Displacement and Deflection of AN Optical Beam by Airborne Ultrasound

NASA Astrophysics Data System (ADS)

Caron, James N.

2008-02-01

Gas-Coupled Laser Acoustic Detection enables laser-based sensing of ultrasound from a solid without contact of the surface, and independent of the optical properties of the solid surface. The interaction between the probe beam and acoustic field has typically been modeled as creating a deflection in the optical beam. This paper describes this interaction as a combination of displacement and deflection. Sensing displacement can significantly decrease the system's dependence of length.

Experimental investigation of ash deposits on convection heating surfaces of a circulating fluidized bed municipal solid waste incinerator.

PubMed

Tang, Zhi; Chen, Xiaoping; Liu, Daoyin; Zhuang, Yaming; Ye, Minghua; Sheng, Hongchan; Xu, Shaojuan

2016-10-01

Incineration of municipal solid waste (MSW) is a waste treatment method which can be sustainable in terms of waste volume reduction, as well as a source of renewable energy. During MSW combustion, increased formation of deposits on convection heating exchanger surfaces can pose severe operational problems, such as fouling, slagging and corrosion. These problems can cause lower heat transfer efficiency from the hot flue gas to the working fluid inside the tubes. A study was performed where experiments were carried out to examine the ash deposition characteristics in a full-scale MSW circulating fluidized bed (CFB) incinerator, using a newly designed deposit probe that was fitted with six thermocouples and four removable half rings. The influence of probe exposure time and probe surface temperature (500, 560, and 700°C) on ash deposit formation rate was investigated. The results indicate that the deposition mass and collection efficiency achieve a minimum at the probe surface temperature of 560°C. Ash particles are deposited on both the windward and leeward sides of the probe by impacting and thermophoretic/condensation behavior. The major inorganic elements present in the ash deposits are Ca, Al and Si. Compared to ash deposits formed on the leeward side of the probe, windward-side ash deposits contain relatively higher Ca and S concentrations, but lower levels of Al and Si. Among all cases at different surface temperatures, the differences in elemental composition of the ash deposits from the leeward side are insignificant. However, as the surface temperature increases, the concentrations of Al, Si, K and Na in the windward-side ash deposits increase, but the Ca concentration is reduced. Finally, governing mechanisms are proposed on the basis of the experimental data, such as deposit morphology, elemental composition and thermodynamic calculations. Copyright © 2016. Published by Elsevier B.V.

Evaluation of crystallization behavior on the surface of nifedipine solid dispersion powder using inverse gas chromatography.

PubMed

Miyanishi, Hideo; Nemoto, Takayuki; Mizuno, Masayasu; Mimura, Hisashi; Kitamura, Satoshi; Iwao, Yasunori; Noguchi, Shuji; Itai, Shigeru

2013-02-01

To investigate crystallization behavior on the surface of amorphous solid dispersion powder using inverse gas chromatography (IGC) and to predict the physical stability at temperatures below the glass transition temperature (T (g)). Amorphous solid dispersion powder was prepared by melt-quenching of a mixture of crystalline nifedipine and polyvinylpyrrolidon (PVP) K-30. IGC was conducted by injecting undecane (probe gas) and methane (reference gas) repeatedly to the solid dispersion at temperatures below T (g). Surface crystallization was evaluated by the retention volume change of undecane based on the observation that the surface of the solid dispersion with crystallized nifedipine gives an increased retention volume. On applying the retention volume change to the Hancock-Sharp equation, surface crystallization was found to follow a two-dimensional growth of nuclei mechanism. Estimation of the crystallization rates at temperatures far below T (g) using the Avrami-Erofeev equation and Arrhenius equation showed that, to maintain its quality for at least three years, the solid dispersion should be stored at -20°C (T (g) - 65°C). IGC can be used to evaluate crystallization behavior on the surface of a solid dispersion powder, and, unlike traditional techniques, can also predict the stability of the solid dispersion based on the surface crystallization behavior.

Charging Characteristics of an Insulating Hollow Cylinder in Vacuum

NASA Astrophysics Data System (ADS)

Yamamoto, Osamu; Hayashi, Hirotaka; Wadahama, Toshihiko; Takeda, Daisuke; Hamada, Shoji; Ohsawa, Yasuharu

This paper deals with charging characteristics of the inner surface of an insulating hollow cylinder in vacuum. We conducted measurements of electric field strength near the triple points on cathode by using an electrostatic probe. Also we conducted a computer simulation of charging based on the Secondary Electron Emission Avalanche (SEEA) mechanism. These results are compared with those obtained previously for solid cylinders. As a result, we have clarified that hollow cylinders acquire surface charge which is larger than that of solid cylinders. We have also found that charge controlling effect by roughening the inner surface, which have been proved effective to depress charging on the surface of solid cylinders in our previous studies, is limited for hollow cylinders.

Desorption in Mass Spectrometry.

PubMed

Usmanov, Dilshadbek Tursunbayevich; Ninomiya, Satoshi; Chen, Lee Chuin; Saha, Subhrakanti; Mandal, Mridul Kanti; Sakai, Yuji; Takaishi, Rio; Habib, Ahsan; Hiraoka, Kenzo; Yoshimura, Kentaro; Takeda, Sen; Wada, Hiroshi; Nonami, Hiroshi

2017-01-01

In mass spectrometry, analytes must be released in the gas phase. There are two representative methods for the gasification of the condensed samples, i.e. , ablation and desorption. While ablation is based on the explosion induced by the energy accumulated in the condensed matrix, desorption is a single molecular process taking place on the surface. In this paper, desorption methods for mass spectrometry developed in our laboratory: flash heating/rapid cooling, Leidenfrost phenomenon-assisted thermal desorption (LPTD), solid/solid friction, liquid/solid friction, electrospray droplet impact (EDI) ionization/desorption, and probe electrospray ionization (PESI), will be described. All the methods are concerned with the surface and interface phenomena. The concept of how to desorb less-volatility compounds from the surface will be discussed.

Surface Temperature Dependence of Hydrogen Ortho-Para Conversion on Amorphous Solid Water.

PubMed

Ueta, Hirokazu; Watanabe, Naoki; Hama, Tetsuya; Kouchi, Akira

2016-06-24

The surface temperature dependence of the ortho-to-para conversion of H_{2} on amorphous solid water is first reported. A combination of photostimulated desorption and resonance-enhanced multiphoton ionization techniques allowed us to sensitively probe the conversion on the surface of amorphous solid water at temperatures of 9.2-16 K. Within a narrow temperature window of 8 K, the conversion time steeply varied from ∼4.1×10^{3} to ∼6.4×10^{2}  s. The observed temperature dependence is discussed in the context of previously suggested models and the energy dissipation process. The two-phonon process most likely dominates the conversion rate at low temperatures.

Development and Application of Wide Bandwidth Magneto-Resistive Sensor Based Eddy Current Probe

NASA Technical Reports Server (NTRS)

Wincheski, Russell A.; Simpson, John

2010-01-01

The integration of magneto-resistive sensors into eddy current probes can significantly expand the capabilities of conventional eddy current nondestructive evaluation techniques. The room temperature solid-state sensors have typical bandwidths in the megahertz range and resolutions of tens of microgauss. The low frequency sensitivity of magneto-resistive sensors has been capitalized upon in previous research to fabricate very low frequency eddy current sensors for deep flaw detection in multilayer conductors. In this work a modified probe design is presented to expand the capabilities of the device. The new probe design incorporates a dual induction source enabling operation from low frequency deep flaw detection to high frequency high resolution near surface material characterization. Applications of the probe for the detection of localized near surface conductivity anomalies are presented. Finite element modeling of the probe is shown to be in good agreement with experimental measurements.

Cold cathode vacuum discharge tube

DOEpatents

Boettcher, Gordon E.

1998-01-01

A cold cathode vacuum discharge tube, and method for making same, with an interior surface of the trigger probe coated with carbon deposited by carbon vapor deposition (CVD) or diamond-like carbon (DLC) deposition. Preferably a solid graphite insert is employed in the probe-cathode structure in place of an aluminum bushing employed in the prior art. The CVD or DLC probe face is laser scribed to allow resistance trimming to match available trigger voltage signals and to reduce electrical aging.

Sum frequency generation and solid-state NMR study of the structure, orientation, and dynamics of polystyrene-adsorbed peptides

PubMed Central

Weidner, Tobias; Breen, Nicholas F.; Li, Kun; Drobny, Gary P.; Castner, David G.

2010-01-01

The power of combining sum frequency generation (SFG) vibrational spectroscopy and solid-state nuclear magnetic resonance (ssNMR) spectroscopy to quantify, with site specificity and atomic resolution, the orientation and dynamics of side chains in synthetic model peptides adsorbed onto polystyrene (PS) surfaces is demonstrated in this study. Although isotopic labeling has long been used in ssNMR studies to site-specifically probe the structure and dynamics of biomolecules, the potential of SFG to probe side chain orientation in isotopically labeled surface-adsorbed peptides and proteins remains largely unexplored. The 14 amino acid leucine-lysine peptide studied in this work is known to form an α-helical secondary structure at liquid-solid interfaces. Selective, individual deuteration of the isopropyl group in each leucine residue was used to probe the orientation and dynamics of each individual leucine side chain of LKα14 adsorbed onto PS. The selective isotopic labeling methods allowed SFG analysis to determine the orientations of individual side chains in adsorbed peptides. Side chain dynamics were obtained by fitting the deuterium ssNMR line shape to specific motional models. Through the combined use of SFG and ssNMR, the dynamic trends observed for individual side chains by ssNMR have been correlated with side chain orientation relative to the PS surface as determined by SFG. This combination provides a more complete and quantitative picture of the structure, orientation, and dynamics of these surface-adsorbed peptides than could be obtained if either technique were used separately. PMID:20628016

A robust molecular probe for Ångstrom-scale analytics in liquids

PubMed Central

Nirmalraj, Peter; Thompson, Damien; Dimitrakopoulos, Christos; Gotsmann, Bernd; Dumcenco, Dumitru; Kis, Andras; Riel, Heike

2016-01-01

Traditionally, nanomaterial profiling using a single-molecule-terminated scanning probe is performed at the vacuum–solid interface often at a few Kelvin, but is not a notion immediately associated with liquid–solid interface at room temperature. Here, using a scanning tunnelling probe functionalized with a single C60 molecule stabilized in a high-density liquid, we resolve low-dimensional surface defects, atomic interfaces and capture Ångstrom-level bond-length variations in single-layer graphene and MoS2. Atom-by-atom controllable imaging contrast is demonstrated at room temperature and the electronic structure of the C60–metal probe complex within the encompassing liquid molecules is clarified using density functional theory. Our findings demonstrates that operating a robust single-molecular probe is not restricted to ultra-high vacuum and cryogenic settings. Hence the scope of high-precision analytics can be extended towards resolving sub-molecular features of organic elements and gauging ambient compatibility of emerging layered materials with atomic-scale sensitivity under experimentally less stringent conditions. PMID:27516157

Enhanced solid-phase recombinase polymerase amplification and electrochemical detection.

PubMed

Del Río, Jonathan Sabaté; Lobato, Ivan Magriñà; Mayboroda, Olena; Katakis, Ioanis; O'Sullivan, Ciara K

2017-05-01

Recombinase polymerase amplification (RPA) is an elegant method for the rapid, isothermal amplification of nucleic acids. Here, we elucidate the optimal surface chemistry for rapid and efficient solid-phase RPA, which was fine-tuned in order to obtain a maximum signal-to-noise ratio, defining the optimal DNA probe density, probe-to-lateral spacer ratio (1:0, 1:1, 1:10 and 1:100) and length of a vertical spacer of the probe as well as investigating the effect of different types of lateral spacers. The use of different labelling strategies was also examined in order to reduce the number of steps required for the analysis, using biotin or horseradish peroxidase-labelled reverse primers. Optimisation of the amplification temperature used and the use of surface blocking agents were also pursued. The combination of these changes facilitated a significantly more rapid amplification and detection protocol, with a lowered limit of detection (LOD) of 1 · 10 -15 M. The optimised protocol was applied to the detection of Francisella tularensis in real samples from hares and a clear correlation with PCR and qPCR results observed and the solid-phase RPA demonstrated to be capable of detecting 500 fM target DNA in real samples. Graphical abstract Relative size of thiolated lateral spacers tested versus the primer and the uvsx recombinase protein.

Cold cathode vacuum discharge tube

DOEpatents

Boettcher, G.E.

1998-03-10

A cold cathode vacuum discharge tube, and method for making same, are disclosed with an interior surface of the trigger probe coated with carbon deposited by carbon vapor deposition (CVD) or diamond-like carbon (DLC) deposition. Preferably a solid graphite insert is employed in the probe-cathode structure in place of an aluminum bushing employed in the prior art. The CVD or DLC probe face is laser scribed to allow resistance trimming to match available trigger voltage signals and to reduce electrical aging. 15 figs.

Cold cathode vacuum discharge tube

DOEpatents

Boettcher, G.E.

1998-04-14

A cold cathode vacuum discharge tube, and method for making same, with an interior surface of the trigger probe coated with carbon deposited by chemical vapor deposition (CVD) or diamond-like carbon (DLC) deposition are disclosed. Preferably a solid graphite insert is employed in the probe-cathode structure in place of an aluminum bushing employed in the prior art. The CVD or DLC probe face is laser scribed to allow resistance trimming to match available trigger voltage signals and to reduce electrical aging. 14 figs.

Desorption in Mass Spectrometry

PubMed Central

Usmanov, Dilshadbek Tursunbayevich; Ninomiya, Satoshi; Chen, Lee Chuin; Saha, Subhrakanti; Mandal, Mridul Kanti; Sakai, Yuji; Takaishi, Rio; Habib, Ahsan; Hiraoka, Kenzo; Yoshimura, Kentaro; Takeda, Sen; Wada, Hiroshi; Nonami, Hiroshi

2017-01-01

In mass spectrometry, analytes must be released in the gas phase. There are two representative methods for the gasification of the condensed samples, i.e., ablation and desorption. While ablation is based on the explosion induced by the energy accumulated in the condensed matrix, desorption is a single molecular process taking place on the surface. In this paper, desorption methods for mass spectrometry developed in our laboratory: flash heating/rapid cooling, Leidenfrost phenomenon-assisted thermal desorption (LPTD), solid/solid friction, liquid/solid friction, electrospray droplet impact (EDI) ionization/desorption, and probe electrospray ionization (PESI), will be described. All the methods are concerned with the surface and interface phenomena. The concept of how to desorb less-volatility compounds from the surface will be discussed. PMID:28337398

Direct mapping of ion diffusion times on LiCoO2 surfaces with nanometer resolution

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

Guo, Senli; Jesse, Stephen; Kalnaus, Sergiy

2011-01-01

The strong coupling between the molar volume and mobile ion concentration in ionically-conductive solids is used for spatially-resolved studies of ionic transport on the polycrystalline LiCoO2 surface by time-resolved spectroscopy. Strong variability between ionic transport at the grain boundaries and within the grains is observed, and the relationship between relaxation and hysteresis loop formation is established. The use of the strain measurements allows ionic transport be probed on the nanoscale, and suggests enormous potential for probing ionic materials and devices.

Investigating buried polymer interfaces using sum frequency generation vibrational spectroscopy

PubMed Central

Chen, Zhan

2010-01-01

This paper reviews recent progress in the studies of buried polymer interfaces using sum frequency generation (SFG) vibrational spectroscopy. Both buried solid/liquid and solid/solid interfaces involving polymeric materials are discussed. SFG studies of polymer/water interfaces show that different polymers exhibit varied surface restructuring behavior in water, indicating the importance of probing polymer/water interfaces in situ. SFG has also been applied to the investigation of interfaces between polymers and other liquids. It has been found that molecular interactions at such polymer/liquid interfaces dictate interfacial polymer structures. The molecular structures of silane molecules, which are widely used as adhesion promoters, have been investigated using SFG at buried polymer/silane and polymer/polymer interfaces, providing molecular-level understanding of polymer adhesion promotion. The molecular structures of polymer/solid interfaces have been examined using SFG with several different experimental geometries. These results have provided molecular-level information about polymer friction, adhesion, interfacial chemical reactions, interfacial electronic properties, and the structure of layer-by-layer deposited polymers. Such research has demonstrated that SFG is a powerful tool to probe buried interfaces involving polymeric materials, which are difficult to study by conventional surface sensitive analytical techniques. PMID:21113334

Probing Atom-Surface Interactions by Diffraction of Bose-Einstein Condensates

NASA Astrophysics Data System (ADS)

Bender, Helmar; Stehle, Christian; Zimmermann, Claus; Slama, Sebastian; Fiedler, Johannes; Scheel, Stefan; Buhmann, Stefan Yoshi; Marachevsky, Valery N.

2014-01-01

In this article, we analyze the Casimir-Polder interaction of atoms with a solid grating and the repulsive interaction between the atoms and the grating in the presence of an external laser source. The Casimir-Polder potential is evaluated exactly in terms of Rayleigh reflection coefficients and via an approximate Hamaker approach. The laser-tuned repulsive interaction is given in terms of Rayleigh transmission coefficients. The combined potential landscape above the solid grating is probed locally by diffraction of Bose-Einstein condensates. Measured diffraction efficiencies reveal information about the shape of the potential landscape in agreement with the theory based on Rayleigh decompositions.

Fabrication and surface-modification of implantable microprobes for neuroscience studies

NASA Astrophysics Data System (ADS)

Cao, H.; Nguyen, C. M.; Chiao, J. C.

2012-06-01

In this work implantable micro-probes for central nervous system (CNS) studies were developed on silicon and polyimide substrates. The probes which contained micro-electrode arrays with different surface modifications were designed for implantation in the CNS. The electrode surfaces were modified with nano-scale structures that could greatly increase the active surface area in order to enhance the electrochemical current outputs while maintaining micro-scale dimensions of the electrodes and probes. The electrodes were made of gold or platinum, and designed with different sizes. The silicon probes were modified by silicon nanowires fabricated with the vapor-liquid-solid mechanism at high temperatures. With polyimide substrates, the nanostructure modification was carried out by applying concentrated gold or silver colloid solutions onto the micro-electrodes at room temperature. The surfaces of electrodes before and after modification were observed by scanning electron microscopy. The silicon nanowire-modified surface was characterized by cyclic voltammetry. Experiments were carried out to investigate the improvement in sensing performance. The modified electrodes were tested with H2O2, electrochemical L-glutamate and dopamine. Comparisons between electrodes with and without nanostructure modification were conducted showing that the modifications have enhanced the signal outputs of the electrochemical neurotransmitter sensors.

Cross-section analysis of the Magnum-PSI plasma beam using a 2D multi-probe system

NASA Astrophysics Data System (ADS)

Costin, C.; Anita, V.; Ghiorghiu, F.; Popa, G.; De Temmerman, G.; van den Berg, M. A.; Scholten, J.; Brons, S.

2015-02-01

The linear plasma generator Magnum-PSI was designed for the study of plasma-surface interactions under relevant conditions of fusion devices. A key factor for such studies is the knowledge of a set of parameters that characterize the plasma interacting with the solid surface. This paper reports on the electrical diagnosis of the plasma beam in Magnum-PSI using a multi-probe system consisting of 64 probes arranged in a 2D square matrix. Cross-section distributions of floating potential and ion current intensity were registered for a hydrogen plasma beam under various discharge currents (80-175 A) and magnetic field strengths (0.47-1.41 T in the middle of the coils). Probe measurements revealed a high level of flexibility of plasma beam parameters with respect to the operating conditions.

Local Environment and Interactions of Liquid and Solid Interfaces Revealed by Spectral Line Shape of Surface Selective Nonlinear Vibrational Probe

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

Chen, Shun-Li; Fu, Li; Chase, Zizwe A.

Vibrational spectral lineshape contains important detailed information of molecular vibration and reports its specific interactions and couplings to its local environment. In this work, recently developed sub-1 cm-1 high-resolution broadband sum frequency generation vibrational spectroscopy (HR-BB-SFG-VS) was used to measure the -C≡N stretch vibration in the 4-n-octyl-4’-cyanobiphenyl (8CB) Langmuir or Langmuir-Blodgett (LB) monolayer as a unique vibrational probe, and the spectral lineshape analysis revealed the local environment and interactions at the air/water, air/glass, air/calcium fluoride and air/-quartz interfaces for the first time. The 8CB Langmuir or LB film is uniform and the vibrational spectral lineshape of its -C≡N group hasmore » been well characterized, making it a good choice as the surface vibrational probe. Lineshape analysis of the 8CB -C≡N stretch SFG vibrational spectra suggests the coherent vibrational dynamics and the structural and dynamic inhomogeneity of the -C≡N group at each interface are uniquely different. In addition, it is also found that there are significantly different roles for water molecules in the LB films on different substrate surfaces. These results demonstrated the novel capabilities of the surface nonlinear spectroscopy in characterization and in understanding the specific structures and chemical interactions at the liquid and solid interfaces in general.« less

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

PubMed

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

2017-01-04

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

Role of the external NH2 linker on the conformation of surface immobilized single strand DNA probes and their SERS detection

NASA Astrophysics Data System (ADS)

He, Lijie; Langlet, Michel; Stambouli, Valerie

2017-03-01

The conformation and topological properties of DNA single strand probe molecules attached on solid surfaces are important, notably for the performances of devices such as biosensors. Commonly, the DNA probes are tethered to the surface using external linkers such as NH2. In this study, the role and influence of this amino-linker on the immobilization way and conformation of DNA probes on Ag nanoparticle surface is emphasized using Surface Enhanced Raman Spectroscopy (SERS). We compare the SERS spectra and their reproducibility in the case of two groups of DNA polybase probes which are polyA, polyC, polyT, and polyG. In the first group, the polybases exhibit an external NH2 functional linker while in the second group the polybases are NH2-free. The results show that the reproducibility of SERS spectra is enhanced in the case of the first group. It leads us to propose two models of polybase conformation on Ag surface according to the presence or the absence of the external NH2 linker. In the presence of the NH2 external linker, the latter would act as a major anchoring point. As a result, the polybases are much ordered with a less random orientation than in the case of NH2-free polybases. Consequently, in view of further in situ hybridization for biosensing applications, it is strongly recommended to use NH2 linker functionalized DNA probes.

Identification and formation mechanism of individual degradation products in lithium-ion batteries studied by liquid chromatography/electrospray ionization mass spectrometry and atmospheric solid analysis probe mass spectrometry.

