effect of changing the N2/CH4 feedgas ratio on the structure and mechanical properties of microwave plasma chemical vapor deposited diamond films grown on Ti-6Al-4V alloy substrates was investigated. The relative concentration of CH4 and N2 (in a balance of H2) was shown to strongly influence film structure, hardness, and adhesion. For high CH4 concentration (15% by volume), nanostructured diamond films with roughness magnitudes of 15-30 nm, good adhesion and a high hardness value of 90 GPa was obtained. A distinct correlation was found between the nanoindentation hardness of the deposited film and the N2/CH4 ratio in the plasma, as well as a correlation of hardness to the ratio of the Raman peak intensities (1332 and 1555 cm-1). Scratch adhesion testing of nanostructured diamond films showed delamination at a critical force of 33 N using acoustic emission techniques. These results demonstrate that nanostructured diamond films can be tailored on metallic surfaces with hardness ranging from 10 GPa (medium-hard) to 100 GPa (superhard) and may be considered for wear resistant applications such as in the design of articulating medical implant devices.

  12. Nanoindentation study of the mechanical behavior of TiO{sub 2} nanotube arrays

    SciTech Connect

    Xu, Y. N.; Wang, M. C.; Oloyede, A.; Bell, J. M.; Yan, C.; Liu, M. N.

    2015-10-14

    Titanium dioxide (TiO{sub 2}) nanotube arrays are attracting increasing attention for use in solar cells, lithium-ion batteries, and biomedical implants. To take full advantage of their unique physical properties, such arrays need to maintain adequate mechanical integrity in applications. However, the mechanical performance of TiO{sub 2} nanotube arrays is not well understood. In this work, we investigate the deformation and failure of TiO{sub 2} nanotube arrays using the nanoindentation technique. We found that the load–displacement response of the arrays strongly depends on the indentation depth and indenter shape. Substrate-independent elastic modulus and hardness can be obtained when the indentation depth is less than 2.5% of the array height. The deformation mechanisms of TiO{sub 2} nanotube arrays by Berkovich and conical indenters are closely associated with the densification of TiO{sub 2} nanotubes under compression. A theoretical model for deformation of the arrays under a large-radius conical indenter is also proposed.

  13. Volumetric and timescale analysis of phase transformation in single-crystal silicon during nanoindentation

    NASA Astrophysics Data System (ADS)

    Huang, Hu; Yan, Jiwang

    2016-06-01

    Clarifying the phase transformation process and mechanism of single-crystal silicon induced by high pressure is essential for preparation of new silicon phases. Although many previous researches have focused in this area, the volume of high-pressure phases and the duration of phase transformation are still unclear. In this paper, the volume change and the duration of phase transformation from Si-II phase into Si-XII/Si-III phases were investigated quantitatively by introducing a holding process in the unloading stage of a nanoindentation test. Experimental results indicate that the high-pressure phase volume is dependent strongly on the maximum indentation load and independent of the loading/unloading rate and the holding time at the maximum indentation load, while phase transformation duration is independent of the aforementioned experimental parameters. By analyzing the results, a critical volume of Si-XII/Si-III phases was identified which determines the occurrence of sudden phase transformation, and a modified nucleation and growth mechanism of high-pressure phases was proposed. These results provide new insights into high-pressure phase transformations in single-crystal silicon.

  14. Bi-stability of amplitude modulation AFM in air: deterministic and stochastic outcomes for imaging biomolecular systems.

    PubMed

    Santos, Sergio; Barcons, Victor; Font, Josep; Thomson, Neil H

    2010-06-01

    The dynamics of the oscillating microcantilever for amplitude modulation atomic force microscopy (AM AFM) operating in air is well understood theoretically but the experimental outcomes are still emerging. We use double-stranded DNA on mica as a model biomolecular system for investigating the connection between theory and experiment. A demonstration that the switching between the two cantilever oscillation states is stochastic in nature is achieved, and it can be induced by means of topographical anomalies on the surface. Whether one or the other attractor basin is accessed depends on the tip-sample separation history used to achieve the imaging conditions, and we show that the behaviour is reproducible when the tip is stable and well characterized. Emergence of background noise occurs in certain regions of parameter space regardless of whether two cantilever oscillation states coexist. The low state has been explored in detail and we note that at low to intermediate values of the free amplitude, noise-free imaging is achieved. The outcomes shown here are general and demonstrate that a thorough and systematic experimental approach in conjunction with standard modelling gives insight into the mechanisms behind image contrast formation in AM AFM in air. PMID:20453275

  15. An investigation using atomic force microscopy nanoindentation of dental enamel demineralization as a function of undissociated acid concentration and differential buffer capacity

    NASA Astrophysics Data System (ADS)

    Barbour, Michele E.; Shellis, R. Peter

    2007-02-01

    Acidic drinks and foodstuffs can demineralize dental hard tissues, leading to a pathological condition known as dental erosion, which is of increasing clinical concern. The first step in enamel dissolution is a demineralization of the outer few micrometres of tissue, which results in a softening of the structure. The primary determinant of dissolution rate is pH, but the concentration of undissociated acid, which is related to buffer capacity, also appears to be important. In this study, atomic force microscopy nanoindentation was used to measure the first initial demineralization (softening) induced within 1 min by exposure to solutions with a range of undissociated acid concentration and natural pH of 3.3 or with an undissociated acid concentration of 10 mmol l-1 and pH adjusted to 3.3. The results indicate that differential buffering capacity is a better determinant of softening than undissociated acid concentration. Under the conditions of these experiments, a buffer capacity of >3 mmol l-1 pH-1 does not have any further effect on dissolution rate. These results imply that differential buffering capacity should be used for preference over undissociated acid concentration or titratable acidity, which are more commonly employed in the literature.

  16. Improving the Lateral Resolution of Quartz Tuning Fork-Based Sensors in Liquid by Integrating Commercial AFM Tips into the Fiber End

    PubMed Central

    Gonzalez, Laura; Martínez-Martín, David; Otero, Jorge; de Pablo, Pedro José; Puig-Vidal, Manel; Gómez-Herrero, Julio

    2015-01-01

    The use of quartz tuning fork sensors as probes for scanning probe microscopy is growing in popularity. Working in shear mode, some methods achieve a lateral resolution comparable with that obtained with standard cantilevered probes, but only in experiments conducted in air or vacuum. Here, we report a method to produce and use commercial AFM tips in electrically driven quartz tuning fork sensors operating in shear mode in a liquid environment. The process is based on attaching a standard AFM tip to the end of a fiber probe which has previously been sharpened. Only the end of the probe is immersed in the buffer solution during imaging. The lateral resolution achieved is about 6 times higher than that of the etched microfiber on its own. PMID:25594596

  17. Nanoindentation study of niobium nitride thin films on niobium fabricated by reactive pulsed laser deposition

    SciTech Connect

    Mamun, Md Abdullah Al; Farha, Ashraf Hassan; Ufuktepe, Yüksel; Elsayed-Ali, Hani E.; Elmustafa, Abdelmageed A.

    2015-03-01

    Nanomechanical and structural properties of NbNx films deposited on single crystal Nb using pulsed laser deposition for different substrate temperature were previously investigated as a function of film/substrate crystal structure (Mamun et al. (2012) [30]). In this study we focus on the effect of laser fluences and background nitrogen pressure on the nanomechanical and structural properties of NbNx films. The crystal structure and surface morphology of the thin films were tested by X-ray diffraction, scanning electron microscopy, and atomic force microscopy. Using nanoindentation, the investigation of the nanomechanical properties revealed that the hardness of the NbNx films was directly influenced by the laser fluence for low background nitrogen pressure, whereas the nanomechanical hardness showed no apparent correlation with laser fluence at high background nitrogen pressure. The NbNx film hardness measured at 30% film thickness increased from 14.0 ± 1.3 to 18.9 ± 2.4 GPa when the laser fluence was increased from 15 to 25 J/cm2 at 10.7 Pa N2 pressure. X-ray diffraction showed NbNx films with peaks that correspond to δ-NbN cubic and β-Nb2N hexagonal phases in addition to the δ'-NbN hexagonal phase. Finally, increasing the laser fluence resulted in NbNx films with larger grain sizes.