PubMed

Takeda, Sahori; Morimura, Wataru; Liu, Yi-Hung; Sakai, Tetsuo; Saito, Yuria

2016-08-15

Improvement of lithium ion batteries (LIBs) in terms of performance and robustness requires good understanding of the reaction processes. The analysis of the individual degradation products in LIB electrolytes and on the surface of the electrodes provides vital information in this regard. In this study, mass spectrometric analytical methods were utilized for the identification of the individual degradation products. The degradation products in the electrolytes recovered from cycle-tested cells were separated by liquid chromatography (LC) and their mass spectrometric analysis was conducted by electrospray ionization mass spectrometry (ESI-MS). For identification of degradation products on the surface of electrodes, atmospheric solid analysis probe (ASAP)-MS analysis was conducted by time-of-flight mass spectrometry with an ASAP probe and an atmospheric pressure chemical ionization source. The degradation products in the electrolytes, namely carbonate oligomers and organophosphates, were identified simultaneously by LC/ESI-MS. Their formation mechanisms were estimated, which explain their different compositions at different temperatures. One degradation product was found on the anode surface by ASAP-MS, and its formation mechanism was explained similarly to those in the electrolyte. The results suggest that the electrolyte degradation is correlated with the formation of a solid electrolyte interphase, which is an important factor in the performance of LIBs. We expect that further investigation of the degradation products by LC/ESI-MS and ASAP-MS will be helpful for studying their degradation processes in LIBs. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Volumetrical Characterization of Sheet Molding Compounds

PubMed Central

Calvimontes, Alfredo; Grundke, Karina; Müller, Anett

2010-01-01

For a comprehensive study of Sheet Molding Compound (SMC) surfaces, topographical data obtained by chromatic confocal imaging were submitted systematically for the development of a profile model to understand the formation of cavities on the surface. In order to qualify SMC surfaces and to predict their coatability, a characterization of cavities is applied. To quantify the effect of surface modification treatments, a new parameter (Surface Relative Smooth) is presented, applied and probed. The parameter proposed can be used for any surface modification of any solid material. PMID:28883370

Investigation of solid phase composition on tablet surfaces by grazing incidence X-ray diffraction.

PubMed

Koradia, Vishal; Tenho, Mikko; Lopez de Diego, Heidi; Ringkjøbing-Elema, Michiel; Møller-Sonnergaard, Jørn; Salonen, Jarno; Lehto, Vesa-Pekka; Rantanen, Jukka

2012-01-01

To investigate solid state transformations of drug substances during compaction using grazing incidence X-ray diffraction (GIXD). The solid forms of three model drugs-theophylline (TP), nitrofurantoin (NF) and amlodipine besylate (AMB)-were compacted at different pressures (from 100 to 1000 MPa); prepared tablets were measured using GIXD. After the initial measurements of freshly compacted tablets, tablets were subjected to suitable recrystallization treatment, and analogous measurements were performed. Solid forms of TP, NF and AMB showed partial amorphization as well as crystal disordering during compaction; the extent of these effects generally increased as a function of pressure. The changes were most pronounced at the outer surface region. The different solid forms showed difference in the formation of amorphicity/crystal disordering. Dehydration due to compaction was observed for the TP monohydrate, whereas hydrates of NF and AMB were stable towards dehydration. With GIXD measurements, it was possible to probe the solid form composition at the different depths of the tablet surfaces and to obtain depth-dependent information on the compaction-induced amorphization, crystal disordering and dehydration.

Surface profile changes of scuffed bearing surfaces. [before and after acid treatment

NASA Technical Reports Server (NTRS)

Lauer, J. L.; Fung, S. S.; Jones, W. R., Jr.

1982-01-01

A phase locked interference microscope capable of resolving depth differences to 30 A and planar displacements of 6000 A was constructed for the examination of the profiles of bearing surfaces without physical contact. This instrument was used to determine surface chemical reactivity by applying a drop of dilute alcoholic hydrochloric acid and measuring the profile of the solid surface before and after application of this probe. Scuffed bearing surfaces reacted much faster than unscuffed ones, but bearing surfaces which had been previously exposed to lubricants containing an organic chloride reacted much more slowly. In a separate series of experiments, a number of stainless steel plates were heated in a nitrogen atmosphere to different temperatures and their reactivity examined later at room temperature. The change of surface contour as a result of the probe reaction followed an Arrhenius type relation with respect to heat treatment temperature. This result could have implications on the scuffing mechanism.

Structural phase transitions and time-resolved dynamics of solid-supported interfacial methanol observed by reflection electron diffraction

NASA Astrophysics Data System (ADS)

Yang, Ding-Shyue; He, Xing; Wu, Chengyi

Due to their large scattering cross sections with matter, electrons are suitable for contactless probing of solid-supported surface assemblies, especially in a reflection geometry. Direct visualization of assembly structures through electron diffraction further enables studies of ultrafast structural dynamics through the pump-probe scheme as well as discoveries of hidden phase changes in equilibrium that have been obscure in spectroscopic measurements. In this presentation, we report our first observation of unique two-stage transformations of interfacial methanol on smooth hydrophobic surfaces. The finding may reconcile the inconsistent previous reports of the crystallization temperature using various indirect methods. Dynamically, energy transfer across a solid-molecule interface following photoexcitation of the substrate is found to be highly dependent on the structure of interfacial methanol. If it is only 2-dimensionally ordered, as the film thickness increases, a prolonged time in the decrease of diffraction intensity is seen, signifying an inefficient vibrational coupling in the surface normal direction. Implications of the dynamics results and an outlook of interfacial studies using time-resolved and averaged electron diffraction will be discussed. We gratefully acknowledge the support from the R. A. Welch Foundation (Grant No. E-1860), the Donors of the American Chemical Society Petroleum Research Fund (ACS-PRF), and the University of Houston.

The Interaction of Water with Solid Surfaces: Fundamental Aspects Revisited

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

Henderson, Michael A.

2002-05-01

Water is perhaps the most important and most pervasive chemical on our planet. The influence of water permeates virtually all areas of biochemical, chemical and physical importance, and is especially evident in phenomena occurring at the interfaces of solid surfaces. Since 1987, when Thiel and Madey (TM) published their review titled "The Interaction of Water with Solid Surfaces: Fundamental Aspects" in Surface Science Reports, there has been considerable progress made in further understanding the fundamental interactions of water with solid surfaces. In the decade and a half, the increased capability of surface scientists to probe at the molecular-level has resultedmore » in more detailed information of the properties of water on progressively more complicated materials and under more stringent conditions. This progress in understanding the properties of water on solid surfaces is evident both in areas for which surface science methodology has traditionally been strong (catalysis and electronic materials) and also in new areas not traditionally studied by surface scientists, such as electrochemistry, photoconversion, mineralogy, adhesion, sensors, atmospheric chemistry, and tribology. Researchers in all these fields grapple with very basic questions regarding the interactions of water with solid surfaces, such as how is water adsorbed, what are the chemical and electrostatic forces that constitute the adsorbed layer, how is water thermally or non-thermally activated, and how do coadsorbates influence these properties of water. The attention paid to these and other fundamental questions in the past decade and a half has been immense. In this review, experimental studies published since the TM review are assimilated with those covered by TM to provide a current picture of the fundamental interactions of water with solid surfaces.« less

600 eV falcon-linac thomson x-ray source

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

Crane, J K; LeSage, G P; Ditmire, T

2000-12-15

The advent of 3rd generation light sources such as the Advanced Light Source (ALS) at LBL, and the Advanced Photon Source at Argonne, have produced a revolution in x-ray probing of dense matter during the past decade. These machines use electron-synchrotrons in conjunction with undulator stages to produce 100 psec x-ray pulses with photon energies of several kiloelectronvolts (keV). The applications for x-ray probing of matter are numerous and diverse with experiments in medicine and biology, semiconductors and materials science, and plasma and solid state physics. In spite of the success of the 3rd generation light sources there is strongmore » motivation to push the capabilities of x-ray probing into new realms, requiring shorter pulses, higher brightness and harder x-rays. A 4th generation light source, the Linac Coherent Light Source (LCLS), is being considered at the Stanford Linear Accelerator [1]. The LCLS will produce multi-kilovolt x-rays of subpicosecond duration that are 10 orders of magnitude brighter than today's 3rd generation light sources.[1] Although the LCLS will provide unprecedented capability for performing time-resolved x-ray probing of ultrafast phenomena at solid densities, this machine will not be completed for many years. In the meantime there is a serious need for an ultrashort-pulse, high-brightness, hard x-ray source that is capable of probing deep into high-Z solid materials to measure dynamic effects that occur on picosecond time scales. Such an instrument would be ideal for probing the effects of shock propagation in solids using Bragg and Laue diffraction. These techniques can be used to look at phase transitions, melting and recrystallization, and the propagation of defects and dislocations well below the surface in solid materials. [2] These types of dynamic phenomena undermine the mechanical properties of metals and are of general interest in solid state physics, materials science, metallurgy, and have specific relevance to stockpile stewardship. Another x-ray diagnostic technique, extended x-ray absorption fine structure (EXAFS) spectroscopy, can be used to measure small-scale structural changes to understand the underlying atomic physics associated with the formation of defects. [2]« less

Surface and bulk crystallization of amorphous solid water films: Confirmation of “top-down” crystallization

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

Yuan, Chunqing; Smith, R. Scott; Kay, Bruce D.

2016-01-11

Here, the crystallization kinetics of nanoscale amorphous solid water (ASW) films are investigated using temperature-programmed desorption (TPD) and reflection absorption infrared spectroscopy (RAIRS). TPD measurements are used to probe surface crystallization and RAIRS measurements are used to probe bulk crystallization. Isothermal TPD results show that surface crystallization is independent of the film thickness (from 100 to 1000 ML). Conversely, the RAIRS measurements show that the bulk crystallization time increases linearly with increasing film thickness. These results suggest that nucleation and crystallization begin at the ASW/vacuum interface and then the crystallization growth front propagates linearly into the bulk. This mechanism wasmore » confirmed by selective placement of an isotopic layer (5% D 2O in H 2O) at various positions in an ASW (H 2O) film. In this case, the closer the isotopic layer was to the vacuum interface, the earlier the isotopic layer crystallized. These experiments provide direct evidence to confirm that ASW crystallization in vacuum proceeds by a “top-down” crystallization mechanism.« less

ATR-FTIR Spectroscopy in the Undergraduate Chemistry Laboratory: Part II--A Physical Chemistry Laboratory Experiment on Surface Adsorption

ERIC Educational Resources Information Center

Schuttlefield, Jennifer D.; Larsen, Sarah C.; Grassian, Vicki H.

2008-01-01

Attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy is a useful technique for measuring the infrared spectra of solids and liquids as well as probing adsorption on particle surfaces. The use of FTIR-ATR spectroscopy in organic and inorganic chemistry laboratory courses as well as in undergraduate research was presented…

Optimization of monolithic columns for microfluidic devices

NASA Astrophysics Data System (ADS)

Pagaduan, Jayson V.; Yang, Weichun; Woolley, Adam T.

2011-06-01

Monolithic columns offer advantages as solid-phase extractors because they offer high surface area that can be tailored to a specific function, fast mass transport, and ease of fabrication. Porous glycidyl methacrylate-ethylene glycol dimethacrylate monoliths were polymerized in-situ in microfluidic devices, without pre-treatment of the poly(methyl methacrylate) channel surface. Cyclohexanol, 1-dodecanol and Tween 20 were used to control the pore size of the monoliths. The epoxy groups on the monolith surface can be utilized to immobilize target-specific probes such as antibodies, aptamers, or DNA for biomarker detection. Microfluidic devices integrated with solid-phase extractors should be useful for point-of-care diagnostics in detecting specific biomarkers from complex biological fluids.

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

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

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

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

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

PubMed

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

2016-12-13

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

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

DOE PAGES

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

2017-01-04

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

Characteristics of heat transfer fouling of thin stillage using model thin stillage and evaporator concentrates

NASA Astrophysics Data System (ADS)

Challa, Ravi Kumar

The US fuel ethanol demand was 50.3 billion liters (13.3 billion gallons) in 2012. Corn ethanol was produced primarily by dry grind process. Heat transfer equipment fouling occurs during corn ethanol production and increases the operating expenses of ethanol plants. Following ethanol distillation, unfermentables are centrifuged to separate solids as wet grains and liquid fraction as thin stillage. Evaporator fouling occurs during thin stillage concentration to syrup and decreases evaporator performance. Evaporators need to be shutdown to clean the deposits from the evaporator surfaces. Scheduled and unscheduled evaporator shutdowns decrease process throughput and results in production losses. This research were aimed at investigating thin stillage fouling characteristics using an annular probe at conditions similar to an evaporator in a corn ethanol production plant. Fouling characteristics of commercial thin stillage and model thin stillage were studied as a function of bulk fluid temperature and heat transfer surface temperature. Experiments were conducted by circulating thin stillage or carbohydrate mixtures in a loop through the test section which consisted of an annular fouling probe while maintaining a constant heat flux by electrical heating and fluid flow rate. The change in fouling resistance with time was measured. Fouling curves obtained for thin stillage and concentrated thin stillage were linear with time but no induction periods were observed. Fouling rates for concentrated thin stillage were higher compared to commercial thin stillage due to the increase in solid concentration. Fouling rates for oil skimmed and unskimmed concentrated thin stillage were similar but lower than concentrated thin stillage at 10% solids concentration. Addition of post fermentation corn oil to commercial thin stillage at 0.5% increments increased the fouling rates up to 1% concentration but decreased at 1.5%. As thin stillage is composed of carbohydrates, protein, lipid, fiber and minerals, simulated thin stillage was prepared with carbohydrate mixtures and tested for fouling rates. Induction period, maximum fouling resistance and mean fouling rates were determined. Two experiments were performed with two varieties of starch, waxy and high amylose and short chain carbohydrates, corn syrup solids and glucose. Interaction effects of glucose with starch varieties were studied. In the first experiment, short chain carbohydrates individual and interaction effects with starch were studied. For mixtures prepared from glucose and corn syrup solids, no fouling was observed. Mixtures prepared from starch, a long glucose polymer, showed marked fouling. Corn syrup solids and glucose addition to pure starch decreased the mean fouling rates and maximum fouling resistances. Between corn syrup solids and glucose, starch fouling rates were reduced with addition of glucose. Induction periods of pure mixtures of either glucose or corn syrup solids were longer than the test period (5 h). Pure starch mixture had no induction period. Maximum fouling resistance was higher for mixtures with higher concentration of longer polymers. Waxy starch had a longer induction period than high amylose starch. Maximum fouling resistance was higher for waxy than high amylose starch. Addition of glucose to waxy or high amylose starch increased induction period of mixtures longer than 5 h test period. It appears that the bulk fluid temperature plays an important role on carbohydrate mixture fouling rates. Higher bulk fluid temperatures increased the initial fouling rates of the carbohydrate mixtures. Carbohydrate type, depending on the polymer length, influenced the deposit formation. Longer chain carbohydrate, starch, had higher fouling rates compared to shorter carbohydrates such as glucose and corn syrup solids. For insoluble carbohydrate mixtures, fouling was severe. As carbohydrate solubility increased with bulk fluid temperature, surface reaction increased at probe surface and resulted in deposit formation. Higher surface temperatures eliminated induction periods for thin stillage and fouling was rapid on probe surface.

Critical evaluation of dipolar, acid-base and charge interactions I. Electron displacement within and between molecules, liquids and semiconductors.

PubMed

Rosenholm, Jarl B

2017-09-01

Specific dipolar, acid-base and charge interactions involve electron displacements. For atoms, single bonds and molecules electron displacement is characterized by electronic potential, absolute hardness, electronegativity and electron gap. In addition, dissociation, bonding, atomization, formation, ionization, affinity and lattice enthalpies are required to quantify the electron displacement in solids. Semiconductors are characterized by valence and conduction band energies, electron gaps and average Fermi energies which in turn determine Galvani potentials of the bulk, space charge layer and surface states. Electron displacement due to interaction between (probe) molecules, liquids and solids are characterized by parameters such as Hamaker constant, solubility parameter, exchange energy density, surface tension, work of adhesion and immersion. They are determined from permittivity, refractive index, enthalpy of vaporization, molar volume, surface pressure and contact angle. Moreover, acidic and basic probes may form adducts which are adsorbed on target substrates in order to establish an indirect measure of polarity, acidity, basicity or hydrogen bonding. Acidic acceptor numbers (AN), basic donor numbers (DN), acidic and basic "electrostatic" (E) and "covalent" (C) parameters determined by enthalpy of adduct formation are considered as general acid-base scales. However, the formal grounds for assignments as dispersive, Lifshitz-van der Waals, polar, acid, base and hydrogen bond interactions are inconsistent. Although correlations are found no of the parameters are mutually fully compatible and moreover the enthalpies of acid-base interaction do not correspond to free energies. In this review the foundations of different acid-base parameters relating to electron displacement within and between (probe) molecules, liquids and (semiconducting) solids are thoroughly investigated and their mutual relationships are evaluated. Copyright © 2017 Elsevier B.V. All rights reserved.

Ultrafast control and monitoring of material properties using terahertz pulses

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

Bowlan, Pamela Renee

These are a set of slides on ultrafast control and monitoring of material properties using terahertz pulses. A few of the topics covered in these slides are: How fast is a femtosecond (fs), Different frequencies probe different properties of molecules or solids, What can a THz pulse do to a material, Ultrafast spectroscopy, Generating and measuring ultrashort THz pulses, Tracking ultrafast spin dynamics in antiferromagnets through spin wave resonances, Coherent two-dimensional THz spectroscopy, and Probing vibrational dynamics at a surface. Conclusions are: Coherent two-dimensional THz spectroscopy: a powerful approach for studying coherence and dynamics of low energy resonances. Applying thismore » to graphene we investigated the very strong THz light mater interaction which dominates over scattering. Useful for studying coupled excitations in multiferroics and monitoring chemical reactions. Also, THz-pump, SHG-probe spectoscopy: an ultrafast, surface sensitive probe of atomic-scale symmetry changes and nonlinear phonon dymanics. We are using this in Bi 2Se 3 to investigate the nonlinear surface phonon dynamics. This is potentially very useful for studying catalysis.« less

Surface topographical changes measured by phase-locked interferometry

NASA Technical Reports Server (NTRS)

Lauer, J. L.; Fung, S. S.

1984-01-01

An electronic optical laser interferometer capable of resolving depth differences of as low as 30 A and planar displacements of 6000 A was constructed to examine surface profiles of bearing surfaces without physical contact. Topological chemical reactivity was determined by applying a drop of dilute alcoholic hydrochloric acid and measuring the profile of the solid surface before and after application of this probe. Scuffed bearing surfaces reacted much faster than virgin ones but that bearing surfaces exposed to lubricants containing an organic chloride reacted much more slowly. The reactivity of stainless steel plates, heated in a nitrogen atmosphere to different temperatures, were examined later at ambient temperature. The change of surface contour as a result of the probe reaction followed Arrhenius-type relation with respect to heat treatment temperature. The contact area of the plate of a ball/plate sliding elastohydrodynamic contact run on trimethylopropane triheptanoate with or without additives was optically profiled periodically. As scuffing was approached, the change of profile within the contact region changed much more rapidly by the acid probe and assumed a constant high value after scuffing. A nonetching metallurgical phase was found in the scuff mark, which was apparently responsible for the high reactivity.

Probing Intrawire, Interwire, and Diameter-Dependent Variations in Silicon Nanowire Surface Trap Density with Pump-Probe Microscopy.

PubMed

Cating, Emma E M; Pinion, Christopher W; Christesen, Joseph D; Christie, Caleb A; Grumstrup, Erik M; Cahoon, James F; Papanikolas, John M

2017-10-11

Surface trap density in silicon nanowires (NWs) plays a key role in the performance of many semiconductor NW-based devices. We use pump-probe microscopy to characterize the surface recombination dynamics on a point-by-point basis in 301 silicon NWs grown using the vapor-liquid-solid (VLS) method. The surface recombination velocity (S), a metric of the surface quality that is directly proportional to trap density, is determined by the relationship S = d/4τ from measurements of the recombination lifetime (τ) and NW diameter (d) at distinct spatial locations in individual NWs. We find that S varies by as much as 2 orders of magnitude between NWs grown at the same time but varies only by a factor of 2 or three within an individual NW. Although we find that, as expected, smaller-diameter NWs exhibit shorter τ, we also find that smaller wires exhibit higher values of S; this indicates that τ is shorter both because of the geometrical effect of smaller d and because of a poorer quality surface. These results highlight the need to consider interwire heterogeneity as well as diameter-dependent surface effects when fabricating NW-based devices.

Ice Surfaces.

PubMed

Shultz, Mary Jane

2017-05-05

Ice is a fundamental solid with important environmental, biological, geological, and extraterrestrial impact. The stable form of ice at atmospheric pressure is hexagonal ice, I h . Despite its prevalence, I h remains an enigmatic solid, in part due to challenges in preparing samples for fundamental studies. Surfaces of ice present even greater challenges. Recently developed methods for preparation of large single-crystal samples make it possible to reproducibly prepare any chosen face to address numerous fundamental questions. This review describes preparation methods along with results that firmly establish the connection between the macroscopic structure (observed in snowflakes, microcrystallites, or etch pits) and the molecular-level configuration (detected with X-ray or electron scattering techniques). Selected results of probing interactions at the ice surface, including growth from the melt, surface vibrations, and characterization of the quasi-liquid layer, are discussed.

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

Nave, S.E.

Recent advances in fiber optics, diode lasers, CCD detectors, dielectric and holographic optical filters, grating spectrometers, and chemometric data analysis have greatly simplified Raman spectroscopy. In order to make a rugged fiber optic Raman probe for solids/slurries like these at Savannah River, we have designed a probe that eliminates as many optical elements and surfaces as possible. The diffuse reflectance probe tip is modified for Raman scattering by installing thin dielectric in-line filters. Effects of each filter are shown for the NaNO{sub 3} Raman spectrum. By using a diode laser excitation at 780 nm, fluorescence is greatly reduced, and excellentmore » spectra may be obtained from organic solids. At SRS, fiber optic Raman probes are being developed for in situ chemical mapping of radioactive waste storage tanks. Radiation darkening of silica fiber optics is negligible beyond 700 nm. Corrosion resistance is being evaluated. Analysis of process gas (off-gas from SRS processes) is investigated in some detail: hydrogen in nitrogen with NO{sub 2} interference. Other applications and the advantages of the method are pointed out briefly.« less

Carbon-Based Solid-State Calcium Ion-Selective Microelectrode and Scanning Electrochemical Microscopy: A Quantitative Study of pH-Dependent Release of Calcium Ions from Bioactive Glass.

PubMed

Ummadi, Jyothir Ganesh; Downs, Corey J; Joshi, Vrushali S; Ferracane, Jack L; Koley, Dipankar

2016-03-15

Solid-state ion-selective electrodes are used as scanning electrochemical microscope (SECM) probes because of their inherent fast response time and ease of miniaturization. In this study, we report the development of a solid-state, low-poly(vinyl chloride), carbon-based calcium ion-selective microelectrode (Ca(2+)-ISME), 25 μm in diameter, capable of performing an amperometric approach curve and serving as a potentiometric sensor. The Ca(2+)-ISME has a broad linear response range of 5 μM to 200 mM with a near Nernstian slope of 28 mV/log[a(Ca(2+))]. The calculated detection limit for Ca(2+)-ISME is 1 μM. The selectivity coefficients of this Ca(2+)-ISME are log K(Ca(2+),A) = -5.88, -5.54, and -6.31 for Mg(2+), Na(+), and K(+), respectively. We used this new type of Ca(2+)-ISME as an SECM probe to quantitatively map the chemical microenvironment produced by a model substrate, bioactive glass (BAG). In acidic conditions (pH 4.5), BAG was found to increase the calcium ion concentration from 0.7 mM ([Ca(2+)] in artificial saliva) to 1.4 mM at 20 μm above the surface. In addition, a solid-state dual SECM pH probe was used to correlate the release of calcium ions with the change in local pH. Three-dimensional pH and calcium ion distribution mapping were also obtained by using these solid-state probes. The quantitative mapping of pH and Ca(2+) above the BAG elucidates the effectiveness of BAG in neutralizing and releasing calcium ions in acidic conditions.

Investigation on Dynamic Calibration for an Optical-Fiber Solids Concentration Probe in Gas-Solid Two-Phase Flows

PubMed Central

Xu, Guiling; Liang, Cai; Chen, Xiaoping; Liu, Daoyin; Xu, Pan; Shen, Liu; Zhao, Changsui

2013-01-01

This paper presents a review and analysis of the research that has been carried out on dynamic calibration for optical-fiber solids concentration probes. An introduction to the optical-fiber solids concentration probe was given. Different calibration methods of optical-fiber solids concentration probes reported in the literature were reviewed. In addition, a reflection-type optical-fiber solids concentration probe was uniquely calibrated at nearly full range of the solids concentration from 0 to packed bed concentration. The effects of particle properties (particle size, sphericity and color) on the calibration results were comprehensively investigated. The results show that the output voltage has a tendency to increase with the decreasing particle size, and the effect of particle color on calibration result is more predominant than that of sphericity. PMID:23867745

How to distinguish various components of the SHG signal recorded from the solid/liquid interface?

NASA Astrophysics Data System (ADS)

Gassin, Pierre-Marie; Martin-Gassin, Gaelle; Prelot, Benedicte; Zajac, Jerzy

2016-11-01

Second harmonic generation (SHG) may be an important tool to probe buried solid/liquid interfaces because of its inherent surface sensitivity. A detailed interpretation of dye adsorption onto Si-SiO2 wafer is not straightforward because both adsorbent and adsorbate contribute to the overall SHG signal. The polarization resolved SHG analysis points out that the adsorbent and adsorbate contributions are out of phase by π/2 in the present system. The surface nonlinear susceptibility χ(2) represents thus a complex tensor in which its real part is related to the adsorbent contribution and its imaginary part to the adsorbate one.

The birth and evolution of surface science: child of the union of science and technology.

PubMed

Duke, C B

2003-04-01

This article is an account of the birth and evolution of surface science as an interdisciplinary research area. Surface science emanated from the confluence of concepts and tools in physics and chemistry with technological innovations that made it possible to determine the structure and properties of surfaces and interfaces and the dynamics of chemical reactions at surfaces. The combination in the 1960s and 1970s of ultra-high-vacuum (i.e., P < 10(-7) Pascal or 10(-9) Torr) technology with the recognition that electrons in the energy range from 50 to 500 eV exhibited inelastic collision mean free paths of the order of a few angstroms fostered an explosion of activity. The results were a reformulation of the theory of electron solid scattering, the nearly universal use of electron spectroscopies for surface characterization, the rise of surface science as an independent interdisciplinary research area, and the emergence of the American Vacuum Society (AVS) as a major international scientific society. The rise of microelectronics in the 1970s and 1980s resulted in huge increases in computational power. These increases enabled more complex experiments and the utilization of density functional theory for the quantitative prediction of surface structure and dynamics. Development of scanning-probe microscopies in the 1990s led to atomic-resolution images of macroscopic surfaces and interfaces as well as videos of atoms moving about on surfaces during growth and diffusion. Scanning probes have since brought solid-liquid interfaces into the realm of atomic-level surface science, expanding its scope to more complex systems, including fragile biological materials and processes.

Microscopic contour changes of tribological surfaces by chemical and mechanical action

NASA Technical Reports Server (NTRS)

Lauer, J. L.; Fung, S. S.

1982-01-01

An electronic optical laser interferometer capable of resolving depth differences of as low as 30 A and planar displacements of 6000 A was constructed for the examination of surface profiles of bearing surfaces without physical contact. This instrument was used to determine topological chemical reactivity by applying a drop of dilute alcoholic hydrochloric acid and measuring the profile of the solid surface before and after application of this probe. It was found that scuffed bearing surfaces reacted much faster than virgin ones but that bearing surfaces exposed to lubricants containing an organic chloride reacted much more slowly. In a separate series of experiments, a number of stainless steel plates were heated in a nitrogen atmosphere to different temperatures and their reactivity examined later at ambient temperature. The change of surface contour as a result of the probe reaction was found to follow an Arrhenius-type relation with respect to heat treatment temperature. This result could have implications on the scuffing mechanism.

Novel Single-Cell Analysis Platform Based on a Solid-State Zinc-Coadsorbed Carbon Quantum Dots Electrochemiluminescence Probe for the Evaluation of CD44 Expression on Breast Cancer Cells.

PubMed

Qiu, Youyi; Zhou, Bin; Yang, Xiaojuan; Long, Dongping; Hao, Yan; Yang, Peihui

2017-05-24

A novel single-cell analysis platform was fabricated using solid-state zinc-coadsorbed carbon quantum dot (ZnCQDs) nanocomposites as an electrochemiluminescence (ECL) probe for the detection of breast cancer cells and evaluation of the CD44 expression level. Solid-state ZnCQDs nanocomposite probes were constructed through the attachment of ZnCQDs to gold nanoparticles and then the loading of magnetic beads to amplify the ECL signal, exhibiting a remarkable 120-fold enhancement of the ECL intensity. Hyaluronic acid (HA)-functionalized solid-state probes were used to label a single breast cancer cell by the specific recognition of HA with CD44 on the cell surface, revealing more stable, sensitive, and effective tagging in comparison with the water-soluble CQDs. This strategy exhibited a good analytical performance for the analysis of MDA-MB-231 and MCF-7 single cells with linear range from 1 to 18 and from 1 to 12 cells, respectively. Furthermore, this single-cell analysis platform was used for evaluation of the CD44 expression level of these two cell lines, in which the MDA-MB-231 cells revealed a 2.8-5.2-fold higher CD44 expression level. A total of 20 single cells were analyzed individually, and the distributions of the ECL intensity revealed larger variations, indicating the high cellular heterogeneity of the CD44 expression level on the same cell line. The as-proposed single-cell analysis platform might provide a novel protocol to effectively study the individual cellular function and cellular heterogeneity.

Probing ultrafast dynamics of solid-density plasma generated by high-contrast intense laser pulses

NASA Astrophysics Data System (ADS)

Jana, Kamalesh; Blackman, David R.; Shaikh, Moniruzzaman; Lad, Amit D.; Sarkar, Deep; Dey, Indranuj; Robinson, Alex P. L.; Pasley, John; Ravindra Kumar, G.

2018-01-01

We present ultrafast dynamics of solid-density plasma created by high-contrast (picosecond contrast ˜10-9), high-intensity (˜4 × 1018 W/cm2) laser pulses using time-resolved pump-probe Doppler spectrometry. Experiments show a rapid rise in blue-shift at early time delay (2-4.3 ps) followed by a rapid fall (4.3-8.3 ps) and then a slow rise in blue-shift at later time delays (>8.3 ps). Simulations show that the early-time observations, specifically the absence of any red-shifting of the reflected probe, can only be reproduced if the front surface is unperturbed by the laser pre-pulse at the moment that the high intensity pulse arrives. A flexible diagnostic which is capable of diagnosing the presence of low-levels of pre-plasma formation would be useful for potential applications in laser-produced proton and ion production, such as cancer therapy and security imaging.

Extreme ultraviolet interferometry of warm dense matter in laser plasmas.

PubMed

Gartside, L M R; Tallents, G J; Rossall, A K; Wagenaars, E; Whittaker, D S; Kozlová, M; Nejdl, J; Sawicka, M; Polan, J; Kalal, M; Rus, B

2010-11-15

We demonstrate that interferometric probing with extreme ultraviolet (EUV) laser light enables determination of the degree of ionization of the "warm dense matter" produced between the critical and ablation surfaces of laser plasmas. Interferometry has been utilized to measure both transmission and phase information for an EUV laser beam at the photon energy of 58.5 eV, probing longitudinally through laser-irradiated plastic (parylene-N) targets (thickness 350 nm) irradiated by a 300 ps duration pulse of wavelength 438 nm and peak irradiance 10(12) W cm(-2). The transmission of the EUV probe beam provides a measure of the rate of target ablation, as ablated plasma becomes close to transparent when the photon energy is less than the ionization energy of the predominant ion species. We show that refractive indices η below the solid parylene N (η(solid) = 0.946) and expected plasma values are produced in the warm dense plasma created by laser irradiation due to bound-free absorption in C(+).

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

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

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

2016-06-15

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

Study of plasma-facing components in the Lithium Tokamak Experiment with the Materials Analysis and Particle Probe

NASA Astrophysics Data System (ADS)

Lucia, M.; Kaita, R.; Majeski, R.; Boyle, D. P.; Granstedt, E. M.; Jacobson, C. M.; Schmitt, J. C.; Allain, J. P.; Bedoya, F.; Gonderman, S.

2013-10-01

The Lithium Tokamak Experiment (LTX) is a spherical torus designed to accommodate solid or liquid lithium as the primary plasma-facing component (PFC). We present initial results from the implementation on LTX of the Materials Analysis and Particle Probe (MAPP) diagnostic, a collaboration among PPPL, Purdue University, and the University of Illinois. MAPP is a compact in vacuo surface science diagnostic, and its operation on LTX will provide the first ever in situ surface measurements of a tokamak first wall environment. With MAPP's analysis techniques, we will study the evolution of the surface chemistry of LTX's first wall as a function of varied temperature and lithium coating. During its 2013 run campaign, LTX will use an electron beam to evaporate lithium onto the first wall from an in-vessel reservoir. We will use two quartz crystal microbalances to estimate thickness of lithium coatings thus applied to the MAPP probe. We have recently installed a set of triple Langmuir probes on LTX, and they will be used to relate LTX edge plasma parameters to MAPP results. We will combine data from MAPP and the triple probes to estimate the local edge recycling coefficient based on desorption of retained hydrogen. This work was supported by U.S. DOE contract DE-AC02-09CH11466.

Non-invasive, transient determination of the core temperature of a heat-generating solid body

PubMed Central

Anthony, Dean; Sarkar, Daipayan; Jain, Ankur

2016-01-01

While temperature on the surface of a heat-generating solid body can be easily measured using a variety of methods, very few techniques exist for non-invasively measuring the temperature inside the solid body as a function of time. Measurement of internal temperature is very desirable since measurement of just the surface temperature gives no indication of temperature inside the body, and system performance and safety is governed primarily by the highest temperature, encountered usually at the core of the body. This paper presents a technique to non-invasively determine the internal temperature based on the theoretical relationship between the core temperature and surface temperature distribution on the outside of a heat-generating solid body as functions of time. Experiments using infrared thermography of the outside surface of a thermal test cell in a variety of heating and cooling conditions demonstrate good agreement of the predicted core temperature as a function of time with actual core temperature measurement using an embedded thermocouple. This paper demonstrates a capability to thermally probe inside solid bodies in a non-invasive fashion. This directly benefits the accurate performance prediction and control of a variety of engineering systems where the time-varying core temperature plays a key role. PMID:27804981

Non-invasive, transient determination of the core temperature of a heat-generating solid body

NASA Astrophysics Data System (ADS)

Anthony, Dean; Sarkar, Daipayan; Jain, Ankur

2016-11-01

While temperature on the surface of a heat-generating solid body can be easily measured using a variety of methods, very few techniques exist for non-invasively measuring the temperature inside the solid body as a function of time. Measurement of internal temperature is very desirable since measurement of just the surface temperature gives no indication of temperature inside the body, and system performance and safety is governed primarily by the highest temperature, encountered usually at the core of the body. This paper presents a technique to non-invasively determine the internal temperature based on the theoretical relationship between the core temperature and surface temperature distribution on the outside of a heat-generating solid body as functions of time. Experiments using infrared thermography of the outside surface of a thermal test cell in a variety of heating and cooling conditions demonstrate good agreement of the predicted core temperature as a function of time with actual core temperature measurement using an embedded thermocouple. This paper demonstrates a capability to thermally probe inside solid bodies in a non-invasive fashion. This directly benefits the accurate performance prediction and control of a variety of engineering systems where the time-varying core temperature plays a key role.

Immobilized enzymes: understanding enzyme - surface interactions at the molecular level.

PubMed

Hoarau, Marie; Badieyan, Somayesadat; Marsh, E Neil G

2017-11-22

Enzymes immobilized on solid supports have important and industrial and medical applications. However, their uses are limited by the significant reductions in activity and stability that often accompany the immobilization process. Here we review recent advances in our understanding of the molecular level interactions between proteins and supporting surfaces that contribute to changes in stability and activity. This understanding has been facilitated by the application of various surface-sensitive spectroscopic techniques that allow the structure and orientation of enzymes at the solid/liquid interface to be probed, often with monolayer sensitivity. An appreciation of the molecular interactions between enzyme and surface support has allowed the surface chemistry and method of enzyme attachement to be fine-tuned such that activity and stability can be greatly enhanced. These advances suggest that a much wider variety of enzymes may eventually be amenable to immobilization as green catalysts.

In situ solid-state electrochemistry of mass-selected ions at well-defined electrode–electrolyte interfaces

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

Prabhakaran, Venkateshkumar; Johnson, Grant E.; Wang, Bingbing

2016-11-07

Molecular-level understanding of electrochemical processes occurring at electrode-electrolyte interfaces (EEI) is key to the rational development of high-performance and sustainable electrochemical technologies. This article reports the development and first application of solid-state in situ electrochemical probes to study redox and catalytic processes occurring at well-defined EEI generated using soft-landing of mass- and charge-selected cluster ions (SL). In situ electrochemical probes with excellent mass transfer properties are fabricated using carefully-designed nanoporous ionic liquid membranes. SL enables deposition of pure active species that are not obtainable with other techniques onto electrode surfaces with precise control over charge state, composition, and kinetic energy.more » SL is, therefore, a unique tool for studying fundamental processes occurring at EEI. For the first time using an aprotic electrochemical probe, the effect of charge state (PMo12O403-/2-) and the contribution of building blocks of Keggin polyoxometalate (POM) clusters to redox processes are characterized by populating EEI with novel POM anions generated by electrospray ionization and gas phase dissociation. Additionally, a proton conducting electrochemical probe has been developed to characterize the reactive electrochemistry (oxygen reduction activity) of bare Pt clusters (Pt40 ~1 nm diameter), thus demonstrating the capability of the probe for studying reactions in controlled gaseous environments. The newly developed in situ electrochemical probes combined with ion SL provide a versatile method to characterize the EEI in solid-state redox systems and reactive electrochemistry at precisely-defined conditions. This capability will advance molecular-level understanding of processes occurring at EEI that are critical to many energy-related technologies.« less

Probing viscoelastic surfaces with bimodal tapping-mode atomic force microscopy: Underlying physics and observables for a standard linear solid model.

PubMed

Solares, Santiago D

2014-01-01

This paper presents computational simulations of single-mode and bimodal atomic force microscopy (AFM) with particular focus on the viscoelastic interactions occurring during tip-sample impact. The surface is modeled by using a standard linear solid model, which is the simplest system that can reproduce creep compliance and stress relaxation, which are fundamental behaviors exhibited by viscoelastic surfaces. The relaxation of the surface in combination with the complexities of bimodal tip-sample impacts gives rise to unique dynamic behaviors that have important consequences with regards to the acquisition of quantitative relationships between the sample properties and the AFM observables. The physics of the tip-sample interactions and its effect on the observables are illustrated and discussed, and a brief research outlook on viscoelasticity measurement with intermittent-contact AFM is provided.

Pressure cell for investigations of solid-liquid interfaces by neutron reflectivity.

PubMed

Kreuzer, Martin; Kaltofen, Thomas; Steitz, Roland; Zehnder, Beat H; Dahint, Reiner

2011-02-01

We describe an apparatus for measuring scattering length density and structure of molecular layers at planar solid-liquid interfaces under high hydrostatic pressure conditions. The device is designed for in situ characterizations utilizing neutron reflectometry in the pressure range 0.1-100 MPa at temperatures between 5 and 60 °C. The pressure cell is constructed such that stratified molecular layers on crystalline substrates of silicon, quartz, or sapphire with a surface area of 28 cm(2) can be investigated against noncorrosive liquid phases. The large substrate surface area enables reflectivity to be measured down to 10(-5) (without background correction) and thus facilitates determination of the scattering length density profile across the interface as a function of applied load. Our current interest is on the stability of oligolamellar lipid coatings on silicon surfaces against aqueous phases as a function of applied hydrostatic pressure and temperature but the device can also be employed to probe the structure of any other solid-liquid interface.

Real-time and label-free ring-resonator monitoring of solid-phase recombinase polymerase amplification.

PubMed

Sabaté Del Río, Jonathan; Steylaerts, Tim; Henry, Olivier Y F; Bienstman, Peter; Stakenborg, Tim; Van Roy, Wim; O'Sullivan, Ciara K

2015-11-15

In this work we present the use of a silicon-on-insulator (SOI) chip featuring an array of 64 optical ring resonators used as refractive index sensors for real-time and label-free DNA detection. Single ring functionalisation was achieved using a click reaction after precise nanolitre spotting of specific hexynyl-terminated DNA capture probes to link to an azido-silanised chip surface. To demonstrate detectability using the ring resonators and to optimise conditions for solid-phase amplification, hybridisation between short 25-mer single stranded DNA (ssDNA) fragments and a complementary capture probe immobilised on the surface of the ring resonators was carried out and detected through the shift in the resonant wavelength. Using the optimised conditions demonstrated via the solid-phase hybridisation, a 144-bp double stranded DNA (dsDNA) was then detected directly using recombinase and polymerase proteins through on-chip target amplification and solid-phase elongation of immobilised forward primers on specific rings, at a constant temperature of 37°C and in less than 60min, achieving a limit of detection of 7.8·10(-13)M (6·10(5) copies in 50µL). The use of an automatic liquid handler injection instrument connected to an integrated resealable chip interface (RCI) allowed programmable multiple injection protocols. Air plugs between different solutions were introduced to prevent intermixing and a proportional-integral-derivative (PID) temperature controller minimised temperature based drifts. Published by Elsevier B.V.

Contact Dependence and Velocity Crossover in Friction between Microscopic Solid/Solid Contacts.

PubMed

McGraw, Joshua D; Niguès, Antoine; Chennevière, Alexis; Siria, Alessandro

2017-10-11

Friction at the nanoscale differs markedly from that between surfaces of macroscopic extent. Characteristically, the velocity dependence of friction between apparent solid/solid contacts can strongly deviate from the classically assumed velocity independence. Here, we show that a nondestructive friction between solid tips with radius on the scale of hundreds of nanometers and solid hydrophobic self-assembled monolayers has a strong velocity dependence. Specifically, using laterally oscillating quartz tuning forks, we observe a linear scaling in the velocity at the lowest accessed velocities, typically hundreds of micrometers per second, crossing over into a logarithmic velocity dependence. This crossover is consistent with a general multicontact friction model that includes thermally activated breaking of the contacts at subnanometric elongation. We find as well a strong dependence of the friction on the dimensions of the frictional probe.

ATR-FTIR Spectroscopy in the Undergraduate Chemistry Laboratory: Part I--Fundamentals and Examples

ERIC Educational Resources Information Center

Schuttlefield, Jennifer D.; Grassian, Vicki H.

2008-01-01

Attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy is a useful technique for measuring the infrared spectra of solids and liquids as well as probing adsorption on particle surfaces. Several examples of the use of FTIR-ATR spectroscopy in different undergraduate chemistry laboratory courses are presented here. These…

Studies of minute quantities of natural abundance molecules using 2D heteronuclear correlation spectroscopy under 100kHz MAS

DOE PAGES

Nishiyama, Y.; Kobayashi, T.; Malon, M.; ...

2015-02-16

Two-dimensional 1H{ 13C} heteronuclear correlation solid-state NMR spectra of naturally abundant solid materials are presented, acquired using the 0.75-mm magic angle spinning (MAS) probe at spinning rates up to 100 kHz. In spite of the miniscule sample volume (290 nL), high-quality HSQC-type spectra of bulk samples as well as surface-bound molecules can be obtained within hours of experimental time. The experiments are compared with those carried out at 40 kHz MAS using a 1.6-mm probe, which offered higher overall sensitivity due to a larger rotor volume. The benefits of ultrafast MAS in such experiments include superior resolution in 1H dimensionmore » without resorting to 1H– 1H homonuclear RF decoupling, easy optimization, and applicability to mass-limited samples. As a result, the HMQC spectra of surface-bound species can be also acquired under 100 kHz MAS, although the dephasing of transverse magnetization has significant effect on the efficiency transfer under MAS alone.« less

Colossal super saturation of oxygen at the iron-aluminum interfaces fabricated using solid state welding

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

Sridharan, Niyanth; Isheim, D.; Seidman, David N.

Solid state joining is achieved in three steps, (i) interface asperity deformation, (ii) oxide dispersion, followed by (iii) atomic contact and bonding. Atomically clean metallic surfaces without an oxide layer bond spontaneously. Despite its importance the oxide dispersion mechanism is not well studied. In this work the first ever atom probe study of iron-aluminum solid state welds show that the oxygen concentration at the interface is 20 at.%. This is significantly lower than any equilibrium oxide concentration. Here, we therefore propose that the high-strain rate deformation at the interfaces renders the oxide unstable resulting in the observed concentration of oxygen.

Colossal super saturation of oxygen at the iron-aluminum interfaces fabricated using solid state welding

DOE PAGES

Sridharan, Niyanth; Isheim, D.; Seidman, David N.; ...

2016-12-14

Solid state joining is achieved in three steps, (i) interface asperity deformation, (ii) oxide dispersion, followed by (iii) atomic contact and bonding. Atomically clean metallic surfaces without an oxide layer bond spontaneously. Despite its importance the oxide dispersion mechanism is not well studied. In this work the first ever atom probe study of iron-aluminum solid state welds show that the oxygen concentration at the interface is 20 at.%. This is significantly lower than any equilibrium oxide concentration. Here, we therefore propose that the high-strain rate deformation at the interfaces renders the oxide unstable resulting in the observed concentration of oxygen.

The influence of water on the nanomechanical behavior of the plant biopolyester cutin as studied by AFM and solid-state NMR.

PubMed

Round, A N; Yan, B; Dang, S; Estephan, R; Stark, R E; Batteas, J D

2000-11-01

Atomic force microscopy and solid-state nuclear magnetic resonance have been used to investigate the effect of water absorption on the nanoscale elastic properties of the biopolyester, cutin, isolated from tomato fruit cuticle. Changes in the humidity and temperature at which fruits are grown or stored can affect the plant surface (cuticle) and modify its susceptibility to pathogenic attack by altering the cuticle's rheological properties. In this work, atomic force microscopy measurements of the surface mechanical properties of isolated plant cutin have been made as a first step to probing the impact of water uptake from the environment on surface flexibility. A dramatic decrease in surface elastic modulus (from approximately 32 to approximately 6 MPa) accompanies increases in water content as small as 2 wt %. Complementary solid-state nuclear magnetic resonance measurements reveal enhanced local mobility of the acyl chain segments with increasing water content, even at molecular sites remote from the covalent cross-links that are likely to play a crucial role in cutin's elastic properties.