  18. Mechanobiological Assessment of TMJ Disc Surfaces: Nanoindentation and Transmission Electron Microscopy

    PubMed Central

    Juran, Cassandra M.; Dolwick, M. Franklin

    2015-01-01

    ABSTRACT Objectives Temporomandibular disc is a mechanically robust fibrocartilage tissue exhibiting highly elastic compressive, shear, and tensile moduli with structurally dense extracellular matrix that supports functional loading of the joint. The aim of this study was to illustrate structural complexities of the superior and inferior disc surfaces, to demonstrate the robust mechanical ability of the disc as a whole may be due to depth-dependent regional/layered variation, and also to provide characterization data imperative for future tissue engineering efforts focused on restoring function to the joint. Material and Methods Nanoindentation was used to assess tissue zones in conjunction with detailed Transmission Electron Microscopy to define structural attributes that influence the temporomandibular disc function. Results The disc architecture adjacent to the superior surface was shown to have three distinct regional segments within the interface layer: 1-a surface peripheral layer; 2-subsurface region; and 3-a layer of helical matrix bundles. The inferior surface displayed an interface layer (20 µm) that showed limited cell populations with little depth-dependent structural variation, a stiffer elastic modulus and reduced energy dissipation compared to the superior surface. These data indicate that the primary function of the inferior surface is resistance to compression rather than load distribution during joint motion. Conclusions These are the first works that demonstrate that the superior central surface of the he temporomandibular disc is structured in depth-dependent isometric layers, each of which provides different mechanical function supporting the bulk tissue’s properties. From a clinical perspective these data have potential to define regions susceptible to fatigue that may translate to diagnostic criteria to better define the stages of dysfunction. PMID:26904180

  19. Measurement of fracture toughness by nanoindentation methods: Recent advances and future challenges

    DOE PAGESBeta

    Sebastiani, Marco; Johanns, K. E.; Herbert, Erik G.; Pharr, George M.

    2015-04-30

    In this study, we describe recent advances and developments for the measurement of fracture toughness at small scales by the use of nanoindentation-based methods including techniques based on micro-cantilever beam bending and micro-pillar splitting. A critical comparison of the techniques is made by testing a selected group of bulk and thin film materials. For pillar splitting, cohesive zone finite element simulations are used to validate a simple relationship between the critical load at failure, the pillar radius, and the fracture toughness for a range of material properties and coating/substrate combinations. The minimum pillar diameter required for nucleation and growth ofmore » a crack during indentation is also estimated. An analysis of pillar splitting for a film on a dissimilar substrate material shows that the critical load for splitting is relatively insensitive to the substrate compliance for a large range of material properties. Experimental results from a selected group of materials show good agreement between single cantilever and pillar splitting methods, while a discrepancy of ~25% is found between the pillar splitting technique and double-cantilever testing. It is concluded that both the micro-cantilever and pillar splitting techniques are valuable methods for micro-scale assessment of fracture toughness of brittle ceramics, provided the underlying assumptions can be validated. Although the pillar splitting method has some advantages because of the simplicity of sample preparation and testing, it is not applicable to most metals because their higher toughness prevents splitting, and in this case, micro-cantilever bend testing is preferred.« less

  20. Measurement of fracture toughness by nanoindentation methods: Recent advances and future challenges

    SciTech Connect

    Sebastiani, Marco; Johanns, K. E.; Herbert, Erik G.; Pharr, George M.

    2015-04-30

    In this study, we describe recent advances and developments for the measurement of fracture toughness at small scales by the use of nanoindentation-based methods including techniques based on micro-cantilever beam bending and micro-pillar splitting. A critical comparison of the techniques is made by testing a selected group of bulk and thin film materials. For pillar splitting, cohesive zone finite element simulations are used to validate a simple relationship between the critical load at failure, the pillar radius, and the fracture toughness for a range of material properties and coating/substrate combinations. The minimum pillar diameter required for nucleation and growth of a crack during indentation is also estimated. An analysis of pillar splitting for a film on a dissimilar substrate material shows that the critical load for splitting is relatively insensitive to the substrate compliance for a large range of material properties. Experimental results from a selected group of materials show good agreement between single cantilever and pillar splitting methods, while a discrepancy of ~25% is found between the pillar splitting technique and double-cantilever testing. It is concluded that both the micro-cantilever and pillar splitting techniques are valuable methods for micro-scale assessment of fracture toughness of brittle ceramics, provided the underlying assumptions can be validated. Although the pillar splitting method has some advantages because of the simplicity of sample preparation and testing, it is not applicable to most metals because their higher toughness prevents splitting, and in this case, micro-cantilever bend testing is preferred.

  1. Viscoelastic properties of cell walls of single living plant cells determined by dynamic nanoindentation

    PubMed Central

    Hayot, Céline M.; Forouzesh, Elham; Goel, Ashwani; Avramova, Zoya; Turner, Joseph A.

    2012-01-01

    Plant development results from controlled cell divisions, structural modifications, and reorganizations of the cell wall. Thereby, regulation of cell wall behaviour takes place at multiple length scales involving compositional and architectural aspects in addition to various developmental and/or environmental factors. The physical properties of the primary wall are largely determined by the nature of the complex polymer network, which exhibits time-dependent behaviour representative of viscoelastic materials. Here, a dynamic nanoindentation technique is used to measure the time-dependent response and the viscoelastic behaviour of the cell wall in single living cells at a micron or sub-micron scale. With this approach, significant changes in storage (stiffness) and loss (loss of energy) moduli are captured among the tested cells. The results reveal hitherto unknown differences in the viscoelastic parameters of the walls of same-age similarly positioned cells of the Arabidopsis ecotypes (Col 0 and Ws 2). The technique is also shown to be sensitive enough to detect changes in cell wall properties in cells deficient in the activity of the chromatin modifier ATX1. Extensive computational modelling of the experimental measurements (i.e. modelling the cell as a viscoelastic pressure vessel) is used to analyse the influence of the wall thickness, as well as the turgor pressure, at the positions of our measurements. By combining the nanoDMA technique with finite element simulations quantifiable measurements of the viscoelastic properties of plant cell walls are achieved. Such techniques are expected to find broader applications in quantifying the influence of genetic, biological, and environmental factors on the nanoscale mechanical properties of the cell wall. PMID:22291130

  2. Nanoindentation analysis of αtricalcium phosphate-poly(lactide-co-glycolide) nanocomposite degradation.

    PubMed

    Barrett, C E; Cameron, R E

    2014-09-01

    The internal mechanical property characteristics as functions of position and degradation time of PLGA(50:50)-αTCP nanocomposites of varying ceramic-polymer ratios degraded in an aqueous medium have been assessed using depth-sensing nanoindentation. The addition of nanoparticulate αTCP increases the elastic modulus of undegraded specimens from 3.72 ± 0.12 GPa for pure PLGA(50:50) samples to 7.23 ± 0.16 GPa recorded for undegraded 40 wt.% TCP nanocomposites. Additionally αTCP incorporation decreases the viscoelastic loss tangent from 0.189 ± 0.040 measured for pure undegraded PLGA(50:50) to an average of 0.091 ± 0.006 for undegraded ceramic-polymer composites. No variation in viscosity for the composites with ceramic loading was evidenced. The stiffening effect of αTCP addition closely conforms to the lower Hashin-Shtrikman bounds demonstrating that an evenly dispersed nano-filler is the least amenable ceramic configuration to enhance the mechanical properties of PLGA-αTCP nanocomposites. The mechanical property evolution for all composite types in an aqueous degradation medium is dominated by material hydration which effects reduced material stiffness and increased specimen viscosity generating a core-periphery mechanical property distribution in terms of elastic modulus and viscoelastic phase angle. The mechanical property core-periphery structure correlates strongly with the core-periphery density structure characterized using X-ray microtomography. Hydrated regions exhibit significant reductions in elastic modulus and viscosity increases which are typical of elastomers. PMID:25063157

  3. Novel Way to Characterize Metal-Insulator-Metal Devices via Nanoindentation: Preprint

    SciTech Connect

    Periasamy, P.; Packard, C. E.; O?Hayre, R. P.; Berry, J. J.; Parilla, P. A.; Ginley, D. S.

    2011-07-01

    Metal-Insulator-Metal (MIM) devices are crucial components for applications ranging from optical rectennas for harvesting sunlight to infrared detectors. To date, the relationship between materials properties and device performance in MIM devices is not fully understood, partly due to the difficulty in making and reproducing reliable devices. One configuration that is popular due to its simplicity and ease of fabrication is the point-contact diode where a metal tip serves as one of the metals in the MIM device. The intrinsic advantage of the point-contact configuration is that it is possible to achieve very small contact areas for the device thereby allowing very high-frequency operation. In this study, precise control over the contact area and penetration depth of an electrically conductive tip into a metal/insulator combination is achieved using a nanoindenter with in-situ electrical contact resistance measurement capabilities. A diamond probe tip, doped (degeneratively) with boron for conductivity, serves as the point contact and second 'metal' (b-Diamond) of the MIM diode. The base layer consists of Nb/Nb2O5 thin films on Si substrates and serves as the first metal /insulator combination of the MIM structure. The current-voltage response of the diodes is measured under a range of conditions to assess the validity and repeatability of the technique. Additionally, we compare the results of this technique to those acquired using a bent-wire approach and find that Nb/Nb2O5/b-Diamond MIM devices show an excellent asymmetry (60-300) and nonlinearity values (~6-9). This technique shows great promise for screening metal-insulator combinations for performance without the uncertainty that stems from a typical bent-wire point-contact.

  4. Viscoelastic properties of cell walls of single living plant cells determined by dynamic nanoindentation.

    PubMed

    Hayot, Céline M; Forouzesh, Elham; Goel, Ashwani; Avramova, Zoya; Turner, Joseph A

    2012-04-01

    Plant development results from controlled cell divisions, structural modifications, and reorganizations of the cell wall. Thereby, regulation of cell wall behaviour takes place at multiple length scales involving compositional and architectural aspects in addition to various developmental and/or environmental factors. The physical properties of the primary wall are largely determined by the nature of the complex polymer network, which exhibits time-dependent behaviour representative of viscoelastic materials. Here, a dynamic nanoindentation technique is used to measure the time-dependent response and the viscoelastic behaviour of the cell wall in single living cells at a micron or sub-micron scale. With this approach, significant changes in storage (stiffness) and loss (loss of energy) moduli are captured among the tested cells. The results reveal hitherto unknown differences in the viscoelastic parameters of the walls of same-age similarly positioned cells of the Arabidopsis ecotypes (Col 0 and Ws 2). The technique is also shown to be sensitive enough to detect changes in cell wall properties in cells deficient in the activity of the chromatin modifier ATX1. Extensive computational modelling of the experimental measurements (i.e. modelling the cell as a viscoelastic pressure vessel) is used to analyse the influence of the wall thickness, as well as the turgor pressure, at the positions of our measurements. By combining the nanoDMA technique with finite element simulations quantifiable measurements of the viscoelastic properties of plant cell walls are achieved. Such techniques are expected to find broader applications in quantifying the influence of genetic, biological, and environmental factors on the nanoscale mechanical properties of the cell wall. PMID:22291130

  5. Microstructure and nanoindentation of the CLAM steel with nanocrystalline grains under Xe irradiation

    NASA Astrophysics Data System (ADS)

    Chang, Yongqin; Zhang, Jing; Li, Xiaolin; Guo, Qiang; Wan, Farong; Long, Yi

    2014-12-01

    This work presents an early look at irradiation effects on China low activation martensitic (CLAM) steel with nanocrystalline grains (NC-CLAM steels) under 500 keV Xe-ion bombardment at room temperature to doses up to 5.3 displacements per atom (dpa). The microstructure in the topmost region of the steel is composed of nanocrystalline grains with an average diameter of 13 nm. As the samples were implanted at low dose, the nanocrystalline grains had martensite lath structure, and many dislocations and high density bubbles were introduced into the NC-CLAM steels. As the irradiation dose up to 5.3 dpa, a tangled dislocation network exists in the lath region, and the size of the bubbles increases. X-ray diffraction results show that the crystal quality decreases after irradiation, although the nanocrystals obviously coarsen. Grain growth under irradiation may be ascribed to the direct impact of the thermal spike on grain boundaries in the NC-CLAM steels. In irradiated samples, a compressive stress exists in the surface layer because of grain growth and irradiation-introduced defects, while the irradiation introduced grain-size coarsening and defects gradients from the surface to matrix result in a tensile stress in the irradiated NC-CLAM steels. Nanoindentation was used to estimate changes in mechanical properties during irradiation, and the results show that the hardness of the NC-CLAM steels increases with increasing irradiation dose, which was ascribed to the competition between the grain boundaries and the irradiation-introduced defects.

  6. AFM as an analysis tool for high-capacity sulfur cathodes for Li-S batteries.

    PubMed

    Hiesgen, Renate; Sörgel, Seniz; Costa, Rémi; Carlé, Linus; Galm, Ines; Cañas, Natalia; Pascucci, Brigitta; Friedrich, K Andreas

    2013-01-01

    In this work, material-sensitive atomic force microscopy (AFM) techniques were used to analyse the cathodes of lithium-sulfur batteries. A comparison of their nanoscale electrical, electrochemical, and morphological properties was performed with samples prepared by either suspension-spraying or doctor-blade coating with different binders. Morphological studies of the cathodes before and after the electrochemical tests were performed by using AFM and scanning electron microscopy (SEM). The cathodes that contained polyvinylidene fluoride (PVDF) and were prepared by spray-coating exhibited a superior stability of the morphology and the electric network associated with the capacity and cycling stability of these batteries. A reduction of the conductive area determined by conductive AFM was found to correlate to the battery capacity loss for all cathodes. X-ray diffraction (XRD) measurements of Li2S exposed to ambient air showed that insulating Li2S hydrolyses to insulating LiOH. This validates the significance of electrical ex-situ AFM analysis after cycling. Conductive tapping mode AFM indicated the existence of large carbon-coated sulfur particles. Based on the analytical findings, the first results of an optimized cathode showed a much improved discharge capacity of 800 mA·g(sulfur)(-1) after 43 cycles. PMID:24205455

  7. Sub-surface imaging of carbon nanotube-polymer composites using dynamic AFM methods.

    PubMed

    Cadena, Maria J; Misiego, Rocio; Smith, Kyle C; Avila, Alba; Pipes, Byron; Reifenberger, Ron; Raman, Arvind