Direct Electrospray Ionization Mass Spectrometric Profiling of Real-World Samples via a Solid Sampling Probe

NASA Astrophysics Data System (ADS)

Yu, Zhan; Chen, Lee Chuin; Mandal, Mridul Kanti; Yoshimura, Kentaro; Takeda, Sen; Hiraoka, Kenzo

2013-10-01

This study presents a novel direct analysis strategy for rapid mass spectrometric profiling of biochemicals in real-world samples via a direct sampling probe (DSP) without sample pretreatments. Chemical modification is applied to a disposable stainless steel acupuncture needle to enhance its surface area and hydrophilicity. After insertion into real-world samples, biofluid can be attached on the DSP surface. With the presence of a high DC voltage and solvent vapor condensing on the tip of the DSP, analyte can be dissolved and electrosprayed. The simplicity in design, versatility in application aspects, and other advantages such as low cost and disposability make this new method a competitive tool for direct analysis of real-world samples.

Probing viscoelastic surfaces with bimodal tapping-mode atomic force microscopy: Underlying physics and observables for a standard linear solid model

PubMed Central

2014-01-01

Summary This paper presents computational simulations of single-mode and bimodal atomic force microscopy (AFM) with particular focus on the viscoelastic interactions occurring during tip–sample impact. The surface is modeled by using a standard linear solid model, which is the simplest system that can reproduce creep compliance and stress relaxation, which are fundamental behaviors exhibited by viscoelastic surfaces. The relaxation of the surface in combination with the complexities of bimodal tip–sample impacts gives rise to unique dynamic behaviors that have important consequences with regards to the acquisition of quantitative relationships between the sample properties and the AFM observables. The physics of the tip–sample interactions and its effect on the observables are illustrated and discussed, and a brief research outlook on viscoelasticity measurement with intermittent-contact AFM is provided. PMID:25383277

A Surface Science Paradigm for a Post-Huygens Titan Mission

NASA Technical Reports Server (NTRS)

Zimmerman, Wayne F.; Lunine, Jonathan; Lorenz, Ralph

2005-01-01

With the Cassini-Huygens atmospheric probe drop-off mission fast approaching, it is essential that scientists and engineers start scoping potential follow-on surface science missions. This paper provides a summary of the first year of a two year design study which examines in detail the desired surface science measurements and resolution, potential instrument suite, and complete payload delivery system. Also provided are design concepts for both an aerial inflatable mobility platform and deployable instrument sonde. The tethered deployable sonde provides the capability to sample near surface atmosphere, sub-surface liquid (if it exists), and surface solid material. Actual laboratory tests of the amphibious sonde prototype are also presented.

Water at surfaces with tunable surface chemistries

NASA Astrophysics Data System (ADS)

Sanders, Stephanie E.; Vanselous, Heather; Petersen, Poul B.

2018-03-01

Aqueous interfaces are ubiquitous in natural environments, spanning atmospheric, geological, oceanographic, and biological systems, as well as in technical applications, such as fuel cells and membrane filtration. Where liquid water terminates at a surface, an interfacial region is formed, which exhibits distinct properties from the bulk aqueous phase. The unique properties of water are governed by the hydrogen-bonded network. The chemical and physical properties of the surface dictate the boundary conditions of the bulk hydrogen-bonded network and thus the interfacial properties of the water and any molecules in that region. Understanding the properties of interfacial water requires systematically characterizing the structure and dynamics of interfacial water as a function of the surface chemistry. In this review, we focus on the use of experimental surface-specific spectroscopic methods to understand the properties of interfacial water as a function of surface chemistry. Investigations of the air-water interface, as well as efforts in tuning the properties of the air-water interface by adding solutes or surfactants, are briefly discussed. Buried aqueous interfaces can be accessed with careful selection of spectroscopic technique and sample configuration, further expanding the range of chemical environments that can be probed, including solid inorganic materials, polymers, and water immiscible liquids. Solid substrates can be finely tuned by functionalization with self-assembled monolayers, polymers, or biomolecules. These variables provide a platform for systematically tuning the chemical nature of the interface and examining the resulting water structure. Finally, time-resolved methods to probe the dynamics of interfacial water are briefly summarized before discussing the current status and future directions in studying the structure and dynamics of interfacial water.

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

NASA Astrophysics Data System (ADS)

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

2000-05-01

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

A photo-cleavable biotin affinity tag for the facile release of a photo-crosslinked carbohydrate-binding protein.

PubMed

Chang, Tsung-Che; Adak, Avijit K; Lin, Ting-Wei; Li, Pei-Jhen; Chen, Yi-Ju; Lai, Chain-Hui; Liang, Chien-Fu; Chen, Yu-Ju; Lin, Chun-Cheng

2016-03-15

The use of photo-crosslinking glycoprobes represents a powerful strategy for the covalent capture of labile protein complexes and allows detailed characterization of carbohydrate-mediated interactions. The selective release of target proteins from solid support is a key step in functional proteomics. We envisaged that light activation can be exploited for releasing labeled protein in a dual photo-affinity probe-based strategy. To investigate this possibility, we designed a trifunctional, galactose-based, multivalent glycoprobe for affinity labeling of carbohydrate-binding proteins. The resulting covalent protein-probe adduct is attached to a photo-cleavable biotin affinity tag; the biotin moiety enables specific presentation of the conjugate on streptavidin-coated beads, and the photolabile linker allows the release of the labeled proteins. This dual probe promotes both the labeling and the facile cleavage of the target protein complexes from the solid surfaces and the remainder of the cell lysate in a completely unaltered form, thus eliminating many of the common pitfalls associated with traditional affinity-based purification methods. Copyright © 2016 Elsevier Ltd. All rights reserved.

A Surface Science Paradigm for a Post-Huygens Titan Mission

NASA Technical Reports Server (NTRS)

Zimmerman, Wayne; Lunine, Jonathan; Lorenz, Ralph

2004-01-01

With the Cassini-Huygens atmospheric probe drop-off mission fast approaching, it is essential that scientists and engineers start scoping potential follow-on surface science missions. This paper provides a summary of the first year of a two year design study which examines in detail the desired surface science measurements and resolution, potential instrument suite, and complete payload delivery system. Also provided are design concepts for both an aerial inflatable mobility platform and deployable instrument sonde. The tethered deployable sonde provides the capability to sample nearsurface atmosphere, sub-surface liquid (if it exists), and surface solid material. Actual laboratory tests of the amphibious sonde prototype are also presented.

Solid-phase microextraction/gas chromatography-mass spectrometry method optimization for characterization of surface adsorption forces of nanoparticles.

PubMed

Omanovic-Miklicanin, Enisa; Valzacchi, Sandro; Simoneau, Catherine; Gilliland, Douglas; Rossi, Francois

2014-10-01

A complete characterization of the different physico-chemical properties of nanoparticles (NPs) is necessary for the evaluation of their impact on health and environment. Among these properties, the surface characterization of the nanomaterial is the least developed and in many cases limited to the measurement of surface composition and zetapotential. The biological surface adsorption index approach (BSAI) for characterization of surface adsorption properties of NPs has recently been introduced (Xia et al. Nat Nanotechnol 5:671-675, 2010; Xia et al. ACS Nano 5(11):9074-9081, 2011). The BSAI approach offers in principle the possibility to characterize the different interaction forces exerted between a NP's surface and an organic--and by extension biological--entity. The present work further develops the BSAI approach and optimizes a solid-phase microextraction gas chromatography-mass spectrometry (SPME/GC-MS) method which, as an outcome, gives a better-defined quantification of the adsorption properties on NPs. We investigated the various aspects of the SPME/GC-MS method, including kinetics of adsorption of probe compounds on SPME fiber, kinetic of adsorption of probe compounds on NP's surface, and optimization of NP's concentration. The optimized conditions were then tested on 33 probe compounds and on Au NPs (15 nm) and SiO2 NPs (50 nm). The procedure allowed the identification of three compounds adsorbed by silica NPs and nine compounds by Au NPs, with equilibrium times which varied between 30 min and 12 h. Adsorption coefficients of 4.66 ± 0.23 and 4.44 ± 0.26 were calculated for 1-methylnaphtalene and biphenyl, compared to literature values of 4.89 and 5.18, respectively. The results demonstrated that the detailed optimization of the SPME/GC-MS method under various conditions is a critical factor and a prerequisite to the application of the BSAI approach as a tool to characterize surface adsorption properties of NPs and therefore to draw any further conclusions on their potential impact on health.

Formation of relief on Europa's surface and analysis of a melting probe movement through the ice

NASA Astrophysics Data System (ADS)

Erokhina, O. S.; Chumachenko, E. N.; Dunham, D. W.; Aksenov, S. A.; Logashina, I. V.

2013-12-01

These days, studies of planetary bodies' are of great interest. And of special interest are the icy moons of the giant planets like Jupiter and Saturn. Analysis of 'Voyager 1', 'Voyager 2', 'Galileo' and 'Cassini' spacecraft data showed that icy covers were observed on Jupiter's moons Ganymede, Europa and Calisto, and Saturn's moons Titan and Enceladus. Of particular interest is the relatively smooth surface of Europa. The entire surface is covered by a system of bands, valleys, and ridges. These structures are explained by the mobility of surface ice, and the impact of stress and large-scale tectonic processes. Also conditions on these moons allow speculation about possible life, considering these moons from an astrobiological point of view. To study the planetary icy body in future space missions, one of the problems to solve is the problem of design of a special device capable of penetrating through the ice, as well as the choice of the landing site of this probe. To select a possible landing site, analysis of Europa's surface relief formation is studied. This analysis showed that compression, extention, shearing, and bending can influence some arbitrarily separated section of Europe's icy surface. The computer simulation with the finite element method (FEM) was performed to see what types of defects could arise from such effects. The analysis showed that fractures and cracks could have various forms depending on the stress-strained state arising in their vicinity. Also the problem of a melting probe's movement through the ice is considered: How the probe will move in low gravity and low atmospheric pressure; whether the hole formed in the ice will be closed when the probe penetrates far enough or not; what is the influence of the probe's characteristics on the melting process; what would be the order of magnitude of the penetration velocity. This study explores the technique based on elasto-plastic theory and so-called 'solid water' theory to estimate the melting velocity and to study the melting process. Based on this technique, several cases of melting probe motion are considered, the velocity of the melting probe is estimated, the influence of different factors are studied and discussed, and an easy way to optimize the parameters of the probe is proposed.

Probing the Surface of Platinum during the Hydrogen Evolution Reaction in Alkaline Electrolyte

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

Stoerzinger, Kelsey A.; Favaro, Marco; Ross, Philip N.

Understanding the surface chemistry of electrocatalysts in operando can bring insight into the reaction mechanism, and ultimately the design of more efficient materials for sustainable energy storage and conversion. Recent progress in synchrotron based X-ray spectroscopies for in operando characterization allows us to probe the solid/liquid interface directly while applying an external potential, applied here to the model system of Pt in alkaline electrolyte for the hydrogen evolution reaction (HER). We employ ambient pressure X-ray photoelectron spectroscopy (AP-XPS) to identify the oxidation and reduction of Pt-oxides and hydroxides on the surface as a function of applied potential, and further assessmore » the potential for hydrogen adsorption and absorption (hydride formation) during and after the HER. This new window into the surface chemistry of Pt in alkaline brings insight into the nature of the rate limiting step, the extent of H ad/absorption and it’s persistence at more anodic potentials.« less

Hydrodynamic capture of microswimmers into sphere-bound orbits.

PubMed

Takagi, Daisuke; Palacci, Jérémie; Braunschweig, Adam B; Shelley, Michael J; Zhang, Jun

2014-03-21

Self-propelled particles can exhibit surprising non-equilibrium behaviors, and how they interact with obstacles or boundaries remains an important open problem. Here we show that chemically propelled micro-rods can be captured, with little change in their speed, into close orbits around solid spheres resting on or near a horizontal plane. We show that this interaction between sphere and particle is short-range, occurring even for spheres smaller than the particle length, and for a variety of sphere materials. We consider a simple model, based on lubrication theory, of a force- and torque-free swimmer driven by a surface slip (the phoretic propulsion mechanism) and moving near a solid surface. The model demonstrates capture, or movement towards the surface, and yields speeds independent of distance. This study reveals the crucial aspects of activity–driven interactions of self-propelled particles with passive objects, and brings into question the use of colloidal tracers as probes of active matter.

Axisymmetric Lattice Boltzmann Model of Droplet Impact on Solid Surfaces

NASA Astrophysics Data System (ADS)

Dalgamoni, Hussein; Yong, Xin

2017-11-01

Droplet impact is a ubiquitous fluid phenomena encountered in scientific and engineering applications such as ink-jet printing, coating, electronics manufacturing, and many others. It is of great technological importance to understand the detailed dynamics of drop impact on various surfaces. The lattice Boltzmann method (LBM) emerges as an efficient method for modeling complex fluid systems involving rapidly evolving fluid-fluid and fluid-solid interfaces with complex geometries. In this work, we model droplet impact on flat solid substrates with well-defined wetting behavior using a two-phase axisymmetric LBM with high density and viscosity contrasts. We extend the two-dimensional Lee and Liu model to capture axisymmetric effect in the normal impact. First we compare the 2D axisymmetric results with the 2D and 3D results reported by Lee and Liu to probe the effect of axisymmetric terms. Then, we explore the effects of Weber number, Ohnesorge number, and droplet-surface equilibrium contact angle on the impact. The dynamic contact angle and spreading factor of the droplet during impact are investigated to qualitatively characterize the impact dynamics.

Imbedded Thermocouples as a Solid Propellant Combustion Probe

DTIC Science & Technology

1985-04-01

IMBEDDED THERMOCOUPLES AS A SOLID PROPELLANT COMBUSTION PROBE Martin S. Miller Terence P. Coffee Anthony J. Kotlar April 1985 APPROVEO FOR PUBUC...COMPLETING FORM RECIPIENT’S CATALOG NUMBER 4. TITLE (and Subtitle) IMBEDDED THERMOCOUPLES AS A SOLID PROPELLANT COMBUSTION PROBE 7. AuTHORf...this report were presented at the 1984 JANNAF Combustion Meeting 19 KEY WOROS (Continue on reveree aide tl neceeemry end Identity by block number

Carbon fiber brush electrode as a novel substrate for atmospheric solids analysis probe (ASAP) mass spectrometry: Electrochemical oxidation of brominated phenols.

PubMed

Skopalová, Jana; Barták, Petr; Bednář, Petr; Tomková, Hana; Ingr, Tomáš; Lorencová, Iveta; Kučerová, Pavla; Papoušek, Roman; Borovcová, Lucie; Lemr, Karel

2018-01-25

A carbon fiber brush electrode (CFBE) was newly designed and used as a substrate for both controlled potential electrolysis and atmospheric solids analysis probe (ASAP) mass spectrometry. Electropolymerized and strongly adsorbed products of electrolysis were directly desorbed and ionized from the electrode surface. Electrochemical properties of the electrode investigated by cyclic voltammetry revealed large electroactive surface area (23 ± 3 cm 2 ) at 1.3 cm long array of carbon fibers with diameter 6-9 μm. Some products of electrochemical oxidation of pentabromophenol and 2,4,6-tribromophenol formed a compact layer on the carbon fibers and were analyzed using ASAP. Eleven new oligomeric products were identified including quinones and biphenoquinones. These compounds were not observed previously in electrolyzed solutions by liquid or gas chromatography/mass spectrometry. The thickness around 58 nm and 45 nm of the oxidation products layers deposited on carbon fibers during electrolysis of pentabromophenol and 2,4,6-tribromophenol, respectively, was estimated from atomic force microscopy analysis and confirmed by scanning electron microscopy with energy-dispersive X-ray spectroscopy measurements. Copyright © 2017 Elsevier B.V. All rights reserved.

The coupled effects of environmental composition, temperature and contact size-scale on the tribology of molybdenum disulfide

NASA Astrophysics Data System (ADS)

Khare, Harmandeep S.

Liquid lubricants are precluded in an exceedingly large number of consumer as well as extreme applications as a means to reduce friction and wear at the sliding interface of two bodies. The extraterrestrial environment is one such example of an extreme environment which has motivated the development of advanced solid lubricant materials. Mechanical systems for space require fabrication, assembly, transportation and testing on earth before launch and deployment. Solid lubricants for space are expected to not only operate efficiently in the hard vacuum of space but also withstand interactions with moisture or oxygen during the terrestrial storage, transportation and assembly prior to deployment and launch. Molybdenum disulfide (MoS2) is considered the gold standard in solid lubricants for space due to its excellent tribological properties in ultra-high vacuum. However in the presence of environmental species such as water and oxygen or at elevated temperatures, the lubricity and endurance of MoS2 is severely limited. Past studies have offered several hypotheses for the breakdown of lubrication of MoS2 under the influence of water and oxygen, although exact mechanisms remain unknown. Furthermore, it is unclear if temperature acts as a driver solely for oxidation or for thermally activated slip and thermally activated desorption as well. The answers to these questions are of fundamental importance to improving the reliability of existing MoS2-based solid lubricants for space, as well as for guiding the design of advanced lamellar solid lubricant coatings. This dissertation aims to elucidate: (1) the role of water on MoS2 oxidation, (2) the role of water on MoS2 friction, (3) the role of oxygen on MoS2 friction, (4) the contribution of thermal activation to ambient-temperature friction, and (5) effects of length-scale. The results of this study showed that water does not cause oxidation of MoS2. Water increases ambient-temperature friction of MoS2 directly through a combination of both surface adsorption and diffusion into the coating subsurface. Thermally activated desiccation effectively dries the bulk of the coating, yielding low values of friction coefficient even at ambient humidity and temperature. Friction of MoS2 decreases with increasing temperature between 25°C and 100°C in the presence of environmental water and increases in the presence of oxygen alone. At temperatures greater than 100°C, friction generally increases with temperature only in the presence of environmental oxygen; at these elevated temperatures, friction decreases with increasing humidity. The transition from room-temperature increase to elevated-temperature decrease in friction with increasing humidity is found to be a strong function of the contact history as well as coating microstructure. Lastly, the contribution of nanoscale tribofilms to macroscale friction was studied through nanotribometry. Friction measured on the worn MoS2 coating with a nano-scale AFM probe showed direct and quantifiable evidence of sliding-induced surface modification of MoS2; friction measured on the perfectly ordered single crystal MoS2 was nearly an order of magnitude lower than friction on worn MoS2. Although friction coefficients measured with a nanoscale probe showed high surface sensitivity, micron-sized AFM probes gave friction coefficients similar to those obtained in the macroscale, suggesting the formation of surface films in-situ during sliding with the colloidal probe. A reduction in friction is observed after annealing for both the nanoscale and microscale probes, suggesting a strong overriding effect of the desiccated bulk over surface adsorption in driving the friction response at these length-scales.

Optical detection of ultrasound using an apertureless near-field scanning optical microscopy system

NASA Astrophysics Data System (ADS)

Ahn, Phillip; Zhang, Zhen; Sun, Cheng; Balogun, Oluwaseyi

2013-01-01

Laser ultrasonics techniques are power approaches for non-contact generation and detection of high frequency ultrasound on a local scale. In these techniques, optical diffraction limits the spatial information that can be accessed from a measurement. In order to improve the lateral spatial resolution, we incorporate an apertureless near-field scanning optical microscope (aNSOM) into laser ultrasonics setup for local detection of laser generated ultrasound. The aNSOM technique relies on the measurement of a weak backscattered near-field light intensity resulting from the oblique illumination of a nanoscale probe-tip positioned close to a sample surface. We enhance the optical near-field intensity by coupling light to surface plasmon polaritons (SPPs) on the shaft of an atomic force microscopy (AFM) cantilever. The SPPs propagate down the AFM shaft, localize at the tip apex, and are backscattered to the far-field when the separation distance between the probe tip and the sample surface is comparable to the probe-tip radius. The backscattered near-field intensity is dynamically modulated when an ultrasonic wave arrives at the sample surface leading to a transient change in the tip-sample separation distance. We present experimental results detailing measurement of broadband and narrowband laser generated ultrasound in solids with frequencies reaching up to 180 MHz range.

On the possibility of controlling the hydrophilic/hydrophobic characteristics of toroid Mo138 nanocluster polyoxometalates

NASA Astrophysics Data System (ADS)

Grzhegorzhevskii, K. V.; Adamova, L. V.; Eremina, E. V.; Ostroushko, A. A.

2017-03-01

The possibility of changing the hydrophilic (polar) surfaces of toroid nanocluster polyoxomolibdates to hydrophobic (nonpolar) surfaces via the modification of Mo138 nanoclusters by surfactant molecules (dodecylpyridinium chloride) as a result of the interaction between these compounds in solutions is demonstrated. Benzene and methanol are used as molecular probes (indicators of the condition of nanocluster surfaces). Comparative characteristics of the equilibrium sorption of benzene and methanol vapors on the initial and modified surfaces of the solid polyoxometalate, and data on the sorption of organic molecules on the surfaces of Rhodamine B-modified nanoclusters of the toroid (Mo138) and keplerate (Mo132) types are obtained.

A hot tip: imaging phenomena using in situ multi-stimulus probes at high temperatures

NASA Astrophysics Data System (ADS)

Nonnenmann, Stephen S.

2016-02-01

Accurate high temperature characterization of materials remains a critical challenge to the continued advancement of various important energy, nuclear, electronic, and aerospace applications. Future experimental studies must assist these communities to progress past empiricism and derive deliberate, predictable designs of material classes functioning within active, extreme environments. Successful realization of systems ranging from fuel cells and batteries to electromechanical nanogenerators and turbines requires a dynamic understanding of the excitation, surface-mediated, and charge transfer phenomena which occur at heterophase interfaces (i.e. vapor-solid, liquid-solid, solid-solid) and impact overall performance. Advancing these frontiers therefore necessitates in situ (operando) characterization methods capable of resolving, both spatially and functionally, the coherence between these complex, collective excitations, and their respective response dynamics, through studies within the operating regime. This review highlights recent developments in scanning probe microscopy in performing in situ imaging at high elevated temperatures. The influence of and evolution from vacuum-based electron and tunneling microscopy are briefly summarized and discussed. The scope includes the use of high temperature imaging to directly observe critical phase transition, electronic, and electrochemical behavior under dynamic temperature settings, thus providing key physical parameters. Finally, both challenges and directions in combined instrumentation are proposed and discussed towards the end.

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

Prabhakaran, Venkateshkumar; Johnson, Grant E.; Wang, Bingbing

Molecular-level understanding of electrochemical processes occurring at electrode-electrolyte interfaces (EEI) is key to the rational development of high-performance and sustainable electrochemical technologies. This article reports the development and first application of solid-state in situ electrochemical probes to study redox and catalytic processes occurring at well-defined EEI generated using soft-landing of mass- and charge-selected cluster ions (SL). In situ electrochemical probes with excellent mass transfer properties are fabricated using carefully-designed nanoporous ionic liquid membranes. SL enables deposition of pure active species that are not obtainable with other techniques onto electrode surfaces with precise control over charge state, composition, and kinetic energy.more » SL is, therefore, a unique tool for studying fundamental processes occurring at EEI. For the first time using an aprotic electrochemical probe, the effect of charge state (PMo12O403-/2-) and the contribution of building blocks of Keggin polyoxometalate (POM) clusters to redox processes are characterized by populating EEI with novel POM anions generated by electrospray ionization and gas phase dissociation. Additionally, a proton conducting electrochemical probe has been developed to characterize the reactive electrochemistry (oxygen reduction activity) of bare Pt clusters (Pt40 ~1 nm diameter), thus demonstrating the capability of the probe for studying reactions in controlled gaseous environments. The newly developed in situ electrochemical probes combined with ion SL provide a versatile method to characterize the EEI in solid-state redox systems and reactive electrochemistry at precisely-defined conditions. This capability will advance molecular-level understanding of processes occurring at EEI that are critical to many energy-related technologies.« less

Site-specific orientation of an α-helical peptide ovispirin-1 from isotope-labeled SFG spectroscopy.