    2013-04-01

    High-resolution sub-surface imaging of carbon nanotube (CNT) networks within polymer nanocomposites is demonstrated through electrical characterization techniques based on dynamic atomic force microscopy (AFM). We compare three techniques implemented in the single-pass configuration: DC-biased amplitude modulated AFM (AM-AFM), electrostatic force microscopy (EFM) and Kelvin probe force microscopy (KPFM) in terms of the physics of sub-surface image formation and experimental robustness. The methods were applied to study the dispersion of sub-surface networks of single-walled nanotubes (SWNTs) in a polyimide (PI) matrix. We conclude that among these methods, the KPFM channel, which measures the capacitance gradient (∂C/∂d) at the second harmonic of electrical excitation, is the best channel to obtain high-contrast images of the CNT network embedded in the polymer matrix, without the influence of surface conditions. Additionally, we propose an analysis of the ∂C/∂d images as a tool to characterize the dispersion and connectivity of the CNTs. Through the analysis we demonstrate that these AFM-based sub-surface methods probe sufficiently deep within the SWNT composites, to resolve clustered networks that likely play a role in conductivity percolation. This opens up the possibility of dynamic AFM-based characterization of sub-surface dispersion and connectivity in nanostructured composites, two critical parameters for nanocomposite applications in sensors and energy storage devices. PMID:23478510

  8. Nanoscale crystallization of phase change Ge2Sb2Te5 film with AFM lithography.

    PubMed

    Kim, JunHo

    2010-01-01

    We have made nanoindents on Ge(2)Sb(2)Te(5)(GST) films using electric field-assisted atomic force microscope (AFM) lithography. GST shows increase of material density and electric conductivity as it changes from amorphous to crystalline phases. By applying electric field between AFM probe-tip and GST surface, nanoscale crystallization could be induced on tip contact area. As the crystallized GST exhibits increase of material density, that is to say depression of volume, nanoindented surface with crystallization is created on host amorphous GST (a-GST) film. For the AFM lithography, a highly conductive tip, which showed voltage-switching characteristics in current-voltage spectroscopy of GST film, was found to be very suitable for recording and sensing crystallized nanoindents on the GST film. By varying sample bias voltages, we performed nanoscale crystallization, and measured the nanostructured film in AFM conductance-image (C-image) mode and topography-image (T-image) mode, simultaneously. Two types of crystallized wires were fabricated on (a-GST) film. Type-I was sensed in only C-image, whereas Type-II was sensed in both C-image and T-image. These nanowires are discussed in terms of crystallization of GST and sensitivity of current (or topography) sensing. By repeated lithography, larger size of nanoindented wires were also produced, which indicates line-dimension controllability of AFM lithography. PMID:20853405

  9. AFM as an analysis tool for high-capacity sulfur cathodes for Li–S batteries

    PubMed Central

    Sörgel, Seniz; Costa, Rémi; Carlé, Linus; Galm, Ines; Cañas, Natalia; Pascucci, Brigitta; Friedrich, K Andreas

    2013-01-01

    Summary In this work, material-sensitive atomic force microscopy (AFM) techniques were used to analyse the cathodes of lithium–sulfur batteries. A comparison of their nanoscale electrical, electrochemical, and morphological properties was performed with samples prepared by either suspension-spraying or doctor-blade coating with different binders. Morphological studies of the cathodes before and after the electrochemical tests were performed by using AFM and scanning electron microscopy (SEM). The cathodes that contained polyvinylidene fluoride (PVDF) and were prepared by spray-coating exhibited a superior stability of the morphology and the electric network associated with the capacity and cycling stability of these batteries. A reduction of the conductive area determined by conductive AFM was found to correlate to the battery capacity loss for all cathodes. X-ray diffraction (XRD) measurements of Li2S exposed to ambient air showed that insulating Li2S hydrolyses to insulating LiOH. This validates the significance of electrical ex-situ AFM analysis after cycling. Conductive tapping mode AFM indicated the existence of large carbon-coated sulfur particles. Based on the analytical findings, the first results of an optimized cathode showed a much improved discharge capacity of 800 mA·g(sulfur)−1 after 43 cycles. PMID:24205455

  10. Enabling accurate gate profile control with inline 3D-AFM

    NASA Astrophysics Data System (ADS)

    Bao, Tianming; Lopez, Andrew; Dawson, Dean

    2009-05-01

    The logic and memory semiconductor device technology strives to follow the aggressive ITRS roadmap. The ITRS calls for increased 3D metrology to meet the demand for tighter process control at 45nm and 32nm nodes. In particular, gate engineering has advanced to a level where conventional metrology by CD-SEM and optical scatterometry (OCD) faces fundamental limitations without involvement of 3D atomic force microscope (3D-AFM or CD-AFM). This paper reports recent progress in 3D-AFM to address the metrology need to control gate dimension in MOSFET transistor formation. 3D-AFM metrology measures the gate electrode at post-etch with the lowest measurement uncertainty for critical gate geometry, including linewidth, sidewall profile, sidewall angle (SWA), line width roughness (LWR), and line edge roughness (LER). 3D-AFM enables accurate gate profile control in three types of metrology applications: reference metrology to validate CD-SEM and OCD, inline depth or 3D monitoring, or replacing TEM for 3D characterization for engineering analysis.

  11. Development of a new generation of active AFM tools for applications in liquids

    NASA Astrophysics Data System (ADS)

    Rollier, A.-S.; Jenkins, D.; Dogheche, E.; Legrand, B.; Faucher, M.; Buchaillot, L.

    2010-08-01

    Atomic force microscopy (AFM) is a powerful imaging tool with high-resolution imaging capability. AFM probes consist of a very sharp tip at the end of a silicon cantilever that can respond to surface artefacts to produce an image of the topography or surface features. They are intrinsically passive devices. For imaging soft biological samples, and also for samples in liquid, it is essential to control the AFM tip position, both statically and dynamically, and this is not possible using external actuators mounted on the AFM chip. AFM cantilevers have been fabricated using silicon micromachining to incorporate a piezoelectric thin film actuator for precise control. The piezoelectric thin films have been fully characterized to determine their actuation performance and to characterize the operation of the integrated device. Examples of the spatial and vertical response are presented to illustrate their imaging capability. For operation in a liquid environment, the dynamic behaviour has been modelled and verified experimentally. The optimal drive conditions for the cantilever, along with their dynamic response, including frequency and phase in air and water, are presented.

  12. AFM1 in Milk: Physical, Biological, and Prophylactic Methods to Mitigate Contamination

    PubMed Central

    Giovati, Laura; Magliani, Walter; Ciociola, Tecla; Santinoli, Claudia; Conti, Stefania; Polonelli, Luciano

    2015-01-01

    Aflatoxins (AFs) are toxic, carcinogenic, immunosuppressive secondary metabolites produced by some Aspergillus species which colonize crops, including many dietary staple foods and feed components. AFB1 is the prevalent and most toxic among AFs. In the liver, it is biotransformed into AFM1, which is then excreted into the milk of lactating mammals, including dairy animals. AFM1 has been shown to be cause of both acute and chronic toxicoses. The presence of AFM1 in milk and dairy products represents a worldwide concern since even small amounts of this metabolite may be of importance as long-term exposure is concerned. Contamination of milk may be mitigated either directly, decreasing the AFM1 content in contaminated milk, or indirectly, decreasing AFB1 contamination in the feed of dairy animals. Current strategies for AFM1 mitigation include good agricultural practices in pre-harvest and post-harvest management of feed crops (including storage) and physical or chemical decontamination of feed and milk. However, no single strategy offers a complete solution to the issue. PMID:26512694

  13. The physics of pulling polyproteins: a review of single molecule force spectroscopy using the AFM to study protein unfolding

    NASA Astrophysics Data System (ADS)

    Hughes, Megan L.; Dougan, Lorna

    2016-07-01

    One of the most exciting developments in the field of biological physics in recent years is the ability to manipulate single molecules and probe their properties and function. Since its emergence over two decades ago, single molecule force spectroscopy has become a powerful tool to explore the response of biological molecules, including proteins, DNA, RNA and their complexes, to the application of an applied force. The force versus extension response of molecules can provide valuable insight into its mechanical stability, as well as details of the underlying energy landscape. In this review we will introduce the technique of single molecule force spectroscopy using the atomic force microscope (AFM), with particular focus on its application to study proteins. We will review the models which have been developed and employed to extract information from single molecule force spectroscopy experiments. Finally, we will end with a discussion of future directions in this field.

  14. AFM-based force spectroscopy measurements of mature amyloid fibrils of the peptide glucagon

    NASA Astrophysics Data System (ADS)

    Dong, Mingdong; Bruun Hovgaard, Mads; Mamdouh, Wael; Xu, Sailong; Otzen, Daniel Erik; Besenbacher, Flemming

    2008-09-01

    We report on the mechanical characterization of individual mature amyloid fibrils by atomic force microscopy (AFM) and AFM-based single-molecule force spectroscopy (SMFS). These self-assembling materials, formed from the 29-residue amphiphatic peptide hormone glucagon, were found to display a reversible elastic behaviour. Based on AFM morphology and SMFS studies, we suggest that the observed elasticity is due to a force-induced conformational transition which is reversible due to the β-helical conformation of protofibrils, allowing a high degree of extension. The elastic properties of such mature fibrils contribute to their high stability, suggesting that the internal hydrophobic interactions of amyloid fibrils are likely to be of fundamental importance in the assembly of amyloid fibrils and therefore for the understanding of the progression of their associated pathogenic disorders. In addition, such biological amyloid fibril structures with highly stable mechanical properties can potentially be used to produce nanofibres (nanowires) that may be suitable for nanotechnological applications.

  15. AFM-assisted fabrication of thiol SAM pattern with alternating quantified surface potential

    PubMed Central

    2011-01-01

    Thiol self-assembled monolayers (SAMs) are widely used in many nano- and bio-technology applications. We report a new approach to create and characterize a thiol SAMs micropattern with alternating charges on a flat gold-coated substrate using atomic force microscopy (AFM) and Kelvin probe force microscopy (KPFM). We produced SAMs-patterns made of alternating positively charged, negatively charged, and hydrophobic-terminated thiols by an automated AFM-assisted manipulation, or nanografting. We show that these thiol patterns possess only small topographical differences as revealed by AFM, and distinguished differences in surface potential (20-50 mV), revealed by KPFM. The pattern can be helpful in the development of biosensor technologies, specifically for selective binding of biomolecules based on charge and hydrophobicity, and serve as a model for creating surfaces with quantified alternating surface potential distribution. PMID:21711703

  16. A sub-50 nm three-step height sample for AFM calibration

    NASA Astrophysics Data System (ADS)

    Yang, Shuming; Li, Changsheng; Wang, Chenying; Jiang, Zhuangde

    2014-12-01

    In this paper, a sub-50 nm three-step height sample was made for vertical calibration of atomic force microscopy (AFM) and a new step height evaluation algorithm based on polynomial fitting is discussed. The influences of AFM artefacts such as particles, image bow and high-order errors on step height were studied. The experimental results showed that the polynomial order p2 and threshold t were not critical factors. However, the increment Δh and the polynomial order p used in the calculation of optimal shifting distance were important and must be carefully considered. Δh = 0.1 nm and p ≥ 4 were determined to get a stable step height. The sample had small roughness and good uniformity. It has the potential to serve as a high quality step height standard sample for AFM calibration.

  17. Review and perspectives of AFM application on the study of deformable drop/bubble interactions.

    PubMed

    Wang, Wei; Li, Kai; Ma, Mengyu; Jin, Hang; Angeli, Panagiota; Gong, Jing

    2015-11-01

    The applications of Atomic Force Microscopy (AFM) on the study of dynamic interactions and film drainage between deformable bodies dispersed in aqueous solutions are reviewed in this article. Novel experimental designs and recent advances in experimental methodologies are presented, which show the advantage of using AFM as a tool for probing colloidal interactions. The effects of both DLVO and non-DLVO forces on the colloid stabilization mechanism are discussed. Good agreement is found between the force - drop/bubble deformation behaviour revealed by AFM measurements and the theoretical modeling of film drainage process, giving a convincing explanation of the occurrence of certain phenomenon. However, the behaviour and shape of deformable drops as they approach or retract is still not well resolved. In addition, when surfactants are present further research is needed on the absorption of surfactant molecules into the interfaces, their mobility and the effects on interfacial film properties. PMID:26344865

  18. Imaging and force measurement of LDL and HDL by AFM in air and liquid

    PubMed Central

    Gan, Chaoye; Ao, Meiying; Liu, Zhanghua; Chen, Yong

    2015-01-01

    The size and biomechanical properties of lipoproteins are tightly correlated with their structures/functions. While atomic force microscopy (AFM) has been used to image lipoproteins the force measurement of these nano-sized particles is missing. We detected that the sizes of LDL and HDL in liquid are close to the commonly known values. The Young’s modulus of LDL or HDL is ∼0.4 GPa which is similar to that of some viral capsids or nanovesicles but greatly larger than that of various liposomes. The adhesive force of LDL or HDL is small (∼200 pN). The comparison of AFM detection in air and liquid was also performed which is currently lacking. Our data may provide useful information for better understanding and AFM detection of lipoproteins. PMID:25893163

  19. Mapping site-specific endonuclease binding to DNA by direct imaging with AFM

    SciTech Connect

    Allison, D.P.; Thundat, T.; Doktycz, M.J.; Kerper, P.S.; Warmack, R.J.; Modrich, P.; Isfort, R.J.

    1995-12-31

    Physical mapping of DNA can be accomplished by direct AFM imaging of site specific proteins bound to DNA molecules. Using Gln-111, a mutant of EcoRI endonuclease with a specific affinity for EcoRI sites 1,000 times greater than wild type enzyme but with cleavage rate constants reduced by a factor of 10{sup 4}, the authors demonstrate site-specific mapping by direct AFM imaging. Images are presented showing specific-site binding of Gln-111 to plasmids having either one (pBS{sup +}) or two (pMP{sup 32}) EcoRI sites. Identification of the Gln-111/DNA complex is greatly enhanced by biotinylation of the complex followed by reaction with streptavidin gold prior to imaging. Image enhancement coupled with improvements in the preparation techniques for imaging large DNA molecules, such as lambda DNA (47 kb), has the potential to contribute to direct AFM restriction mapping of cosmid-sized genomic DNAs.