PubMed

Ding, Bei; Laaser, Jennifer E; Liu, Yuwei; Wang, Pengrui; Zanni, Martin T; Chen, Zhan

2013-11-27

Sum-frequency generation (SFG) vibrational spectroscopy is often used to probe the backbone structures and orientations of polypeptides at surfaces. Using the ovispirin-1 polypeptide at the solid/liquid interface of polystyrene, we demonstrate for the first time that SFG can probe the polarization response of a single-isotope-labeled residue. To interpret the spectral intensities, we simulated the spectra using an excitonic Hamiltonian approach. We show that the polarization dependence of either the label or the unlabeled amide I band alone does not provide sufficient structural constraints to obtain both the tilt and the twist of the ovispirin helix at a solid/liquid interface, but that both can be determined from the polarization dependence of the complete spectrum. For ovispirin, the detailed analysis of the polarized SFG experimental data shows that the helix axis is tilted at roughly 138° from the surface normal, and the transition dipole of the isotope-labeled C═O group is tilted at 23° from the surface normal, with the hydrophobic region facing the polystyrene surface. We further demonstrate that the Hamiltonian approach is able to address the coupling effect and the structural disorder. For comparison, we also collected the FTIR spectrum of ovispirin under similar conditions, which reveals the enhanced sensitivity of SFG for structural studies of single monolayer peptide surfaces. Our study provides insight into how structural and environmental effects appear in SFG spectra of the amide I band and establishes that SFG of isotope-labeled peptides will be a powerful technique for elucidating secondary structures with residue-by-residue resolution.

Site-specific Orientation of an α-helical Peptide Ovispirin-1 from Isotope Labeled SFG Spectroscopy

PubMed Central

Ding, Bei; Laaser, Jennifer E.; Liu, Yuwei; Wang, Pengrui; Zanni, Martin T.; Chen, Zhan

2013-01-01

Sum-frequency generation (SFG) vibrational spectroscopy is often used to probe the backbone structures and orientations of polypeptides at surfaces. Using the ovispirin-1 polypeptide at the solid/liquid interface of polystyrene, we demonstrate for the first time that SFG can probe the polarization response of a single isotope labeled residue. To interpret the spectral intensities, we simulated the spectra using an excitonic Hamiltonian approach. We show that the polarization dependence of either the label or the unlabeled amide I band alone does not provide sufficient structural constraints to obtain both the tilt and the twist of the ovispirin helix at a solid/liquid interface, but that both can be determined from the polarization dependence of the complete spectrum. For ovispirin, the detailed analysis of the polarized SFG experimental data shows that the helix axis is tilted at roughly 138 degrees from the surface normal, and the transition dipole of the isotope labeled C=O group is tilted at 23 degrees from the surface normal, with the hydrophobic region facing the polystyrene surface. We further demonstrated that the Hamiltonian approach is able to address the coupling effect and the structural disorder. For comparison, we also collected the FTIR spectrum of ovispirin under similar conditions, which reveals the enhanced sensitivity of SFG for structural studies of single monolayer peptide surfaces. Our study provides insight into how structural and environmental effects appear in SFG spectra of the amide I band and establishes that SFG of isotope labeled peptides will be a powerful technique for elucidating secondary structures with residue-by-residue resolution. PMID:24228619

Chemical Weathering on Venus

NASA Astrophysics Data System (ADS)

Zolotov, Mikhail

2018-01-01

Chemical and phase compositions of Venus's surface could reflect history of gas- and fluid-rock interactions, recent and past climate changes, and a loss of water from the Earth's sister planet. The concept of chemical weathering on Venus through gas-solid type reactions has been established in 1960s after the discovery of hot and dense CO2-rich atmosphere inferred from Earth-based and Mariner 2 radio emission data. Initial works suggested carbonation, hydration, and oxidation of exposed igneous rocks and a control (buffering) of atmospheric gases by solid-gas type chemical equilibria in the near-surface lithosphere. Calcite, quartz, wollastonite, amphiboles, and Fe oxides were considered likely secondary minerals. Since the late 1970s, measurements of trace gases in the sub-cloud atmosphere by Pioneer Venus and Venera entry probes and Earth-based infrared spectroscopy doubted the likelihood of hydration and carbonation. The H2O gas content appeared to be low to allow a stable existence of hydrated and a majority of OH-bearing minerals. The concentration of SO2 was too high to allow the stability of calcite and Ca-rich silicates with respect to sulfatization to CaSO4. In 1980s, the supposed ongoing consumption of atmospheric SO2 to sulfates gained support by the detection of an elevated bulk S content at Venera and Vega landing sites. The induced composition of the near-surface atmosphere implied oxidation of ferrous minerals to magnetite and hematite, consistent with the infrared reflectance of surface materials. The likelihood of sulfatization and oxidation has been illustrated in modeling experiments at simulated Venus conditions. Venus's surface morphology suggests that hot surface rocks and fines of mainly mafic composition contacted atmospheric gases during several hundreds of millions years since a global volcanic resurfacing. Some exposed materials could have reacted at higher and lower temperatures in a presence of diverse gases at different altitudinal, volcanic, impact, and atmospheric settings. On highly deformed tessera terrains, more ancient rocks of unknown composition could reflect interactions with putative water-rich atmospheres and even aqueous solutions. Salt-, Fe oxide, or silica-rich formations would indicate past aqueous processes. The apparent diversity of affected solids, surface temperatures, pressures, and gas/fluid compositions throughout Venus's history implies multiple signs of chemical alteration, which remain to be investigated. The current understanding of chemical weathering is limited by the uncertain composition of the deep atmosphere, by the lack of direct data on the phase composition of surface materials, and by the uncertain data on thermodynamics of minerals and their solid solutions. In the preparation for further entry probe and lander missions, rock alteration needs to be investigated through chemical kinetic experiments and calculations of solid-gas(fluid) equilibria to constrain past and present processes.

Towards attosecond measurement in molecules and at surfaces

NASA Astrophysics Data System (ADS)

Marangos, Jonathan

2015-05-01

1) We will present a number of experimental approaches that are being developed at Imperial College to make attosecond timescale measurements of electronic dynamics in suddenly photoionized molecules and at surfaces. A brief overview will be given of some of the unanswered questions in ultrafast electron and hole dynamics in molecules and solids. These questions include the existence of electronic charge migration in molecules and how this process might couple to nuclear motion even on the few femtosecond timescale. How the timescale of photoemission from a surface may differ from that of an isolated atom, e.g. due to electron transport phenomena associated with the distance from the surface of the emitting atom and the electron dispersion relation, is also an open question. 2) The measurement techniques we are currently developing to answer these questions are HHG spectroscopy, attosecond pump-probe photoelectron/photoion studies, and attosecond pump-probe transient absorption as well as attosecond streaking for measuring surface emission. We will present recent advances in generating two synchronized isolated attosecond pulses at different colours for pump-probe measurements (at 20 eV and 90 eV respectively). Results on generation of isolated attosecond pulses at 300 eV and higher photon energy using a few-cycle 1800 nm OPG source will be presented. The use of these resources for making pump-probe measurements will be discussed. Finally we will present the results of streaking measurement of photoemission wavepackets from two types of surface (WO3 and a evaporated Au film) that show a temporal broadening of ~ 100 as compared to atomic streaks that is consistent with the electron mean free path in these materials. Work supported by ERC and EPSRC.

Femtosecond nonlinear ultrasonics in gold probed with ultrashort surface plasmons.

PubMed

Temnov, Vasily V; Klieber, Christoph; Nelson, Keith A; Thomay, Tim; Knittel, Vanessa; Leitenstorfer, Alfred; Makarov, Denys; Albrecht, Manfred; Bratschitsch, Rudolf

2013-01-01

Fundamental interactions induced by lattice vibrations on ultrafast time scales have become increasingly important for modern nanoscience and technology. Experimental access to the physical properties of acoustic phonons in the terahertz-frequency range and over the entire Brillouin zone is crucial for understanding electric and thermal transport in solids and their compounds. Here we report on the generation and nonlinear propagation of giant (1 per cent) acoustic strain pulses in hybrid gold/cobalt bilayer structures probed with ultrafast surface plasmon interferometry. This new technique allows for unambiguous characterization of arbitrary ultrafast acoustic transients. The giant acoustic pulses experience substantial nonlinear reshaping after a propagation distance of only 100 nm in a crystalline gold layer. Excellent agreement with the Korteveg-de Vries model points to future quantitative nonlinear femtosecond terahertz-ultrasonics at the nano-scale in metals at room temperature.

Guiding, bending, and splitting of coupled defect surface modes in a surface-wave photonic crystal

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

Gao, Zhen; Gao, Fei; Zhang, Baile, E-mail: blzhang@ntu.edu.sg

2016-01-25

We experimentally demonstrate a type of waveguiding mechanism for coupled surface-wave defect modes in a surface-wave photonic crystal. Unlike conventional spoof surface plasmon waveguides, waveguiding of coupled surface-wave defect modes is achieved through weak coupling between tightly localized defect cavities in an otherwise gapped surface-wave photonic crystal, as a classical wave analogue of tight-binding electronic wavefunctions in solid state lattices. Wave patterns associated with the high transmission of coupled defect surface modes are directly mapped with a near-field microwave scanning probe for various structures including a straight waveguide, a sharp corner, and a T-shaped splitter. These results may find usemore » in the design of integrated surface-wave devices with suppressed crosstalk.« less

An efficient solid-state synthesis of fluorescent surface carboxylated carbon dots derived from C60 as a label-free probe for iron ions in living cells.

PubMed

Lan, Jing; Liu, Chunfang; Gao, Mingxuan; Huang, Chengzhi

2015-11-01

In order to achieve the simple, easily repeated, and large scale preparation of fluorescent CDs, a new solid-state synthesis (SSS) approach was developed by calcining the mixture of fullerenes (C60) and solid sodium hydroxide. The cage of fullerenes could be opened and the hydroxyl and carboxyl were successfully introduced in the presence of sodium hydroxide under high temperature. The as-prepared surface carboxylated CDs possess many good properties, such as high water solubility, good photostability, salt tolerance, and nontoxicity. Especially, the fluorescence of CDs could be highly quenched by Fe(3+) because of the strong interaction of hydroxyl or carboxyl on the as-obtained CDs with Fe(3+), which realized a sensitive detection of Fe(3+) in the linear range of 0.02-0.6 μmol/L. What is more, we further applied the obtained CDs into the intracellular imaging of Fe(3+). Copyright © 2015 Elsevier B.V. All rights reserved.

The prediction of the gas environment of the PHILAE probe during its 2014 descent to the nucleus of the comet 67P

NASA Astrophysics Data System (ADS)

Crifo, J.-F.; Zakharov, V. V.; Rodionov, A. V.; Lukyanov, G. A.

2016-11-01

One of the objectives of the ESA "ROSETTA" mission to the comet 67P was to insert, in August 2014, an orbiter probe around the so-called nucleus of the comet, and to deposit the "PHILAE" lander at the surface of the nucleus in November 2014. The selection of the landing site and the definition of the release point and initial descent velocity vector were made in the period August to October 2014 on the basis of simulations of the descent trajectory. This requested an assessment of the gravitational and aerodynamic forces on PHILAE. We here describe the so-called RZC model developed to predict the gas environment of 67P in November 2014 and compute the aerodynamic force. We first outline the unusual diffculties resulting from (1) the complexity of the nucleus surface on all scales, (2) the absence of direct measurements of the gas flux at the surface itself, (3) the time-dependence of the gas production induced by the fast nucleus rotation, (4) the need to perform the whole program within less than three months. Then we outline the physical approach adopted to overcome these diffculties, and describe the RZC model which included three differing tools: (1) a set of gasdynamic/gaskinetic codes to compute the vacuum outflow of a rarefied gas mixture from a highly aspherical rotating solid source; (2) an heuristic approach to deal with the solid/gas initial boundary conditions, and (3) an iterative procedure to derive the gas production parameters on the nucleus surface from the observational data acquired from the orbiter probe. The satisfactory operation of the RZC code in the weeks preceding the November 2014 PHILAE descent is shown, and the forecasted aerodynamic force during the PHILAE descent is compared to the gravitational force.

Integration of Quartz Crystal Microbalance-Dissipation and Reflection-Mode Localized Surface Plasmon Resonance Sensors for Biomacromolecular Interaction Analysis.

PubMed

Ferhan, Abdul Rahim; Jackman, Joshua A; Cho, Nam-Joon

2016-12-20

The combination of label-free, surface-sensitive measurement techniques based on different physical principles enables detailed characterization of biomacromolecular interactions at solid-liquid interfaces. To date, most combined measurement systems have involved experimental techniques with similar probing volumes, whereas the potential of utilizing techniques with different surface sensitivities remains largely unexplored, especially for data interpretation. Herein, we report a combined measurement approach that integrates a conventional quartz crystal microbalance-dissipation (QCM-D) setup with a reflection-mode localized surface plasmon (LSPR) sensor. Using this platform, we investigate vesicle adsorption on a titanium oxide-coated sensing substrate along with the amphipathic, α-helical (AH) peptide-induced structural transformation of surface-adsorbed lipid vesicles into a supported lipid bilayer (SLB) as a model biomacromolecular interaction. While the QCM-D and LSPR signals both detected mass uptake arising from vesicle adsorption, tracking the AH peptide-induced structural transformation revealed more complex measurement responses based on the different surface sensitivities of the two techniques. In particular, the LSPR signal recorded an increase in optical mass near the sensor surface which indicated SLB formation, whereas the QCM-D signals detected a significant loss in net acoustic mass due to excess lipid and coupled solvent leaving the probing volume. Importantly, these measurement capabilities allowed us to temporally distinguish the process of SLB formation at the sensor surface from the overall structural transformation process. Looking forward, these label-free measurement capabilities to simultaneously probe adsorbates at multiple length scales will provide new insights into complex biomacromolecular interactions.

Inclusion of Ti and Zr species on clay surfaces and their effect on the interaction with organic molecules

NASA Astrophysics Data System (ADS)

Rangel-Rivera, Pedro; Bachiller-Baeza, María Belén; Galindo-Esquivel, Ignacio; Rangel-Porras, Gustavo

2018-07-01

The interactions between the clay surface and the organic molecules play an important role in the efficient of these materials in adsorption and catalytic processes. These materials are often modified with the inclusion of other catalytic particles for the purpose of enhancing the activity. In this study, commercial clay K10 was modified with the particles inclusion of titanium and zirconium. The solid surfaces were examined by infrared spectroscopy, scanning electron microscopy (SEM) coupled to an energy-dispersive X-ray spectroscopy device (EDS), and X-ray photoelectron spectroscopy (XPS). Temperature programmed desorption of ammonia (TPD-NH3) and propan-2-ol decomposition test reaction were performed to probe the acid properties. The adsorption of acetic acid, ethanol, and propan-2-ol on the surface of each solid and their thermal stability were studied by diffuse reflectance infrared Fourier transform spectroscopy (DRIFT). Finally, these materials were used in the esterification of acetic acid with penta-1-ol. The real effect over the incorporation of titanium species and zirconium species on clay surface for interacting with the organic molecules was discussed.

A review of the different techniques for solid surface acid-base characterization.

PubMed

Sun, Chenhang; Berg, John C

2003-09-18

In this work, various techniques for solid surface acid-base (AB) characterization are reviewed. Different techniques employ different scales to rank acid-base properties. Based on the results from literature and the authors' own investigations for mineral oxides, these scales are compared. The comparison shows that Isoelectric Point (IEP), the most commonly used AB scale, is not a description of the absolute basicity or acidity of a surface, but a description of their relative strength. That is, a high IEP surface shows more basic functionality comparing with its acidic functionality, whereas a low IEP surface shows less basic functionality comparing with its acidic functionality. The choice of technique and scale for AB characterization depends on the specific application. For the cases in which the overall AB property is of interest, IEP (by electrokinetic titration) and H(0,max) (by indicator dye adsorption) are appropriate. For the cases in which the absolute AB property is of interest such as in the study of adhesion, it is more pertinent to use chemical shift (by XPS) and the heat of adsorption of probe gases (by calorimetry or IGC).

Intense Plasma Waveguide Terahertz Sources for High-Field THz Probe Science with Ultrafast Lasers for Solid State Physics

DTIC Science & Technology

2016-08-25

AFRL-AFOSR-UK-TR-2016-0029 Intense Plasma-Waveguide Terahertz Sources for High-Field THz probe science with ultrafast lasers for Solid State Physics...Plasma-Waveguide Terahertz Sources for High-Field THz probe science with ultrafast lasers for Solid State Physics, 5a.  CONTRACT NUMBER 5b.  GRANT...an existing high energy laser system, has been applied to the study of intense terahertz radiation generated in gaseous plasmas in purpose

Driving CO2 to a Quasi-Condensed Phase at the Interface between a Nanoparticle Surface and a Metal-Organic Framework at 1 bar and 298 K.

PubMed

Lee, Hiang Kwee; Lee, Yih Hong; Morabito, Joseph V; Liu, Yejing; Koh, Charlynn Sher Lin; Phang, In Yee; Pedireddy, Srikanth; Han, Xuemei; Chou, Lien-Yang; Tsung, Chia-Kuang; Ling, Xing Yi

2017-08-23

We demonstrate a molecular-level observation of driving CO 2 molecules into a quasi-condensed phase on the solid surface of metal nanoparticles (NP) under ambient conditions of 1 bar and 298 K. This is achieved via a CO 2 accumulation in the interface between a metal-organic framework (MOF) and a metal NP surface formed by coating NPs with a MOF. Using real-time surface-enhanced Raman scattering spectroscopy, a >18-fold enhancement of surface coverage of CO 2 is observed at the interface. The high surface concentration leads CO 2 molecules to be in close proximity with the probe molecules on the metal surface (4-methylbenzenethiol), and transforms CO 2 molecules into a bent conformation without the formation of chemical bonds. Such linear-to-bent transition of CO 2 is unprecedented at ambient conditions in the absence of chemical bond formation, and is commonly observed only in pressurized systems (>10 5 bar). The molecular-level observation of a quasi-condensed phase induced by MOF coating could impact the future design of hybrid materials in diverse applications, including catalytic CO 2 conversion and ambient solid-gas operation.

Gas sampling system for reactive gas-solid mixtures

DOEpatents

Daum, Edward D.; Downs, William; Jankura, Bryan J.; McCoury, Jr., John M.

1989-01-01

An apparatus and method for sampling a gas containing a reactive particulate solid phase flowing through a duct and for communicating a representative sample to a gas analyzer. A sample probe sheath 32 with an angular opening 34 extends vertically into a sample gas duct 30. The angular opening 34 is opposite the gas flow. A gas sampling probe 36 concentrically located within sheath 32 along with calibration probe 40 partly extend in the sheath 32. Calibration probe 40 extends further in the sheath 32 than gas sampling probe 36 for purging the probe sheath area with a calibration gas during calibration.

Gas sampling system for reactive gas-solid mixtures

DOEpatents

Daum, Edward D.; Downs, William; Jankura, Bryan J.; McCoury, Jr., John M.

1990-01-01

An apparatus and method for sampling gas containing a reactive particulate solid phase flowing through a duct and for communicating a representative sample to a gas analyzer. A sample probe sheath 32 with an angular opening 34 extends vertically into a sample gas duct 30. The angular opening 34 is opposite the gas flow. A gas sampling probe 36 concentrically located within sheath 32 along with calibration probe 40 partly extends in the sheath 32. Calibration probe 40 extends further in the sheath 32 than gas sampling probe 36 for purging the probe sheath area with a calibration gas during calibration.

Nucleic Acid Detection Methods

DOEpatents

Smith, Cassandra L.; Yaar, Ron; Szafranski, Przemyslaw; Cantor, Charles R.

1998-05-19

The invention relates to methods for rapidly determining the sequence and/or length a target sequence. The target sequence may be a series of known or unknown repeat sequences which are hybridized to an array of probes. The hybridized array is digested with a single-strand nuclease and free 3'-hydroxyl groups extended with a nucleic acid polymerase. Nuclease cleaved heteroduplexes can be easily distinguish from nuclease uncleaved heteroduplexes by differential labeling. Probes and target can be differentially labeled with detectable labels. Matched target can be detected by cleaving resulting loops from the hybridized target and creating free 3-hydroxyl groups. These groups are recognized and extended by polymerases added into the reaction system which also adds or releases one label into solution. Analysis of the resulting products using either solid phase or solution. These methods can be used to detect characteristic nucleic acid sequences, to determine target sequence and to screen for genetic defects and disorders. Assays can be conducted on solid surfaces allowing for multiple reactions to be conducted in parallel and, if desired, automated.

Removal forces and adhesion properties of Saccharomyces cerevisiae on glass substrates probed by optical tweezer

NASA Astrophysics Data System (ADS)

Castelain, Mickaël; Pignon, Frédéric; Piau, Jean-Michel; Magnin, Albert; Mercier-Bonin, Muriel; Schmitz, Philippe

2007-10-01

In agroindustry, the hygiene of solid surfaces is of primary importance in order to ensure that products are safe for consumers. To improve safety, one of the major ways consists in identifying and understanding the mechanisms of microbial cell adhesion to nonporous solid surfaces or filtration membranes. In this paper we investigate the adhesion of the yeast cell Saccharomyces cerevisiae (about 5μm in diameter) to a model solid surface, using well-defined hydrophilic glass substrates. An optical tweezer device developed by Piau [J. Non-Newtonian Fluid Mech. 144, 1 (2007)] was applied to yeast cells in contact with well-characterized glass surfaces. Two planes of observation were used to obtain quantitative measurements of removal forces and to characterize the corresponding mechanisms at a micrometer length scale. The results highlight various adhesion mechanisms, depending on the ionic strength, contact time, and type of yeast. The study has allowed to show a considerable increase of adhering cells with the ionic strength and has provided a quantitative measurement of the detachment forces of cultured yeast cells. Force levels are found to grow with ionic strength and differences in mobility are highlighted. The results clearly underline that a microrheological approach is essential for analyzing the adhesion mechanisms of biological systems at the relevant local scales.

Freezing and melting of salt hydrates next to solid surfaces probed by infrared-visible sum frequency generation spectroscopy.

PubMed

Anim-Danso, Emmanuel; Zhang, Yu; Dhinojwala, Ali

2013-06-12

Understanding the freezing of salt solutions near solid surfaces is important in many scientific fields. Here we use sum frequency generation (SFG) spectroscopy to study the freezing of a NaCl solution next to a sapphire substrate. During cooling we observe two transitions. The first corresponds to segregation of concentrated brine next to the sapphire surface as we cool the system down to the region where ice and brine phases coexist. At this transition, the intensity of the ice-like peak decreases, suggesting the disruption of hydrogen-bonding by sodium ions. The second transition corresponds to the formation of NaCl hydrates with abrupt changes in both the SFG intensity and the sharpness of spectral peaks. The similarity in the position of the SFG peaks with those observed using IR and Raman spectroscopy indicates the formation of NaCl·2H2O crystals next to the sapphire substrate. The melting temperatures of the hydrates are very similar to those reported for bulk NaCl·2H2O. This study enhances our understanding of nucleation and freezing of salt solutions on solid surfaces and the effects of salt ions on the structure of interfacial ice.