  20. Multiparametric high-resolution imaging of native proteins by force-distance curve-based AFM.

    PubMed

    Pfreundschuh, Moritz; Martinez-Martin, David; Mulvihill, Estefania; Wegmann, Susanne; Muller, Daniel J

    2014-05-01

    A current challenge in the life sciences is to understand how the properties of individual molecular machines adjust in order to meet the functional requirements of the cell. Recent developments in force-distance (FD) curve-based atomic force microscopy (FD-based AFM) enable researchers to combine sub-nanometer imaging with quantitative mapping of physical, chemical and biological properties. Here we present a protocol to apply FD-based AFM to the multiparametric imaging of native proteins under physiological conditions. We describe procedures for experimental FD-based AFM setup, high-resolution imaging of proteins in the native unperturbed state with simultaneous quantitative mapping of multiple parameters, and data interpretation and analysis. The protocol, which can be completed in 1-3 d, enables researchers to image proteins and protein complexes in the native unperturbed state and to simultaneously map their biophysical and biochemical properties at sub-nanometer resolution. PMID:24743419

  1. AFM characterization of nonwoven material functionalized by ZnO sputter coating

    SciTech Connect

    Deng Bingyao; Yan Xiong; Wei Qufu Gao Weidong

    2007-10-15

    Sputter coatings provide new approaches to the surface functionalization of textile materials. In this study, polyethylene terephthalate (PET) nonwoven material was used as a substrate for creating functional nanostructures on the fiber surfaces. A magnetron sputter coating was used to deposit functional zinc oxide (ZnO) nanostructures onto the nonwoven substrate. The evolution of the surface morphology of the fibers in the nonwoven web was examined using atomic force microscopy (AFM). The AFM observations revealed a significant difference in the morphology of the fibers before and after the sputter coating. The AFM images also indicated the effect of the sputtering conditions on the surface morphology of the fibers. The increase in the sputtering time led to the growth of the ZnO grains on the fiber surfaces. The higher pressure in the sputtering chamber could cause the formation of larger grains on the fiber surfaces. The higher power used also generated larger grains on the fiber surfaces.

  2. High precision attachment of silver nanoparticles on AFM tips by dielectrophoresis.

    PubMed

    Leiterer, Christian; Wünsche, Erik; Singh, Prabha; Albert, Jens; Köhler, Johann M; Deckert, Volker; Fritzsche, Wolfgang

    2016-05-01

    AFM tips are modified with silver nanoparticles using an AC electrical field. The used technique works with sub-micron precision and also does not require chemical modification of the tip. Based on the electrical parameters applied in the process, particle density and particle position on the apex of the tip can be adjusted. The feasibility of the method is proven by subsequent tip-enhanced Raman spectroscopy (TERS) measurements using the fabricated tips as a measurement probe. Since this modification process itself does not require any lithographic processing, the technique can be easily adapted to modify AFM tips with a variety of nanostructures with pre-defined properties, while being parallelizable for a potential commercial application. Graphical abstract Silver nanoparticles attached to AFM tips using dielectrophoresis. Comparing nanoparticles attached using 1 kHz (left) to 1 MHz (right), SEM and optical (inset) images. PMID:26968565

  3. Scale effects in the convoluted thermal/spatial statistics of plasticity initiation in small stressed volumes during nanoindentation

    SciTech Connect

    Li, Tianlei; Bei, Hongbin; Morris, James R.; George, Easo P; Gao, Yanfei

    2012-01-01

    The elastic-plastic transition of crystals at small length scales can be quantitatively evaluated by the sudden discontinuities ( pop-ins ) on nanoindentation load-displacement curves. For defect-free crystals under nano-contacts, pop-in stress fluctuations result purely from the thermally activated process of homogeneous dislocation nucleation, while at intermediate contact sizes fluctuations can arise from the spatial statistics of pre-existing defects. Their convolution exhibits a distinct dependence on the stressed volume; the transition between these two is found to depend on dislocation density and crystallography.

  4. Nanoindentation Mechanical Properties of a Bi-phase Cu29Zr32Ti15Al5Ni19 Alloy

    NASA Astrophysics Data System (ADS)

    Pi, JinHong; Wang, ZhangZhong; He, XianCong; Bai, YunQiang

    2016-01-01

    Mechanical properties of cylindrical bi-phasic high-entropy alloy Cu29Zr32Ti15Al5Ni19 (3 mm in diameter) were characterized by nanoindentation test in each phase. The results show that the constituent FCC phase is of low nanohardness (2.35 GPa) and modulus (60.9 GPa), while another constituent phase in the alloy, the HCP phase, shows much higher nanohardness (6.5 GPa) and modulus (115.3 GPa). Creep occurs in both phases during the indentation.

  5. Indentation Schmid factor and orientation dependence of nanoindentation pop-in behavior of NiAl single crystals

    SciTech Connect

    Li, Tianlei; Gao, Yanfei; Bei, Hongbin; George, Easo P

    2011-01-01

    Instrumented nanoindentation techniques have been widely used to characterize the small-scale mechanical behavior of materials. The elastic-plastic transition during nanoindentation is often indicated by a sudden displacement burst (pop-in) in the measured load-displacement curve. In defect-free single crystals, the pop-in is believed to be the result of homogeneous dislocation nucleation because the maximum shear stress corresponding to the pop-in load approaches the theoretical strength of the materials and because the statistical distribution of pop-in stresses is consistent with what is expected for a thermally activated process of homogeneous dislocation nucleation. This paper investigates whether this process is affected by crystallography and stress components other than the resolved shear stress. A Stroh formalism coupled with the two-dimensional Fourier transformation is used to derive the analytical stress fields in elastically anisotropic solids under Hertzian contact, which allows the determination of an indentation Schmid factor, namely, the ratio of maximum resolved shear stress to the maximum contact pressure. Nanoindentation tests were conducted on B2-structured NiAl single crystals with different surface normal directions. This material was chosen because it deforms at room temperature by {110}<001> slip and thus avoids the complexity of partial dislocation nucleation. Good agreement is obtained between the experimental data and the theoretically predicted orientation dependence of pop-in loads based on the indentation Schmid factor. Pop-in load is lowest for indentation directions close to <111> and highest for those close to <001>. In nanoindentation, since the stress component normal to the slip plane is typically comparable in magnitude to the resolved shear stress, we find that the pressure sensitivity of homogeneous dislocation nucleation cannot be determined from pop-in tests. Our statistical measurements generally confirm the thermal

  6. Accurately evaluating Young's modulus of polymers through nanoindentations: A phenomenological correction factor to the Oliver and Pharr procedure

    NASA Astrophysics Data System (ADS)

    Tranchida, Davide; Piccarolo, Stefano; Loos, Joachim; Alexeev, Alexander

    2006-10-01

    The Oliver and Pharr [J. Mater. Res. 7, 1564 (1992)] procedure is a widely used tool to analyze nanoindentation force curves obtained on metals or ceramics. Its application to polymers is, however, difficult, as Young's moduli are commonly overestimated mainly because of viscoelastic effects and pileup. However, polymers spanning a large range of morphologies have been used in this work to introduce a phenomenological correction factor. It depends on indenter geometry: sets of calibration indentations have to be performed on some polymers with known elastic moduli to characterize each indenter.

  7. An investigation of the physico-mechanical properties of pharmaceutical compounds by compaction simulator and nano-indentation

    NASA Astrophysics Data System (ADS)

    Bordawekar, Mangesh

    In early development, pharmaceutical formulation scientists are often faced with challenges of developing robust and scalable formulations in extremely stringent timelines based on limited API quantities. Hence, tablet formulation development would benefit significantly from tools that enable predictive analysis based on limited quantities of API to enable selection of excipients with appropriate physico-mechanical properties that would result in robust and scalable formulations. With the recent technological advances, especially in sensor technologies, tools such as the compaction simulator, and instrumented nanoindentation offer hitherto unavailable means of assessing material properties with limited quantities. The goal of this work was to evaluate the physico-mechanical properties of selected pharmaceutical excipients and active pharmaceutical ingredients using a macro-scale analysis technique (compaction simulator), and a micro-scale analysis technique (nanoindentation tester) and compare the results obtained from these techniques in order to determine whether a rank order correlation exists between the two. Excipients representing diverse physic-mechanical properties, and a group of APIs were selected for the study. For the compaction simulator studies, tablets were uniaxially compressed using a flat faced 11.28mm round tooling on the STYLCAM® 200R compaction simulator, to a target final porosity at two different cam speeds (5 rpm and 25 rpm). The force displacement profiles, plastic, elastic, and total compression energies, plasticity index, energy density and the Heckel plots were determined for each compact. These compacts were further analyzed with a Berkovich geometry indenter. The plasticity index, hardness, elastic modulus, as well as creep and relaxation were determined from the force-displacement profiles. The nature of force-displacement curves was studied to differentiate compounds based on predominant mechanisms of deformation. Compaction

  8. An advanced AFM sensor for high-aspect ratio pattern profile in-line measurement

    NASA Astrophysics Data System (ADS)

    Watanabe, Masahiro; Baba, Shuichi; Nakata, Toshihiko; Kurenuma, Toru; Kuroda, Hiroshi; Hiroki, Takenori

    2006-03-01

    Design rule shrinkage and the wider adoption of new device structures such as STI, copper damascene interconnects, and deep trench structures have increased the necessity of in-line process monitoring of step heights and profiles of device structures. For monitoring active device patterns, not test patterns as in OCD, AFM is the only non-destructive 3D monitoring tool. The barriers to using AFM in-line monitoring are its slow throughput and the accuracy degradation associated with probe tip wear and spike noise caused by unwanted oscillation on the steep slopes of high-aspect-ratio patterns. Our proprietary AFM scanning method, Step in mode®, is the method best suited to measuring high-aspect-ratio pattern profiles. Because the probe is not dragged on the sample surface as in conventional AFM, the profile trace fidelity across steep slopes is excellent. Because the probe does not oscillate and hit the sample at a high frequency as in AC scanning mode, this mode is free from unwanted spurious noises on steep sample slopes and incurs extremely little probe tip wear. To fully take advantage of the above properties, we have developed an AFM sensor optimized for in-line use, which produces accurate profile data at high speeds. The control scheme we have developed for the AFM sensor, which we call "Smart Step-in", elaborately analyses the contact force signal, enabling efficient probe tip scanning and a low and stable contact force. The mechanism of the AFM sensor has been optimized for the higher scanning rate and has improved the accuracy, such as the scanning planarity, position and height accuracy, and slope angle accuracy. Our prototype AFM sensor can scan high-aspect-ratio patterns while stabilizing the contact force at 3 nN. The step height measurement repeatability was 0.8 nm (3σ). A STI-like test pattern was scanned, and the steep sidewalls with angles of 84° were measured with high fidelity and without spurious noises.

  9. MEMS piezoresistive ring resonator for AFM imaging with pico-Newton force resolution

    NASA Astrophysics Data System (ADS)

    Xiong, Z.; Walter, B.; Mairiaux, E.; Faucher, M.; Buchaillot, L.; Legrand, B.

    2013-03-01

    A new concept of atomic force microscope (AFM) oscillating probes using electrostatic excitation and piezoresistive detection is presented. The probe is characterized by electrical methods in vacuum and by mechanical methods in air. A frequency-mixing measurement technique is developed to reduce the parasitic signal floor. The probe resonance frequencies are in the 1 MHz range and the quality factor is measured about 53 000 in vacuum and 3000 in air. The ring probe is mounted onto a commercial AFM set-up and topographic images of patterned sample surfaces are obtained. The force resolution deduced from the measurements is about 10 pN Hz-0.5.

  10. Studying post-etching silicon crystal defects on 300mm wafer by automatic defect review AFM

    NASA Astrophysics Data System (ADS)

    Zandiatashbar, Ardavan; Taylor, Patrick A.; Kim, Byong; Yoo, Young-kook; Lee, Keibock; Jo, Ahjin; Lee, Ju Suk; Cho, Sang-Joon; Park, Sang-il

    2016-03-01

    Single crystal silicon wafers are the fundamental elements of semiconductor manufacturing industry. The wafers produced by Czochralski (CZ) process are very high quality single crystalline materials with known defects that are formed during the crystal growth or modified by further processing. While defects can be unfavorable for yield for some manufactured electrical devices, a group of defects like oxide precipitates can have both positive and negative impacts on the final device. The spatial distribution of these defects may be found by scattering techniques. However, due to limitations of scattering (i.e. light wavelength), many crystal defects are either poorly classified or not detected. Therefore a high throughput and accurate characterization of their shape and dimension is essential for reviewing the defects and proper classification. While scanning electron microscopy (SEM) can provide high resolution twodimensional images, atomic force microscopy (AFM) is essential for obtaining three-dimensional information of the defects of interest (DOI) as it is known to provide the highest vertical resolution among all techniques [1]. However AFM's low throughput, limited tip life, and laborious efforts for locating the DOI have been the limitations of this technique for defect review for 300 mm wafers. To address these limitations of AFM, automatic defect review AFM has been introduced recently [2], and is utilized in this work for studying DOI on 300 mm silicon wafer. In this work, we carefully etched a 300 mm silicon wafer with a gaseous acid in a reducing atmosphere at a temperature and for a sufficient duration to decorate and grow the crystal defects to a size capable of being detected as light scattering defects [3]. The etched defects form a shallow structure and their distribution and relative size are inspected by laser light scattering (LLS). However, several groups of defects couldn't be properly sized by the LLS due to the very shallow depth and low

  11. Coexistence of orbital and CE-AFM orders in colossal magnetoresistance manganites: A symmetry perspective

    NASA Astrophysics Data System (ADS)

    Ribeiro, J. L.

    2016-07-01

    The complex interplay between order parameters of different nature that dominates the physics of colossal magnetoresistance manganites is analysed from a symmetry based perspective. Phenomenological energies are given for the different competing phases. It is shown that the general trends observed in different systems, such as the mutual exclusion of orbital order and A-AFM order and the related stabilization of the CE-AFM order, stem to large extend from the symmetry of the parameters involved. The possible stabilization of complex phases where charge and orbital order coexist with magnetic and ferroelectric states is also anticipated.

  12. FRAME (Force Review Automation Environment): MATLAB-based AFM data processor.

    PubMed

    Partola, Kostyantyn R; Lykotrafitis, George

    2016-05-01

    Data processing of force-displacement curves generated by atomic force microscopes (AFMs) for elastic moduli and unbinding event measurements is very time consuming and susceptible to user error or bias. There is an evident need for consistent, dependable, and easy-to-use AFM data processing software. We have developed an open-source software application, the force review automation environment (or FRAME), that provides users with an intuitive graphical user interface, automating data processing, and tools for expediting manual processing. We did not observe a significant difference between manually processed and automatically processed results from the same data sets. PMID:26972765

  13. Direct visualization of the trimeric structure of the ASIC1a channel, using AFM imaging

    SciTech Connect

    Carnally, Stewart M.; Dev, Harveer S.; Stewart, Andrew P.; Barrera, Nelson P.; Van Bemmelen, Miguel X.; Schild, Laurent; Henderson, Robert M.; Edwardson, J.Michael

    2008-08-08

    There has been confusion about the subunit stoichiometry of the degenerin family of ion channels. Recently, a crystal structure of acid-sensing ion channel (ASIC) 1a revealed that it assembles as a trimer. Here, we used atomic force microscopy (AFM) to image unprocessed ASIC1a bound to mica. We detected a mixture of subunit monomers, dimers and trimers. In some cases, triple-subunit clusters were clearly visible, confirming the trimeric structure of the channel, and indicating that the trimer sometimes disaggregated after adhesion to the mica surface. This AFM-based technique will now enable us to determine the subunit arrangement within heteromeric ASICs.