The significance of the amorphous potential energy landscape for dictating glassy dynamics and driving solid-state crystallisation.

PubMed

Ruggiero, Michael T; Krynski, Marcin; Kissi, Eric Ofosu; Sibik, Juraj; Markl, Daniel; Tan, Nicholas Y; Arslanov, Denis; van der Zande, Wim; Redlich, Britta; Korter, Timothy M; Grohganz, Holger; Löbmann, Korbinian; Rades, Thomas; Elliott, Stephen R; Zeitler, J Axel

2017-11-15

The fundamental origins surrounding the dynamics of disordered solids near their characteristic glass transitions continue to be fiercely debated, even though a vast number of materials can form amorphous solids, including small-molecule organic, inorganic, covalent, metallic, and even large biological systems. The glass-transition temperature, T g , can be readily detected by a diverse set of techniques, but given that these measurement modalities probe vastly different processes, there has been significant debate regarding the question of why T g can be detected across all of them. Here we show clear experimental and computational evidence in support of a theory that proposes that the shape and structure of the potential-energy surface (PES) is the fundamental factor underlying the glass-transition processes, regardless of the frequency that experimental methods probe. Whilst this has been proposed previously, we demonstrate, using ab initio molecular-dynamics (AIMD) simulations, that it is of critical importance to carefully consider the complete PES - both the intra-molecular and inter-molecular features - in order to fully understand the entire range of atomic-dynamical processes in disordered solids. Finally, we show that it is possible to utilise this dependence to directly manipulate and harness amorphous dynamics in order to control the behaviour of such solids by using high-powered terahertz pulses to induce crystallisation and preferential crystal-polymorph growth in glasses. Combined, these findings provide compelling evidence that the PES landscape, and the corresponding energy barriers, are the ultimate controlling feature behind the atomic and molecular dynamics of disordered solids, regardless of the frequency at which they occur.

SpectraFox: A free open-source data management and analysis tool for scanning probe microscopy and spectroscopy

NASA Astrophysics Data System (ADS)

Ruby, Michael

In the last decades scanning probe microscopy and spectroscopy have become well-established tools in nanotechnology and surface science. This opened the market for many commercial manufacturers, each with different hardware and software standards. Besides the advantage of a wide variety of available hardware, the diversity may software-wise complicate the data exchange between scientists, and the data analysis for groups working with hardware developed by different manufacturers. Not only the file format differs between manufacturers, but also the data often requires further numerical treatment before publication. SpectraFox is an open-source and independent tool which manages, processes, and evaluates scanning probe spectroscopy and microscopy data. It aims at simplifying the documentation in parallel to measurement, and it provides solid evaluation tools for a large number of data.

Physics. Creating and probing electron whispering-gallery modes in graphene.

PubMed

Zhao, Yue; Wyrick, Jonathan; Natterer, Fabian D; Rodriguez-Nieva, Joaquin F; Lewandowski, Cyprian; Watanabe, Kenji; Taniguchi, Takashi; Levitov, Leonid S; Zhitenev, Nikolai B; Stroscio, Joseph A

2015-05-08

The design of high-finesse resonant cavities for electronic waves faces challenges due to short electron coherence lengths in solids. Complementing previous approaches to confine electronic waves by carefully positioned adatoms at clean metallic surfaces, we demonstrate an approach inspired by the peculiar acoustic phenomena in whispering galleries. Taking advantage of graphene's gate-tunable light-like carriers, we create whispering-gallery mode (WGM) resonators defined by circular pn junctions, induced by a scanning tunneling probe. We can tune the resonator size and the carrier concentration under the probe in a back-gated graphene device over a wide range. The WGM-type confinement and associated resonances are a new addition to the quantum electron-optics toolbox, paving the way to develop electronic lenses and resonators. Copyright © 2015, American Association for the Advancement of Science.

Patterning of a-C DLC films: exploration of an aqueous electro-oxidative mechanism

NASA Astrophysics Data System (ADS)

Mühl, Thomas; Myhra, Sverre

2007-06-01

Conducting ion-beam assisted CVD deposited a-C type DLC films can be patterned electro-oxidatively by masked and maskless probe-induced STM-based lithography. The former constitutes a parallel rapid processing technology, with the tip acting as a distant stationary electrode. The latter is a higher spatial resolution serial technology, with the tip defining a travelling local electro-chemical cell. The mechanism is based on electro-oxidative conversion of solid carbon to gaseous CO or CO2 in the presence of an aqueous phase, either as a bulk fluid or as a thin adsorbed film. The process is constrained kinetically in the early stages by limitations on charge transport through the surface barrier at the fluid-to-solid interface and subsequently by the availability of oxidants and by their transport to reactive sites. The as-received surface is terminated by chemisorbed oxygen, leading to the formation of an insulating surface barrier. The threshold potential for initiation of conversion depends on the width of the barrier. The results may have implications for new technologies exploiting the properties of carbon-based materials, but may also add to the present understanding of the electrochemistry of carbon solids.

Picosecond Laser Pulse Interactions with Metallic and Semiconductor Surfaces.

DTIC Science & Technology

1983-11-01

Materials Research Society-Europe Meeting, Laset Solid Interactions and Transient Thermal Processing of Materials. Strasbourg, May 1983, 3. de Physique...of or assisting the heating of the sample. In this experiment the the Brillouin zone are involved, the index variations are de - probe fluence was...the entire range -of fluences below the threshold for phase transition. A de - tailed analysis of this fitting procedure is beyond the scope of 900

Probing the interface between semiconducting nanocrystals and molecular metal chalcogenide surface ligands: insights from first principles

NASA Astrophysics Data System (ADS)

Scalise, Emilio; Wippermann, Stefan; Galli, Giulia; Talapin, Dmitri

Colloidal nanocrystals (NCs) are emerging as cost-effective materials offering exciting prospects for solar energy conversion, light emission and electronic applications. Recent experimental advances demonstrate the synthesis of fully inorganic nanocrystal solids from chemical solution processing. The properties of the NC-solids are heavily determined by the NCs surface and their interactions with the host matrix. However, information on the atomistic structure of such composites is hard to obtain, due to the complexity of the synthesis conditions and the unavailability of robust experimental techniques to probe nanointerfaces at the microscopic level. Here we present a systematic theoretical study of the interaction between InAs and InP NCs with Sn2S64- ligands. Employing a grand canonical ab initio thermodynamic approach we investigate the relative stability of a multitude of configurations possibly realized at the NC-ligand interface. Our study highlights the importance of different structural details and their strong impact on the resulting composite's properties. We show that to obtain a detailed understanding of experimental data it is necessary to take into account complex interfacial structures beyond simplified NC-ligand model interfaces. S. W. acknowledges BMBF NanoMatFutur Grant No. 13N12972. G.G. acknowledges DOE-BES for funding part of this work.

Probing the Structure and Dynamics of Interfacial Water with Scanning Tunneling Microscopy and Spectroscopy.

PubMed

Guo, Jing; You, Sifan; Wang, Zhichang; Peng, Jinbo; Ma, Runze; Jiang, Ying

2018-05-27

Water/solid interfaces are ubiquitous and play a key role in many environmental, biophysical, and technological processes. Resolving the internal structure and probing the hydrogen-bond (H-bond) dynamics of the water molecules adsorbed on solid surfaces are fundamental issues of water science, which remains a great challenge owing to the light mass and small size of hydrogen. Scanning tunneling microscopy (STM) is a promising tool for attacking these problems, thanks to its capabilities of sub-Ångström spatial resolution, single-bond vibrational sensitivity, and atomic/molecular manipulation. The designed experimental system consists of a Cl-terminated tip and a sample fabricated by dosing water molecules in situ onto the Au(111)-supported NaCl(001) surfaces. The insulating NaCl films electronically decouple the water from the metal substrates, so the intrinsic frontier orbitals of water molecules are preserved. The Cl-tip facilitates the manipulation of the single water molecules, as well as gating the orbitals of water to the proximity of Fermi level (EF) via tip-water coupling. This paper outlines the detailed methods of submolecular resolution imaging, molecular/atomic manipulation, and single-bond vibrational spectroscopy of interfacial water. These studies open up a new route for investigating the H-bonded systems at the atomic scale.

Solid-Phase Nucleic Acid Sequence-Based Amplification and Length-Scale Effects during RNA Amplification.

PubMed

Ma, Youlong; Teng, Feiyue; Libera, Matthew

2018-06-05

Solid-phase oligonucleotide amplification is of interest because of possible applications to next-generation sequencing, multiplexed microarray-based detection, and cell-free synthetic biology. Its efficiency is, however, less than that of traditional liquid-phase amplification involving unconstrained primers and enzymes, and understanding how to optimize the solid-phase amplification process remains challenging. Here, we demonstrate the concept of solid-phase nucleic acid sequence-based amplification (SP-NASBA) and use it to study the effect of tethering density on amplification efficiency. SP-NASBA involves two enzymes, avian myeloblastosis virus reverse transcriptase (AMV-RT) and RNase H, to convert tethered forward and reverse primers into tethered double-stranded DNA (ds-DNA) bridges from which RNA - amplicons can be generated by a third enzyme, T7 RNA polymerase. We create microgels on silicon surfaces using electron-beam patterning of thin-film blends of hydroxyl-terminated and biotin-terminated poly(ethylene glycol) (PEG-OH, PEG-B). The tethering density is linearly related to the PEG-B concentration, and biotinylated primers and molecular beacon detection probes are tethered to streptavidin-activated microgels. While SP-NASBA is very efficient at low tethering densities, the efficiency decreases dramatically with increasing tethering density due to three effects: (a) a reduced hybridization efficiency of tethered molecular beacon detection probes; (b) a decrease in T7 RNA polymerase efficiency; (c) inhibition of T7 RNA polymerase activity by AMV-RT.

Comparison of Dorris-Gray and Schultz methods for the calculation of surface dispersive free energy by inverse gas chromatography.

PubMed

Shi, Baoli; Wang, Yue; Jia, Lina

2011-02-11

Inverse gas chromatography (IGC) is an important technique for the characterization of surface properties of solid materials. A standard method of surface characterization is that the surface dispersive free energy of the solid stationary phase is firstly determined by using a series of linear alkane liquids as molecular probes, and then the acid-base parameters are calculated from the dispersive parameters. However, for the calculation of surface dispersive free energy, generally, two different methods are used, which are Dorris-Gray method and Schultz method. In this paper, the results calculated from Dorris-Gray method and Schultz method are compared through calculating their ratio with their basic equations and parameters. It can be concluded that the dispersive parameters calculated with Dorris-Gray method will always be larger than the data calculated with Schultz method. When the measuring temperature increases, the ratio increases large. Compared with the parameters in solvents handbook, it seems that the traditional surface free energy parameters of n-alkanes listed in the papers using Schultz method are not enough accurate, which can be proved with a published IGC experimental result. © 2010 Elsevier B.V. All rights reserved.

Colloid-probe AFM studies of the interaction forces of proteins adsorbed on colloidal crystals.

PubMed

Singh, Gurvinder; Bremmell, Kristen E; Griesser, Hans J; Kingshott, Peter

2015-04-28

In recent years, colloid-probe AFM has been used to measure the direct interaction forces between colloidal particles of different size or surface functionality in aqueous media, as one can study different forces in symmerical systems (i.e., sphere-sphere geometry). The present study investigates the interaction between protein coatings on colloid probes and hydrophilic surfaces decorated with hexagonally close packed single particle layers that are either uncoated or coated with proteins. Controlled solvent evaporation from aqueous suspensions of colloidal particles (coated with or without lysozyme and albumin) produces single layers of close-packed colloidal crystals over large areas on a solid support. The measurements have been carried out in an aqueous medium at different salt concentrations and pH values. The results show changes in the interaction forces as the surface charge of the unmodified or modified particles, and ionic strength or pH of the solution is altered. At high ionic strength or pH, electrostatic interactions are screened, and a strong repulsive force at short separation below 5 nm dominates, suggesting structural changes in the absorbed protein layer on the particles. We also study the force of adhesion, which decreases with an increment in the salt concentration, and the interaction between two different proteins indicating a repulsive interaction on approach and adhesion on retraction.

Electrochemical Quartz Crystal Microbalance with Dissipation Real-Time Hydrodynamic Spectroscopy of Porous Solids in Contact with Liquids.

PubMed

Sigalov, Sergey; Shpigel, Netanel; Levi, Mikhael D; Feldberg, Moshe; Daikhin, Leonid; Aurbach, Doron

2016-10-18

Using multiharmonic electrochemical quartz crystal microbalance with dissipation (EQCM-D) monitoring, a new method of characterization of porous solids in contact with liquids has been developed. The dynamic gravimetric information on the growing, dissolving, or stationary stored solid deposits is supplemented by their precise in-operando porous structure characterization on a mesoscopic scale. We present a very powerful method of quartz-crystal admittance modeling of hydrodynamic solid-liquid interactions in order to extract the porous structure parameters of solids during their formation in real time, using different deposition modes. The unique hydrodynamic spectroscopic characterization of electrolytic and rf-sputtered solid Cu coatings that we use for our "proof of concept" provides a new strategy for probing various electrochemically active thin and thick solid deposits, thereby offering inexpensive, noninvasive, and highly efficient quantitative control over their properties. A broad spectrum of applications of our method is proposed, from various metal electroplating and finishing technologies to deeper insight into dynamic build-up and subsequent development of solid-electrolyte interfaces in the operation of Li-battery electrodes, as well as monitoring hydrodynamic consequences of metal corrosion, and growth of biomass coatings (biofouling) on different solid surfaces in seawater.

Probing and mapping electrode surfaces in solid oxide fuel cells.

PubMed

Blinn, Kevin S; Li, Xiaxi; Liu, Mingfei; Bottomley, Lawrence A; Liu, Meilin

2012-09-20

Solid oxide fuel cells (SOFCs) are potentially the most efficient and cost-effective solution to utilization of a wide variety of fuels beyond hydrogen (1-7). The performance of SOFCs and the rates of many chemical and energy transformation processes in energy storage and conversion devices in general are limited primarily by charge and mass transfer along electrode surfaces and across interfaces. Unfortunately, the mechanistic understanding of these processes is still lacking, due largely to the difficulty of characterizing these processes under in situ conditions. This knowledge gap is a chief obstacle to SOFC commercialization. The development of tools for probing and mapping surface chemistries relevant to electrode reactions is vital to unraveling the mechanisms of surface processes and to achieving rational design of new electrode materials for more efficient energy storage and conversion(2). Among the relatively few in situ surface analysis methods, Raman spectroscopy can be performed even with high temperatures and harsh atmospheres, making it ideal for characterizing chemical processes relevant to SOFC anode performance and degradation(8-12). It can also be used alongside electrochemical measurements, potentially allowing direct correlation of electrochemistry to surface chemistry in an operating cell. Proper in situ Raman mapping measurements would be useful for pin-pointing important anode reaction mechanisms because of its sensitivity to the relevant species, including anode performance degradation through carbon deposition(8, 10, 13, 14) ("coking") and sulfur poisoning(11, 15) and the manner in which surface modifications stave off this degradation(16). The current work demonstrates significant progress towards this capability. In addition, the family of scanning probe microscopy (SPM) techniques provides a special approach to interrogate the electrode surface with nanoscale resolution. Besides the surface topography that is routinely collected by AFM and STM, other properties such as local electronic states, ion diffusion coefficient and surface potential can also be investigated(17-22). In this work, electrochemical measurements, Raman spectroscopy, and SPM were used in conjunction with a novel test electrode platform that consists of a Ni mesh electrode embedded in an yttria-stabilized zirconia (YSZ) electrolyte. Cell performance testing and impedance spectroscopy under fuel containing H2S was characterized, and Raman mapping was used to further elucidate the nature of sulfur poisoning. In situ Raman monitoring was used to investigate coking behavior. Finally, atomic force microscopy (AFM) and electrostatic force microscopy (EFM) were used to further visualize carbon deposition on the nanoscale. From this research, we desire to produce a more complete picture of the SOFC anode.

Probing and Mapping Electrode Surfaces in Solid Oxide Fuel Cells

PubMed Central

Blinn, Kevin S.; Li, Xiaxi; Liu, Mingfei; Bottomley, Lawrence A.; Liu, Meilin

2012-01-01

Solid oxide fuel cells (SOFCs) are potentially the most efficient and cost-effective solution to utilization of a wide variety of fuels beyond hydrogen 1-7. The performance of SOFCs and the rates of many chemical and energy transformation processes in energy storage and conversion devices in general are limited primarily by charge and mass transfer along electrode surfaces and across interfaces. Unfortunately, the mechanistic understanding of these processes is still lacking, due largely to the difficulty of characterizing these processes under in situ conditions. This knowledge gap is a chief obstacle to SOFC commercialization. The development of tools for probing and mapping surface chemistries relevant to electrode reactions is vital to unraveling the mechanisms of surface processes and to achieving rational design of new electrode materials for more efficient energy storage and conversion2. Among the relatively few in situ surface analysis methods, Raman spectroscopy can be performed even with high temperatures and harsh atmospheres, making it ideal for characterizing chemical processes relevant to SOFC anode performance and degradation8-12. It can also be used alongside electrochemical measurements, potentially allowing direct correlation of electrochemistry to surface chemistry in an operating cell. Proper in situ Raman mapping measurements would be useful for pin-pointing important anode reaction mechanisms because of its sensitivity to the relevant species, including anode performance degradation through carbon deposition8, 10, 13, 14 ("coking") and sulfur poisoning11, 15 and the manner in which surface modifications stave off this degradation16. The current work demonstrates significant progress towards this capability. In addition, the family of scanning probe microscopy (SPM) techniques provides a special approach to interrogate the electrode surface with nanoscale resolution. Besides the surface topography that is routinely collected by AFM and STM, other properties such as local electronic states, ion diffusion coefficient and surface potential can also be investigated17-22. In this work, electrochemical measurements, Raman spectroscopy, and SPM were used in conjunction with a novel test electrode platform that consists of a Ni mesh electrode embedded in an yttria-stabilized zirconia (YSZ) electrolyte. Cell performance testing and impedance spectroscopy under fuel containing H2S was characterized, and Raman mapping was used to further elucidate the nature of sulfur poisoning. In situ Raman monitoring was used to investigate coking behavior. Finally, atomic force microscopy (AFM) and electrostatic force microscopy (EFM) were used to further visualize carbon deposition on the nanoscale. From this research, we desire to produce a more complete picture of the SOFC anode. PMID:23023264

Phosphorus Enrichment as a New Composition in the Solid Electrolyte Interphase of High-Voltage Cathodes and Its Effects on Battery Cycling

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

Yan, Pengfei; Zheng, Jianming; Kuppan, Saravanan

2015-11-10

Immersion of a solid into liquid often leads to the modification of both the structure and chemistry of surface of the solid, which subsequently affects the chemical and physical properties of the system. For the case of the rechargeable lithium ion battery, such a surface modification is termed as solid electrolyte interphase (SEI) layer, which has been perceived to play critical role for the stable operation of the batteries. However, the structure and chemical composition of SEI layer and its spatial distribution and dependence on the battery operating condition remain unclear. By using aberration corrected scanning transmission electron microscopy coupledmore » with ultra-high sensitive energy dispersive x-ray spectroscopy, we probed the structure and chemistry of SEI layer on several high voltage cathodes. We show that layer-structured cathodes, when cycled at a high cut off voltage, can form a P-rich SEI layer on their surface, which is a direct evidence of Li-salt (LiPF6) decomposition. Our systematical investigations indicate such cathode/Li-salt side reaction shows strong dependence on structure of the cathode materials, operating voltage and temperature, indicating the feasibility of SEI engineering. These findings provide us valuable insights into the complex interface between the high-voltage cathode and the electrolyte.« less

Probing the molecular-level control of aluminosilicate dissolution: A sensitive solid-state NMR proxy for reactive surface area

NASA Astrophysics Data System (ADS)

Washton, Nancy M.; Brantley, Susan L.; Mueller, Karl T.

2008-12-01

For two suites of volcanic aluminosilicate glasses, the accessible and reactive sites for covalent attachment of the fluorine-containing (3,3,3-trifluoropropyl)dimethylchlorosilane (TFS) probe molecule were measured by quantitative 19F nuclear magnetic resonance (NMR) spectroscopy. The first set of samples consists of six rhyolitic and dacitic glasses originating from volcanic activity in Iceland and one rhyolitic glass from the Bishop Tuff, CA. Due to differences in the reactive species present on the surfaces of these glasses, variations in the rate of acid-mediated dissolution (pH 4) for samples in this suite cannot be explained by variations in geometric or BET-measured surface area. In contrast, the rates scale directly with the surface density of TFS-reactive sites as measured by solid-state NMR. These data are consistent with the inference that the TFS-reactive M-OH species on the glass surface, which are known to be non-hydrogen-bonded Q 3 groups, represent loci accessible to and affected by proton-mediated dissolution. The second suite of samples, originating from a chronosequence in Kozushima, Japan, is comprised of four rhyolites that have been weathered for 1.1, 1.8, 26, and 52 ka. The number of TFS-reactive sites per gram increases with duration of weathering in the laboratory for the "Icelandic" samples and with duration of field weathering for both "Icelandic" and Japanese samples. One hypothesis is consistent with these and published modeling, laboratory, and field observations: over short timescales, dissolution is controlled by fast-dissolving sites, but over long timescales, dissolution is controlled by slower-dissolving sites, the surface density of which is proportional to the number of TFS-reactive Q 3 sites. These latter sites are not part of a hydrogen-bonded network on the surface of the glasses, and measurement of their surface site density allows predictions of trends in reactive surface area. The TFS treatment method, which is easily monitored by quantitative 19F solid-state NMR, therefore provides a chemically specific and quantifiable proxy to understand the nature of how sites on dissolving silicates control dissolution. Furthermore, 27Al NMR techniques are shown here to be useful in identifying clays on the glass surfaces, and these methods are therefore effective for quantifying concentrations of weathering impurities. Our interpretations offer a testable hypothesis for the mechanism of proton-promoted dissolution for low-iron aluminosilicate minerals and glasses and suggest that future investigations of reactive surfaces with high-sensitivity NMR techniques are warranted.

Transfer impedance measurements of the space shuttle Solid Rocket Motor (SRM) joints, wire meshes and a carbon graphite motor case

NASA Technical Reports Server (NTRS)

Papazian, Peter B.; Perala, Rodney A.; Curry, John D.; Lankford, Alan B.; Keller, J. David

1988-01-01

Using three different current injection methods and a simple voltage probe, transfer impedances for Solid Rocket Motor (SRM) joints, wire meshes, aluminum foil, Thorstrand and a graphite composite motor case were measured. In all cases, the surface current distribution for the particular current injection device was calculated analytically or by finite difference methods. The results of these calculations were used to generate a geometric factor which was the ratio of total injected current to surface current density. The results were validated in several ways. For wire mesh measurements, results showed good agreement with calculated results for a 14 by 18 Al screen. SRM joint impedances were independently verified. The filiment wound case measurement results were validated only to the extent that their curve shape agrees with the expected form of transfer impedance for a homogeneous slab excited by a plane wave source.