  14. Multiparametric imaging of biological systems by force-distance curve-based AFM.

    PubMed

    Dufrêne, Yves F; Martínez-Martín, David; Medalsy, Izhar; Alsteens, David; Müller, Daniel J

    2013-09-01

    A current challenge in the life sciences is to understand how biological systems change their structural, biophysical and chemical properties to adjust functionality. Addressing this issue has been severely hampered by the lack of methods capable of imaging biosystems at high resolution while simultaneously mapping their multiple properties. Recent developments in force-distance (FD) curve-based atomic force microscopy (AFM) now enable researchers to combine (sub)molecular imaging with quantitative mapping of physical, chemical and biological interactions. Here we discuss the principles and applications of advanced FD-based AFM tools for the quantitative multiparametric characterization of complex cellular and biomolecular systems under physiological conditions. PMID:23985731

  15. Probing the PEDOT:PSS/cell interface with conductive colloidal probe AFM-SECM

    NASA Astrophysics Data System (ADS)

    Knittel, P.; Zhang, H.; Kranz, C.; Wallace, G. G.; Higgins, M. J.

    2016-02-01

    Conductive colloidal probe Atomic Force-Scanning Electrochemical Microscopy (AFM-SECM) is a new approach, which employs electrically insulated AFM probes except for a gold-coated colloid located at the end of the cantilever. Hence, force measurements can be performed while biasing the conductive colloid under physiological conditions. Moreover, such colloids can be modified by electrochemical polymerization resulting, e.g. in conductive polymer-coated spheres, which in addition may be loaded with specific dopants. In contrast to other AFM-based single cell force spectroscopy measurements, these probes allow adhesion measurements at the cell-biomaterial interface on multiple cells in a rapid manner while the properties of the polymer can be changed by applying a bias. In addition, spatially resolved electrochemical information e.g., oxygen reduction can be obtained simultaneously. Conductive colloid AFM-SECM probes modified with poly(3,4-ethylenedioxythiophene) doped with polystyrene sulfonate (PEDOT:PSS) are used for single cell force measurements in mouse fibroblasts and single cell interactions are investigated as a function of the applied potential.Conductive colloidal probe Atomic Force-Scanning Electrochemical Microscopy (AFM-SECM) is a new approach, which employs electrically insulated AFM probes except for a gold-coated colloid located at the end of the cantilever. Hence, force measurements can be performed while biasing the conductive colloid under physiological conditions. Moreover, such colloids can be modified by electrochemical polymerization resulting, e.g. in conductive polymer-coated spheres, which in addition may be loaded with specific dopants. In contrast to other AFM-based single cell force spectroscopy measurements, these probes allow adhesion measurements at the cell-biomaterial interface on multiple cells in a rapid manner while the properties of the polymer can be changed by applying a bias. In addition, spatially resolved electrochemical

  16. AFM and XPA data on structural features and properties of films and powders based on naphthalocyanines

    NASA Astrophysics Data System (ADS)

    Ramonova, A. G.; Nakusov, A. T.; Sozanov, V. G.; Bliev, A. P.; Magkoev, T. T.

    2015-06-01

    The template synthesis is used to produce powders and films based on naphthalocyanines and the corresponding metal complexes (Pc, CuPc, and NiPc). The atomic-force microscopy (AFM) and X-ray phase analysis (XPA) are employed in the study of structure and phase of fine powders and nanostructured films. The AFM data are used to determine the orientation and density of primary particles packed in the film. The XPA method is used to study the chemical composition and crystal structure of the synthesized samples. The regularities related to the structural features that affect the electrophysical properties of the films under study are revealed.

  17. An Evaluation of the Impacts of AF-M315E Propulsion Systems for Varied Mission Applications

    NASA Technical Reports Server (NTRS)

    Deans, Matthew C.; Oleson, Steven R.; Fittje, James; Colozza, Anthony; Packard, Tom; Gyekenyesi, John; McLean, Christopher H.; Spores, Ronald A.

    2015-01-01

    The purpose of the AF-M315E COMPASS study is to identify near-term (3-5 years) and long term (5 years +) opportunities for infusion, specifically the thruster and associated component technologies being developed as part of the GPIM project. Develop design reference missions which show the advantages of the AF-M315E green propulsion system. Utilize a combination of past COMPASS designs and selected new designs to demonstrate AF-M315E advantages. Use the COMPASS process to show the puts and takes of using AF-M315E at the integrated system level.

  18. Protein Nanocontainers from Nonviral Origin: Testing the Mechanics of Artificial and Natural Protein Cages by AFM.

    PubMed

    Heinze, K; Sasaki, E; King, N P; Baker, D; Hilvert, D; Wuite, G J L; Roos, W H

    2016-07-01

    Self-assembling protein nanocontainers are promising candidates for an increasingly wide scope of purposes. Their applications range from drug delivery vehicles and imaging agents to nanocompartments for controlled enzymatic activity. In order to exploit their full potential in these different fields, characterization of their properties is vital. For example, their mechanical properties give insight into the stability of a particle as a function of their internal content. The mechanics can be probed by atomic force microscopy nanoindentation, and while this single particle method is increasingly used to probe material properties of viral nanocages, it has hardly been used to characterize nonviral nanocages. Here we report nanoindentation studies on two types of nonviral nanocontainers: (i) lumazine synthase from Aquifex aeolicus (AaLS), which naturally self-assembles into icosahedral cages, and (ii) the artificial protein cage O3-33 originating from a computational design approach. In addition, we tested particles that had been engineered toward improved cargo loading capacity and compared these nanocages in empty and loaded states. We found that the thermostable AaLS cages are stiffer and resist higher forces before breaking than the O3-33 particles, but that mutations affecting the size of AaLS particles have a dramatic effect on their structural stability. Furthermore, we show that cargo packaging can occur while maintaining the cage's mechanical properties. PMID:27187612

  19. Measuring the energy landscape of complex bonds using AFM

    NASA Astrophysics Data System (ADS)

    Mayyas, Essa; Hoffmann, Peter; Runyan, Lindsay

    2009-03-01

    We measured rupture force of a complex bond of two interacting proteins with atomic force microscopy. Proteins of interest were active and latent Matrix metalloproteinases (MMPs), type 2 and 9, and their tissue inhibitors TIMP1 and TIMP2. Measurements show that the rupture force depends on the pulling speed; it ranges from 30 pN to 150 pN at pulling speeds 30nm/s to 48000nm/s. Analyzing data using an extended theory enabled us to understand the mechanism of MMP-TIMP interaction; we determined all physical parameters that form the landscape energy of the interaction, in addition to the life time of the bond and its length. Moreover, we used the pulling experiment to study the interaction of TIMP2 with the receptor MT1-MMP on the surface of living cells.

  20. Molecular dynamics investigations of mechanical behaviours in monocrystalline silicon due to nanoindentation at cryogenic temperatures and room temperature.

    PubMed

    Du, Xiancheng; Zhao, Hongwei; Zhang, Lin; Yang, Yihan; Xu, Hailong; Fu, Haishuang; Li, Lijia

    2015-01-01

    Molecular dynamics simulations of nanoindentation tests on monocrystalline silicon (010) surface were conducted to investigate the mechanical properties and deformation mechanism from cryogenic temperature being 10 K to room temperature being 300 K. Furthermore, the load-displacement curves were obtained and the phase transformation was investigated at different temperatures. The results show that the phase transformation occurs both at cryogenic temperatures and at room temperature. By searching for the presence of the unique non-bonded fifth neighbour atom, the metastable phases (Si-III and Si-XII) with fourfold coordination could be distinguished from Si-I phase during the loading stage of nanoindentation process. The Si-II, Si-XIII, and amorphous phase were also found in the region beneath the indenter. Moreover, through the degree of alignment of the metastable phases along specific crystal orientation at different temperatures, it was found that the temperature had effect on the anisotropy of the monocrystalline silicon, and the simulation results indicate that the anisotropy of monocrystalline silicon is strengthened at low temperatures. PMID:26537978