Performance of Surface-Mount Ceramic and Solid Tantalum Capacitors for Cryogenic Applications

NASA Technical Reports Server (NTRS)

Patterson, Richard L.; MacDonald, Thomas L.; Hammoud, Ahmad; Gerber, Scott

1998-01-01

Low temperature electronics are of great interest for space exploration programs. These include missions to the outer planets, earth-orbiting and deep-space probes, remote-sensing and communication satellites. Terrestrial applications would also benefit from the availability of low temperature electronics. Power components capable of low temperature operation would, thus, enhance the technologies needed for the development of advanced power systems suitable for use in harsh environments. In this work, ceramic and solid tantalum capacitors were evaluated in terms of their dielectric properties as a function of temperature and at various frequencies. The surface-mount devices were characterized in terms of their capacitance stability and dissipation factor in the frequency range of 50 Hz to 100 kHz at temperatures ranging from room temperature (20 deg. C) to about liquid nitrogen temperature (-190 deg. C). The results are discussed and conclusions made concerning the suitability of the capacitors investigated for low temperature applications.

Fiber-Optical Sensors: Basics and Applications in Multiphase Reactors

PubMed Central

Li, Xiangyang; Yang, Chao; Yang, Shifang; Li, Guozheng

2012-01-01

This work presents a brief introduction on the basics of fiber-optical sensors and an overview focused on the applications to measurements in multiphase reactors. The most commonly principle utilized is laser back scattering, which is also the foundation for almost all current probes used in multiphase reactors. The fiber-optical probe techniques in two-phase reactors are more developed than those in three-phase reactors. There are many studies on the measurement of gas holdup using fiber-optical probes in three-phase fluidized beds, but negative interference of particles on probe function was less studied. The interactions between solids and probe tips were less studied because glass beads etc. were always used as the solid phase. The vision probes may be the most promising for simultaneous measurements of gas dispersion and solids suspension in three-phase reactors. Thus, the following techniques of the fiber-optical probes in multiphase reactors should be developed further: (1) online measuring techniques under nearly industrial operating conditions; (2) corresponding signal data processing techniques; (3) joint application with other measuring techniques.

Probing electrokinetics in microchannels and nanochannels with electrochemical measurements

NASA Astrophysics Data System (ADS)

Schiffbauer, Jarrod; Park, Sinwook; Yossifon, Gilad

2013-11-01

We present a brief review of recent experimental and theoretical results concerning the use of electrochemical impedance spectroscopy (EIS), in conjunction with other electrochemical measurements (chronoamperometry, linear sweep voltammetry), to characterize the response of micro- and nanofluidic systems. Using these techniques, the interplay between conduction, diffusion, and convection are probed across a range of time- and length scales. The resulting information permits characterization of the respective roles of processes in both micro- and nanchannel regions of a fluidic device. Such techniques provide a useful probe of transient behavior at the micro-nanochannel interface, have great potential in biomolecular sensing applications, and may be useful in the study of surface properties at the fluid-solid interface. We wish to acknowledge Israel Science Foundation, grant number 2015240, the Technion Russel-Berrie Nanotechnology Institute (RBNI) and a fellowship grant from the Techion Faculty of Mechanical Engineering.

Physicochemical characterization of D-mannitol polymorphs: the challenging surface energy determination by inverse gas chromatography in the infinite dilution region.

PubMed

Cares-Pacheco, M G; Vaca-Medina, G; Calvet, R; Espitalier, F; Letourneau, J-J; Rouilly, A; Rodier, E

2014-11-20

Nowadays, it is well known that surface interactions play a preponderant role in mechanical operations, which are fundamental in pharmaceutical processing and formulation. Nevertheless, it is difficult to correlate surface behaviour in processes to physical properties measurement. Indeed, most pharmaceutical solids have multiple surface energies because of varying forms, crystal faces and impurities contents or physical defects, among others. In this paper, D-mannitol polymorphs (α, β and δ) were studied through different characterization techniques highlighting bulk and surface behaviour differences. Due to the low adsorption behaviour of β and δ polymorphs, special emphasis has been paid to surface energy analysis by inverse gas chromatography, IGC. Surface energy behaviour has been studied in Henry's domain showing that, for some organic solids, the classical IGC infinite dilution zone is never reached. IGC studies highlighted, without precedent in literature, dispersive surface energy differences between α and β mannitol, with a most energetically active α form with a γ(s)(d) of 74.9 mJ·m⁻². Surface heterogeneity studies showed a highly heterogeneous α mannitol with a more homogeneous β (40.0 mJ·m⁻²) and δ mannitol (40.3 mJ·m⁻²). Moreover, these last two forms behaved similarly considering surface energy at different probe concentrations. Copyright © 2014 Elsevier B.V. All rights reserved.

Interrelationships among Grain Size, Surface Composition, Air Stability, and Interfacial Resistance of Al-Substituted Li7La3Zr2O12 Solid Electrolytes.

PubMed

Cheng, Lei; Wu, Cheng Hao; Jarry, Angelique; Chen, Wei; Ye, Yifan; Zhu, Junfa; Kostecki, Robert; Persson, Kristin; Guo, Jinghua; Salmeron, Miquel; Chen, Guoying; Doeff, Marca

2015-08-19

The interfacial resistances of symmetrical lithium cells containing Al-substituted Li7La3Zr2O12 (LLZO) solid electrolytes are sensitive to their microstructures and histories of exposure to air. Air exposure of LLZO samples with large grain sizes (∼150 μm) results in dramatically increased interfacial impedances in cells containing them, compared to those with pristine large-grained samples. In contrast, a much smaller difference is seen between cells with small-grained (∼20 μm) pristine and air-exposed LLZO samples. A combination of soft X-ray absorption (sXAS) and Raman spectroscopy, with probing depths ranging from nanometer to micrometer scales, revealed that the small-grained LLZO pellets are more air-stable than large-grained ones, forming far less surface Li2CO3 under both short- and long-term exposure conditions. Surface sensitive X-ray photoelectron spectroscopy (XPS) indicates that the better chemical stability of the small-grained LLZO is related to differences in the distribution of Al and Li at sample surfaces. Density functional theory calculations show that LLZO can react via two different pathways to form Li2CO3. The first, more rapid, pathway involves a reaction with moisture in air to form LiOH, which subsequently absorbs CO2 to form Li2CO3. The second, slower, pathway involves direct reaction with CO2 and is favored when surface lithium contents are lower, as with the small-grained samples. These observations have important implications for the operation of solid-state lithium batteries containing LLZO because the results suggest that the interfacial impedances of these devices is critically dependent upon specific characteristics of the solid electrolyte and how it is prepared.

What experiments on pinned nanobubbles can tell about the critical nucleus for bubble nucleation.

PubMed

Xiao, Qianxiang; Liu, Yawei; Guo, Zhenjiang; Liu, Zhiping; Frenkel, Daan; Dobnikar, Jure; Zhang, Xianren

2017-12-22

The process of homogeneous bubble nucleation is almost impossible to probe experimentally, except near the critical point or for liquids under large negative tension. Elsewhere in the phase diagram, the bubble nucleation barrier is so high as to be effectively insurmountable. Consequently, there is a severe lack of experimental studies of homogenous bubble nucleation under conditions of practical importance (e.g., cavitation). Here we use a simple geometric relation to show that we can obtain information about the homogeneous nucleation process from Molecular Dynamics studies of bubble formation in solvophobic nanopores on a solid surface. The free energy of pinned nanobubbles has two extrema as a function of volume: one state corresponds to a free-energy maximum ("the critical nucleus"), the other corresponds to a free-energy minimum (the metastable, pinned nanobubble). Provided that the surface tension does not depend on nanobubble curvature, the radius of the curvature of the metastable surface nanobubble is independent of the radius of the pore and is equal to the radius of the critical nucleus in homogenous bubble nucleation. This observation opens the way to probe the parameters that determine homogeneous bubble nucleation under experimentally accessible conditions, e.g. with AFM studies of metastable nanobubbles. Our theoretical analysis also indicates that a surface with pores of different sizes can be used to determine the curvature corrections to the surface tension. Our conclusions are not limited to bubble nucleation but suggest that a similar approach could be used to probe the structure of critical nuclei in crystal nucleation.

Dynamic and label-free high-throughput detection of biomolecular interactions based on phase-shift interferometry

NASA Astrophysics Data System (ADS)

Li, Qiang; Huang, Guoliang; Gan, Wupeng; Chen, Shengyi

2009-08-01

Biomolecular interactions can be detected by many established technologies such as fluorescence imaging, surface plasmon resonance (SPR)[1-4], interferometry and radioactive labeling of the analyte. In this study, we have designed and constructed a label-free, real-time sensing platform and its operating imaging instrument that detects interactions using optical phase differences from the accumulation of biological material on solid substrates. This system allows us to monitor biomolecular interactions in real time and quantify concentration changes during micro-mixing processes by measuring the changes of the optical path length (OPD). This simple interferometric technology monitors the optical phase difference resulting from accumulated biomolecular mass. A label-free protein chip that forms a 4×4 probe array was designed and fabricated using a commercial microarray robot spotter on solid substrates. Two positive control probe lines of BSA (Bovine Serum Albumin) and two experimental human IgG and goat IgG was used. The binding of multiple protein targets was performed and continuously detected by using this label-free and real-time sensing platform.

Nucleic acid detection methods

DOEpatents

Smith, C.L.; Yaar, R.; Szafranski, P.; Cantor, C.R.

1998-05-19

The invention relates to methods for rapidly determining the sequence and/or length a target sequence. The target sequence may be a series of known or unknown repeat sequences which are hybridized to an array of probes. The hybridized array is digested with a single-strand nuclease and free 3{prime}-hydroxyl groups extended with a nucleic acid polymerase. Nuclease cleaved heteroduplexes can be easily distinguish from nuclease uncleaved heteroduplexes by differential labeling. Probes and target can be differentially labeled with detectable labels. Matched target can be detected by cleaving resulting loops from the hybridized target and creating free 3-hydroxyl groups. These groups are recognized and extended by polymerases added into the reaction system which also adds or releases one label into solution. Analysis of the resulting products using either solid phase or solution. These methods can be used to detect characteristic nucleic acid sequences, to determine target sequence and to screen for genetic defects and disorders. Assays can be conducted on solid surfaces allowing for multiple reactions to be conducted in parallel and, if desired, automated. 18 figs.

Equivalence of chain conformations in the surface region of a polymer melt and a single Gaussian chain under critical conditions.

PubMed

Skvortsov, A M; Leermakers, F A M; Fleer, G J

2013-08-07

In the melt polymer conformations are nearly ideal according to Flory's ideality hypothesis. Silberberg generalized this statement for chains in the interfacial region. We check the Silberberg argument by analyzing the conformations of a probe chain end-grafted at a solid surface in a sea of floating free chains of concentration φ by the self-consistent field (SCF) method. Apart from the grafting, probe chain and floating chains are identical. Most of the results were obtained for a standard SCF model with freely jointed chains on a six-choice lattice, where immediate step reversals are allowed. A few data were generated for a five-choice lattice, where such step reversals are forbidden. These coarse-grained models describe the equilibrium properties of flexible atactic polymer chains at the scale of the segment length. The concentration was varied over the whole range from φ = 0 (single grafted chain) to φ = 1 (probe chain in the melt). The number of contacts with the surface, average height of the free end and its dispersion, average loop and train length, tail size distribution, end-point and overall segment distributions were calculated for a grafted probe chain as a function of φ, for several chain lengths and substrate∕polymer interactions, which were varied from strong repulsion to strong adsorption. The computations show that the conformations of the probe chain in the melt do not depend on substrate∕polymer interactions and are very similar to the conformations of a single end-grafted chain under critical conditions, and can thus be described analytically. When the substrate∕polymer interaction is fixed at the value corresponding to critical conditions, all equilibrium properties of a probe chain are independent of φ, over the whole range from a dilute solution to the melt. We believe that the conformations of all flexible chains in the surface region of the melt are close to those of an appropriate single chain in critical conditions, provided that one end of the single chain is fixed at the same point as a chain in the melt.

Nonlinear friction dynamics on polymer surface under accelerated movement

NASA Astrophysics Data System (ADS)

Aita, Yuuki; Asanuma, Natsumi; Takahashi, Akira; Mayama, Hiroyuki; Nonomura, Yoshimune

2017-04-01

Nonlinear phenomena on the soft material surface are one of the most exciting topics of chemical physics. However, only a few reports exist on the friction phenomena under accelerated movement, because friction between two solid surfaces is considered a linear phenomenon in many cases. We aim to investigate how nonlinear accelerated motion affects friction on solid surfaces. In the present study, we evaluate the frictional forces between two polytetrafluoroethylene (PTFE) resins using an advanced friction evaluation system. On PTFE surfaces, the normalized delay time δ, which is the time lag in the response of the friction force to the accelerated movement, is observed in the pre-sliding friction process. Under high-velocity conditions, kinetic friction increases with velocity. Based on these experimental results, we propose a two-phase nonlinear model including a pre-sliding process (from the beginning of sliding of a contact probe to the establishment of static friction) and a kinetic friction process. The present model consists of several factors including velocity, acceleration, stiffness, viscosity, and vertical force. The findings reflecting the viscoelastic properties of soft material is useful for various fields such as in the fabrication of clothes, cosmetics, automotive materials, and virtual reality systems as well as for understanding friction phenomena on soft material surfaces.

Designable ultra-smooth ultra-thin solid-electrolyte interphases of three alkali metal anodes.

PubMed

Gu, Yu; Wang, Wei-Wei; Li, Yi-Juan; Wu, Qi-Hui; Tang, Shuai; Yan, Jia-Wei; Zheng, Ming-Sen; Wu, De-Yin; Fan, Chun-Hai; Hu, Wei-Qiang; Chen, Zhao-Bin; Fang, Yuan; Zhang, Qing-Hong; Dong, Quan-Feng; Mao, Bing-Wei

2018-04-09

Dendrite growth of alkali metal anodes limited their lifetime for charge/discharge cycling. Here, we report near-perfect anodes of lithium, sodium, and potassium metals achieved by electrochemical polishing, which removes microscopic defects and creates ultra-smooth ultra-thin solid-electrolyte interphase layers at metal surfaces for providing a homogeneous environment. Precise characterizations by AFM force probing with corroborative in-depth XPS profile analysis reveal that the ultra-smooth ultra-thin solid-electrolyte interphase can be designed to have alternating inorganic-rich and organic-rich/mixed multi-layered structure, which offers mechanical property of coupled rigidity and elasticity. The polished metal anodes exhibit significantly enhanced cycling stability, specifically the lithium anodes can cycle for over 200 times at a real current density of 2 mA cm -2 with 100% depth of discharge. Our work illustrates that an ultra-smooth ultra-thin solid-electrolyte interphase may be robust enough to suppress dendrite growth and thus serve as an initial layer for further improved protection of alkali metal anodes.

Back-surface gold mirrors for vibrationally resonant sum-frequency (VR-SFG) spectroscopy using 3-mercaptopropyltrimethoxysilane as an adhesion promoter.

PubMed

Quast, Arthur D; Zhang, Feng; Linford, Matthew R; Patterson, James E

2011-06-01

Back-surface mirrors are needed as reference materials for vibrationally resonant sum-frequency generation (VR-SFG) probing of liquid-solid interfaces. Conventional noble metal mirrors are not suitable for back-surface applications due to the presence of a metal adhesion layer (chromium or titanium) between the window substrate and the reflective metal surface. Using vapor deposited 3-mercaptopropyltrimethoxysilane (MPTMS) as a bi-functional adhesion promoter, gold mirrors were fabricated on fused silica substrates. These mirrors exhibit excellent gold adhesion as determined by the Scotch(®) tape test. They also produce minimal spectroscopic interference in the C-H stretching region (2800-3000 cm(-1)), as characterized by VR-SFG. These mirrors are thus robust and can be used as back-surface mirrors for a variety of applications, including reference mirrors for VR-SFG.

Complementarity in radiochemical and infrared spectroscopic characterization of electrode adsorption

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

Wieckowski, A.

1994-03-01

Radioactive labelling and infrared spectroscopy are frequently used as direct, in situ probes into the structure of the electrochemical solid/liquid interface. These techniques are compared, in a polemical fashion, in the context of a recent publication by Parry et al. (Langmuir 1993, 9, 1878) where the research potential of the former technique was not adequately depicted. It is shown that radiotracers can clearly differentiate between the surface and solution species, both neutrals and anions. In addition to the surface specificity, the radiotracers offer a quantitative determination of adsorbate surface concentrations, a feature not yet demonstrated with surface infrared spectroscopy inmore » electrochemistry. Therefore, these two techniques are complementary. Examples of the combined radiochemical and spectroscopic measurements of adsorption with equivalent (smooth) electrode surfaces are quoted. 11 refs., 2 figs.« less

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

Yuan, Chunqing; Smith, R. Scott; Kay, Bruce D.

The crystallization kinetics of nanoscale amorphous solid water (ASW) films are investigated using temperature-programmed desorption (TPD) and reflection absorption infrared spectroscopy (RAIRS). TPD measurements are used to probe surface crystallization and RAIRS measurements are used to probe bulk crystallization. Isothermal TPD results show that surface crystallization is independent of the film thickness (from 100 to 1000 ML). Conversely, the RAIRS measurements show that the bulk crystallization time increases linearly with increasing film thickness. These results suggest that nucleation and crystallization begin at the ASW/vacuum interface and then the crystallization growth front propagates linearly into the bulk. This mechanism was confirmedmore » by selective placement of an isotopic layer (5% D2O in H2O) at various positions in an ASW (H2O) film. In this case, the closer the isotopic layer was to the vacuum interface, the earlier the isotopic layer crystallized. These experiments provide direct evidence to confirm that ASW crystallization in vacuum proceeds by a “top-down” crystallization mechanism.« less

Phase coherence and Andreev reflection in topological insulator devices

DOE PAGES

Finck, A. D. K.; Kurter, C.; Hor, Y. S.; ...

2014-11-04

Topological insulators (TIs) have attracted immense interest because they host helical surface states. Protected by time-reversal symmetry, they are robust to nonmagnetic disorder. When superconductivity is induced in these helical states, they are predicted to emulate p-wave pairing symmetry, with Majorana states bound to vortices. Majorana bound states possess non-Abelian exchange statistics that can be probed through interferometry. Here, we take a significant step towards Majorana interferometry by observing pronounced Fabry-Pérot oscillations in a TI sandwiched between a superconducting and a normal lead. For energies below the superconducting gap, we observe a doubling in the frequency of the oscillations, arisingmore » from an additional phase from Andreev reflection. When a magnetic field is applied perpendicular to the TI surface, a number of very sharp and gate-tunable conductance peaks appear at or near zero energy, which has consequences for interpreting spectroscopic probes of Majorana fermions. Our results show that TIs are a promising platform for exploring phase-coherent transport in a solid-state system.« less

One-step synthesis of nitrogen, boron co-doped fluorescent carbon nanoparticles for glucose detection.

PubMed

Liang, Meijuan; Ren, Yi; Zhang, Haijuan; Ma, Yunxia; Niu, Xiaoying; Chen, Xingguo

2017-09-01

Heteroatom-doped carbon nanoparticles (CNPs) have attracted considerable attention due to an effective improvement in their intrinsic properties. Here, a facile and simple synthesis of nitrogen, boron co-doped carbon nanoparticles (NB-CNPs) from a sole precursor, 3-aminophenylboronic acid, was performed via a one-step solid-phase approach. Because of the presence of boronic acid, NB-CNPs can be used directly as a fluorescent probe for glucose. Based on a boronic acid-triggered specific reaction, we developed a simple NB-CNP probe without surface modification for the detection of glucose. When glucose was introduced, the fluorescence of NB-CNPs was suppressed through a surface-quenching states mechanism. Obvious fluorescence quenching allowed the highly sensitive determination of glucose with a limit of detection of 1.8 μM. Moreover, the proposed method has been successfully used to detect glucose in urine from people with diabetes, suggesting potential application in sensing glucose. Copyright © 2017 John Wiley & Sons, Ltd.

Phoenix Dodo Trench

NASA Image and Video Library

2008-06-04

This image was taken by NASA's Phoenix Mars Lander's Robotic Arm Camera (RAC) on the ninth Martian day of the mission, or Sol 9 (June 3, 2008). The center of the image shows a trench informally called "Dodo" after the second dig. "Dodo" is located within the previously determined digging area, informally called "Knave of Hearts." The light square to the right of the trench is the Robotic Arm's Thermal and Electrical Conductivity Probe (TECP). The Robotic Arm has scraped to a bright surface which indicated the Arm has reached a solid structure underneath the surface, which has been seen in other images as well. http://photojournal.jpl.nasa.gov/catalog/PIA10763

Transurethral ultrasonic ureterolithotripsy using a solid-wire probe.

PubMed

Chaussy, C; Fuchs, G; Kahn, R; Hunter, P; Goodfriend, R

1987-05-01

A multicenter study evaluates a new technique for transurethral ultrasonic ureterolithotripsy utilizing a solid-wire probe. The transverse vibrations of the probe cause greater stone disintegration. A small ureteroscope is used and a basket is not required. There was a 96.6 per cent success rate in 118 cases. This technique has significantly improved ultrasonic lithotripsy. It has proved to be useful for upper ureteral stones not amenable to extracorporeal shock-wave lithotripsy and lower ureteral stones including "steinstrasse."

Solid strong base K-Pt/NaY zeolite nano-catalytic system for completed elimination of formaldehyde at room temperature

NASA Astrophysics Data System (ADS)

Song, Shaoqing; Wu, Xi; Lu, Changhai; Wen, Meicheng; Le, Zhanggao; Jiang, Shujuan

2018-06-01

Solid strong base nano-catalytic system of K-modification NaY zeolite supported 0.08% Pt (K-Pt/NaY) were constructed for eliminating HCHO at room temperature. In the catalytic process, activation energy over K-Pt/NaY nano-catalytic system was greatly decreased along with the enhanced reaction rate. Characterization and catalytic tests revealed the surface electron structure of K-Pt/NaY was improved, as reflected by the enhanced HCHO adsorption capability, high sbnd OH concentration, and low-temperature reducibility. Therefore, the optimal K-Pt/NaY showed high catalytic efficiency and strong H2O tolerance for HCHO elimination by directly promoting the reaction between active sbnd OH and formate species. These results may suggest a new way for probing the advanced solid strong base nano-catalytic system for the catalytic elimination of indoor HCHO.

Visualising reacting single atoms under controlled conditions: Advances in atomic resolution in situ Environmental (Scanning) Transmission Electron Microscopy (E(S)TEM)

NASA Astrophysics Data System (ADS)

Boyes, Edward D.; Gai, Pratibha L.

2014-02-01

Advances in atomic resolution Environmental (Scanning) Transmission Electron Microscopy (E(S)TEM) for probing gas-solid catalyst reactions in situ at the atomic level under controlled reaction conditions of gas environment and temperature are described. The recent development of the ESTEM extends the capability of the ETEM by providing the direct visualisation of single atoms and the atomic structure of selected solid state heterogeneous catalysts in their working states in real-time. Atomic resolution E(S)TEM provides a deeper understanding of the dynamic atomic processes at the surface of solids and their mechanisms of operation. The benefits of atomic resolution-E(S)TEM to science and technology include new knowledge leading to improved technological processes with substantial economic benefits, improved healthcare, reductions in energy needs and the management of environmental waste generation. xml:lang="fr"

Minimally invasive photopolymerization in intervertebral disc tissue cavities

NASA Astrophysics Data System (ADS)

Schmocker, Andreas M.; Khoushabi, Azadeh; Gantenbein-Ritter, Benjamin; Chan, Samantha; Bonél, Harald Marcel; Bourban, Pierre-Etienne; Mânson, Jan Anders; Schizas, Constantin; Pioletti, Dominique; Moser, Christophe

2014-03-01

Photopolymerized hydrogels are commonly used for a broad range of biomedical applications. As long as the polymer volume is accessible, gels can easily be hardened using light illumination. However, in clinics, especially for minimally invasive surgery, it becomes highly challenging to control photopolymerization. The ratios between polymerizationvolume and radiating-surface-area are several orders of magnitude higher than for ex-vivo settings. Also tissue scattering occurs and influences the reaction. We developed a Monte Carlo model for photopolymerization, which takes into account the solid/liquid phase changes, moving solid/liquid-boundaries and refraction on these boundaries as well as tissue scattering in arbitrarily designable tissue cavities. The model provides a tool to tailor both the light probe and the scattering/absorption properties of the photopolymer for applications such as medical implants or tissue replacements. Based on the simulations, we have previously shown that by adding scattering additives to the liquid monomer, the photopolymerized volume was considerably increased. In this study, we have used bovine intervertebral disc cavities, as a model for spinal degeneration, to study photopolymerization in-vitro. The cavity is created by enzyme digestion. Using a custom designed probe, hydrogels were injected and photopolymerized. Magnetic resonance imaging (MRI) and visual inspection tools were employed to investigate the successful photopolymerization outcomes. The results provide insights for the development of novel endoscopic light-scattering polymerization probes paving the way for a new generation of implantable hydrogels.

Development and utilization of new diagnostics for dense-phase pneumatic transport

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

Louge, M.Y.; Jenkins, J.T.

Dense-phase pneumatic transport is an attractive means of conveying solids. Unfortunately, because of the high solid concentrations, this transport method is a difficult regime in which to carry out detailed measurements. Hence most details of the flow are unknown. In this context, the main objective of this work is to develop probes for local measurements of solid velocity and holdup in dense gas-solid flows. In particular, the authors have designed capacitance probes to measure local, time-dependent particle concentrations, and a new optical fiber probe based on laser-induced-phosphorescence to measure particle velocities. The principles for the capacitance and optical diagnostics weremore » given in the first and second quarterly reports. A final version of the optical fiber probe was designed in the previous reporting period. Because granular flows depends strongly on the nature of their interaction with a boundary, the authors have sought in the present reporting period to verify the boundary conditions recently calculated by Jenkins (J. Appl. Mech., in press (1991)) using computer simulations. 2 refs., 2 figs.« less

Solid-state electrochemistry on the nanometer and atomic scales: the scanning probe microscopy approach

DOE PAGES

Strelcov, Evgheni; Yang, Sang Mo; Jesse, Stephen; ...

2016-04-21

Energy technologies of the 21st century require an understanding and precise control over ion transport and electrochemistry at all length scales – from single atoms to macroscopic devices. Our short review provides a summary of recent studies dedicated to methods of advanced scanning probe microscopy for probing electrochemical transformations in solids at the meso-, nano- and atomic scales. In this discussion we present the advantages and limitations of several techniques and a wealth of examples highlighting peculiarities of nanoscale electrochemistry.

Solid-state electrochemistry on the nanometer and atomic scales: the scanning probe microscopy approach

PubMed Central

Strelcov, Evgheni; Yang, Sang Mo; Jesse, Stephen; Balke, Nina; Vasudevan, Rama K.; Kalinin, Sergei V.

2016-01-01

Energy technologies of the 21st century require understanding and precise control over ion transport and electrochemistry at all length scales – from single atoms to macroscopic devices. This short review provides a summary of recent works dedicated to methods of advanced scanning probe microscopy for probing electrochemical transformations in solids at the meso-, nano- and atomic scales. Discussion presents advantages and limitations of several techniques and a wealth of examples highlighting peculiarities of nanoscale electrochemistry. PMID:27146961

In-situ surface science studies of the interaction between sulfur dioxide and two-dimensional palladium loaded-cerium/zirconium mixed metal oxide model catalysts

NASA Astrophysics Data System (ADS)

Romano, Esteban Javier

2005-07-01

Cerium and zirconium oxides are important materials in industrial catalysis. Particularly, the great advances attained in the past 30 years in controlling levels of gaseous pollutants released from internal combustion engines can be attributed to the development of catalysts employing these materials. Unfortunately, oxides of sulfur are known threats to the longevity of many catalytic systems by irreversibly interacting with catalytic materials. In this work, polycrystalline cerium-zirconium mixed-metal-oxide (MMO) solid solutions were synthesized. High resolution x-ray photoelectron spectroscopy (XPS) spectral data was collected and examined for revelation of the surface species that form on these metal oxides after in-situ exposures to sulfur dioxide. The model catalysts were exposed to sulfur dioxide using a custom modified in-situ reaction cell and platen heater. The results of this study demonstrate the formation of sulfate and sulfite surface sulfur species. Temperature and compositional dependencies were displayed, with higher temperatures and ceria molar ratios displaying a larger propensity for forming surface sulfur species. In addition to analysis of sulfur photoemission, the photoemission regions of oxygen, zirconium, and cerium were examined for the materials used in this study before and after the aforementioned treatments with sulfur dioxide. The presence of surface hydroxyl groups was observed and metal oxidation state changes were probed to further enhance the understanding of sulfur dioxide adsorption on the synthesized materials. Palladium loaded mixed-metal oxides were synthesized using a unique solid-state methodology to probe the effect of palladium addition on sulfur dioxide adsorption. The addition of palladium to this model system is shown to have a strong effect on the magnitude of adsorption for sulfur dioxide on some material/exposure condition combinations. Ceria/zirconia sulfite and sulfate species are identified on the palladium-loaded MMO materials with adsorption sites located on the exposed oxide sites.

In Situ Potentiodynamic Analysis of the Electrolyte/Silicon Electrodes Interface Reactions - A Sum Frequency Generation Vibrational Spectroscopy Study

DOE PAGES

Horowitz, Yonatan; Han, Hui-Ling; Ross, Philip N.; ...

2015-12-11

The key factor in long-term use of batteries is the formation of an electrically insulating solid layer that allows lithium ion transport but stops further electrolyte redox reactions on the electrode surface, hence solid electrolyte interphase (SEI). In this paper, we have studied a common electrolyte, 1.0 M LiPF 6/ethylene carbonate (EC)/diethyl carbonate (DEC), reduction products on crystalline silicon (Si) electrodes in a lithium (Li) half-cell system under reaction conditions. We employed in situ sum frequency generation vibrational spectroscopy (SFG-VS) with interface sensitivity in order to probe the molecular composition of the SEI surface species under various applied potentials wheremore » electrolyte reduction is expected. We found that, with a Si(100)-hydrogen terminated wafer, a Si-ethoxy (Si-OC 2H 5) surface intermediate forms due to DEC decomposition. Our results suggest that the SEI surface composition varies depending on the termination of Si surface, i.e., the acidity of the Si surface. We provide the evidence of specific chemical composition of the SEI on the anode surface under reaction conditions. This supports an electrochemical electrolyte reduction mechanism in which the reduction of the DEC molecule to an ethoxy moiety plays a key role. Finally, these findings shed new light on the formation mechanism of SEI on Si anodes in particular and on SEI formation in general.« less

Probe Heating Method for the Analysis of Solid Samples Using a Portable Mass Spectrometer

PubMed Central

Kumano, Shun; Sugiyama, Masuyuki; Yamada, Masuyoshi; Nishimura, Kazushige; Hasegawa, Hideki; Morokuma, Hidetoshi; Inoue, Hiroyuki; Hashimoto, Yuichiro

2015-01-01

We previously reported on the development of a portable mass spectrometer for the onsite screening of illicit drugs, but our previous sampling system could only be used for liquid samples. In this study, we report on an attempt to develop a probe heating method that also permits solid samples to be analyzed using a portable mass spectrometer. An aluminum rod is used as the sampling probe. The powdered sample is affixed to the sampling probe or a droplet of sample solution is placed on the tip of the probe and dried. The probe is then placed on a heater to vaporize the sample. The vapor is then introduced into the portable mass spectrometer and analyzed. With the heater temperature set to 130°C, the developed system detected 1 ng of methamphetamine, 1 ng of amphetamine, 3 ng of 3,4-methylenedioxymethamphetamine, 1 ng of 3,4-methylenedioxyamphetamine, and 0.3 ng of cocaine. Even from mixtures consisting of clove powder and methamphetamine powder, methamphetamine ions were detected by tandem mass spectrometry. The developed probe heating method provides a simple method for the analysis of solid samples. A portable mass spectrometer incorporating this method would thus be useful for the onsite screening of illicit drugs. PMID:26819909

A LOW-E MAGIC ANGLE SPINNING PROBE FOR BIOLOGICAL SOLID STATE NMR AT 750 MHz

PubMed Central

McNeill, Seth A.; Gor’kov, Peter L.; Shetty, Kiran; Brey, William W.; Long, Joanna R.

2009-01-01

Crossed-coil NMR probes are a useful tool for reducing sample heating for biological solid state NMR. In a crossed-coil probe, the higher frequency 1H field, which is the primary source of sample heating in conventional probes, is produced by a separate low-inductance resonator. Because a smaller driving voltage is required, the electric field across the sample and the resultant heating is reduced. In this work we describe the development of a magic angle spinning (MAS) solid state NMR probe utilizing a dual resonator. This dual resonator approach, referred to as “Low-E,” was originally developed to reduce heating in samples of mechanically aligned membranes. The study of inherently dilute systems, such as proteins in lipid bilayers, via MAS techniques requires large sample volumes at high field to obtain spectra with adequate signal-to-noise ratio under physiologically relevant conditions. With the Low-E approach, we are able to obtain homogeneous and sufficiently strong radiofrequency fields for both 1H and 13C frequencies in a 4 mm probe with a 1H frequency of 750 MHz. The performance of the probe using windowless dipolar recoupling sequences is demonstrated on model compounds as well as membrane embedded peptides. PMID:19138870

Optical fingerprints of solid-liquid interfaces: a joint ATR-IR and first principles investigation

NASA Astrophysics Data System (ADS)

Yang, L.; Niu, F.; Tecklenburg, S.; Pander, M.; Nayak, S.; Erbe, A.; Wippermann, S.; Gygi, F.; Galli, G.

Despite the importance of understanding the structural and bonding properties of solid-liquid interfaces for a wide range of (photo-)electrochemical applications, there are presently no experimental techniques available to directly probe the microscopic structure of solid-liquid interfaces. To develop robust strategies to interpret experiments and validate theory, we carried out attenuated total internal reflection (ATR-IR) spectroscopy measurements and ab initio molecular dynamics (AIMD) simulations of the vibrational properties of interfaces between liquid water and well-controlled prototypical semiconductor substrates. We show the Ge(100)/H2O interface to feature a reversible potential-dependent surface phase transition between Ge-H and Ge-OH termination. The Si(100)/H2O interface is proposed as a model system for corrosion and oxidation processes. We performed AIMD calculations under finite electric fields, revealing different pathways for initial oxidation. These pathways are predicted to exhibit unique spectral signatures. A significant increase in surface specificity can be achieved utilizing an angle-dependent ATR-IR experiment, which allows to detect such signatures at the interfacial layer and consequently changes in the hydrogen bond network. Funding from DOE-BES Grant No. DE-SS0008939 and the Deutsche Forschungsgemeinschaft (RESOLV, EXC 1069) are gratefully acknowledged.

Self-consistent modeling of electrochemical strain microscopy of solid electrolytes

DOE PAGES

Tselev, Alexander; Morozovska, Anna N.; Udod, Alexei; ...

2014-10-10

Electrochemical strain microscopy (ESM) employs a strong electromechanical coupling in solid ionic conductors to map ionic transport and electrochemical processes with nanometer-scale spatial resolution. To elucidate the mechanisms of the ESM image formation, we performed self-consistent numerical modeling of the electromechanical response in solid electrolytes under the probe tip in a linear, small-signal regime using the Boltzmann–Planck–Nernst–Einstein theory and Vegard's law while taking account of the electromigration and diffusion. We identified the characteristic time scales involved in the formation of the ESM response and found that the dynamics of the charge carriers in the tip-electrolyte system with blocking interfaces canmore » be described as charging of the diffuse layer at the tip-electrolyte interface through the tip contact spreading resistance. At the high frequencies used in the detection regime, the distribution of the charge carriers under the tip is governed by evanescent concentration waves generated at the tip-electrolyte interface. The ion drift length in the electric field produced by the tip determines the ESM response at high frequencies, which follows a 1/f asymptotic law. The electronic conductivity, as well as the electron transport through the electrode-electrolyte interface, do not have a significant effect on the ESM signal in the detection regime. The results indicate, however, that for typical solid electrolytes at room temperature, the ESM response originates at and contains information about the very surface layer of a sample, and the properties of the one-unit-cell-thick surface layer may significantly contribute to the ESM response, implying a high surface sensitivity and a high lateral resolution of the technique. On the other hand, it follows that a rigorous analysis of the ESM signals requires techniques that account for the discrete nature of a solid.« less

AFM probing in aqueous environment of Staphylococcus epidermidis cells naturally immobilised on glass: physico-chemistry behind the successful immobilisation.

PubMed

Méndez-Vilas, A; Gallardo-Moreno, A M; Calzado-Montero, R; González-Martín, M L

2008-05-01

AFM probing of microbial cells in liquid environments usually requires them to be physically or chemically attached to a solid surface. The fixation mechanisms may influence the nanomechanical characterization done by force curve mapping using an AFM. To study the response of a microbial cell surface to this kind of local measurement this study attempts to overcome the problem associated to the uncertainties introduced by the different fixation treatments by analysing the surface of Staphylococcus epidermidis cells naturally (non-artificially mediated) immobilised on a glass support surface. The particularities of this natural bacterial fixation process for AFM surface analysis are discussed in terms of theoretical predictions of the XDLVO model applied to the systems bacteria/support substratum and bacteria/AFM tip immersed in water. In this sense, in the first part of this study the conditions for adequate natural fixation of three S. epidermidis strains have been analyzed by taking into account the geometries of the bacterium, substrate and tip. In the second part, bacteria are probed without the risk of any possible artefacts due to the mechanical or chemical fixation procedures. Forces measured over the successfully adhered cells have (directly) shown that the untreated bacterial surface suffers from a combination of both reversible and non-reversible deformations during acquisition of force curves all taken under the same operational conditions. This is revealed directly through high-resolution tapping-mode imaging of the bacterial surface immediately following force curve mapping. The results agree with the two different types of force curves that were repeatedly obtained. Interestingly, one type of these force curves suggests that the AFM tip is breaking (rather than pushing) the cell surface during acquisition of the force curve. In this case, adhesive peaks were always observed, suggesting a mechanical origin of the measured pull-off forces. The other type of force curves shows no adhesive peaks and exhibits juxtaposing of approaching and retraction curves, reflecting elastic deformations.

Efficient design of multituned transmission line NMR probes: the electrical engineering approach.

PubMed

Frydel, J A; Krzystyniak, M; Pienkowski, D; Pietrzak, M; de Sousa Amadeu, N; Ratajczyk, T; Idzik, K; Gutmann, T; Tietze, D; Voigt, S; Fenn, A; Limbach, H H; Buntkowsky, G

2011-01-01

Transmission line-based multi-channel solid state NMR probes have many advantages regarding the cost of construction, number of RF-channels, and achievable RF-power levels. Nevertheless, these probes are only rarely employed in solid state-NMR-labs, mainly owing to the difficult experimental determination of the necessary RF-parameters. Here, the efficient design of multi-channel solid state MAS-NMR probes employing transmission line theory and modern techniques of electrical engineering is presented. As technical realization a five-channel ((1)H, (31)P, (13)C, (2)H and (15)N) probe for operation at 7 Tesla is described. This very cost efficient design goal is a multi port single coil transmission line probe based on the design developed by Schaefer and McKay. The electrical performance of the probe is determined by measuring of Scattering matrix parameters (S-parameters) in particular input/output ports. These parameters are compared to the calculated parameters of the design employing the S-matrix formalism. It is shown that the S-matrix formalism provides an excellent tool for examination of transmission line probes and thus the tool for a rational design of these probes. On the other hand, the resulting design provides excellent electrical performance. From a point of view of Nuclear Magnetic Resonance (NMR), calibration spectra of particular ports (channels) are of great importance. The estimation of the π/2 pulses length for all five NMR channels is presented. Copyright © 2011 Elsevier Inc. All rights reserved.

Probing functional groups at the gas-aerosol interface using heterogeneous titration reactions: a tool for predicting aerosol health effects?

PubMed

Setyan, Ari; Sauvain, Jean-Jacques; Guillemin, Michel; Riediker, Michael; Demirdjian, Benjamin; Rossi, Michel J

2010-12-17

The complex chemical and physical nature of combustion and secondary organic aerosols (SOAs) in general precludes the complete characterization of both bulk and interfacial components. The bulk composition reveals the history of the growth process and therefore the source region, whereas the interface controls--to a large extent--the interaction with gases, biological membranes, and solid supports. We summarize the development of a soft interrogation technique, using heterogeneous chemistry, for the interfacial functional groups of selected probe gases [N(CH(3))(3), NH(2)OH, CF(3)COOH, HCl, O(3), NO(2)] of different reactivity. The technique reveals the identity and density of surface functional groups. Examples include acidic and basic sites, olefinic and polycyclic aromatic hydrocarbon (PAH) sites, and partially and completely oxidized surface sites. We report on the surface composition and oxidation states of laboratory-generated aerosols and of aerosols sampled in several bus depots. In the latter case, the biomarker 8-hydroxy-2'-deoxyguanosine, signaling oxidative stress caused by aerosol exposure, was isolated. The increase in biomarker levels over a working day is correlated with the surface density N(i)(O3) of olefinic and/or PAH sites obtained from O(3) uptakes as well as with the initial uptake coefficient, γ(0), of five probe gases used in the field. This correlation with γ(0) suggests the idea of competing pathways occurring at the interface of the aerosol particles between the generation of reactive oxygen species (ROS) responsible for oxidative stress and cellular antioxidants.

Accurate description of charged excitations in molecular solids from embedded many-body perturbation theory

NASA Astrophysics Data System (ADS)

Li, Jing; D'Avino, Gabriele; Duchemin, Ivan; Beljonne, David; Blase, Xavier

2018-01-01

We present a novel hybrid quantum/classical approach to the calculation of charged excitations in molecular solids based on the many-body Green's function G W formalism. Molecules described at the G W level are embedded into the crystalline environment modeled with an accurate classical polarizable scheme. This allows the calculation of electron addition and removal energies in the bulk and at crystal surfaces where charged excitations are probed in photoelectron experiments. By considering the paradigmatic case of pentacene and perfluoropentacene crystals, we discuss the different contributions from intermolecular interactions to electronic energy levels, distinguishing between polarization, which is accounted for combining quantum and classical polarizabilities, and crystal field effects, that can impact energy levels by up to ±0.6 eV. After introducing band dispersion, we achieve quantitative agreement (within 0.2 eV) on the ionization potential and electron affinity measured at pentacene and perfluoropentacene crystal surfaces characterized by standing molecules.

Characterisation of a fibre optic Raman probe within a hypodermic needle.

PubMed

Iping Petterson, Ingeborg E; Day, John C C; Fullwood, Leanne M; Gardner, Benjamin; Stone, Nick

2015-11-01

We demonstrate the first use of a multifibre Raman probe that fits inside the bore of a hypodermic needle. A Raman probe containing multiple collection fibres provides improved signal collection efficiency in biological samples compared with a previous two-fibre design. Furthermore, probe performance (signal-to-noise ratios) compared favourably with the performance achieved in previous Raman microscope experiments able to distinguish between benign lymph nodes, primary malignancies in lymph nodes and secondary malignancies in lymph nodes. The experimental measurements presented here give an indication of the sampling volume of the Raman needle probe in lymphoid tissues. Liquid tissue phantoms were used that contained scattering medium encompassing a range of scattering properties similar to those of a variety of tissue types, including lymph node tissues. To validate the appropriateness of the phantoms, the sampling depth of the probe was also measured in excised lymph node tissue. More than 50 % of Raman photons collected were found to originate from between the tip of the needle and a depth of 500 μm into the tissue. The needle probe presented here achieves spectral quality comparable to that in numerous studies previously demonstrating Raman disease discrimination. It is expected that this approach could achieve targeted subcutaneous tissue measurements and be viable for use for the in vivo Raman diagnostics of solid organs located within a few centimetres below the skin's surface. Graphical Abstract Schematic of multi-fibre Raman needle probe with disposible tips and proximal optical filtration.

Detection and isolation of nucleic acid sequences using competitive hybridization probes

DOEpatents

Lucas, Joe N.; Straume, Tore; Bogen, Kenneth T.

1997-01-01

A method for detecting a target nucleic acid sequence in a sample is provided using hybridization probes which competitively hybridize to a target nucleic acid. According to the method, a target nucleic acid sequence is hybridized to first and second hybridization probes which are complementary to overlapping portions of the target nucleic acid sequence, the first hybridization probe including a first complexing agent capable of forming a binding pair with a second complexing agent and the second hybridization probe including a detectable marker. The first complexing agent attached to the first hybridization probe is contacted with a second complexing agent, the second complexing agent being attached to a solid support such that when the first and second complexing agents are attached, target nucleic acid sequences hybridized to the first hybridization probe become immobilized on to the solid support. The immobilized target nucleic acids are then separated and detected by detecting the detectable marker attached to the second hybridization probe. A kit for performing the method is also provided.

Detection and isolation of nucleic acid sequences using competitive hybridization probes

DOEpatents

Lucas, J.N.; Straume, T.; Bogen, K.T.

1997-04-01

A method for detecting a target nucleic acid sequence in a sample is provided using hybridization probes which competitively hybridize to a target nucleic acid. According to the method, a target nucleic acid sequence is hybridized to first and second hybridization probes which are complementary to overlapping portions of the target nucleic acid sequence, the first hybridization probe including a first complexing agent capable of forming a binding pair with a second complexing agent and the second hybridization probe including a detectable marker. The first complexing agent attached to the first hybridization probe is contacted with a second complexing agent, the second complexing agent being attached to a solid support such that when the first and second complexing agents are attached, target nucleic acid sequences hybridized to the first hybridization probe become immobilized on to the solid support. The immobilized target nucleic acids are then separated and detected by detecting the detectable marker attached to the second hybridization probe. A kit for performing the method is also provided. 7 figs.

Molecular Velcro constructed from polymer loop brushes showing enhanced adhesion force

NASA Astrophysics Data System (ADS)

Zhou, Tian; Han, Biao; Han, Lin; Li, Christopher; Department of Materials Science; Engineering Team; School of Biomedical Engineering, Science; Health Systems Team

2015-03-01

Molecular Velcro is commonly seen in biological systems as the formation of strong physical entanglement at molecular scale could induce strong adhesion, which is crucial to many biological processes. To mimic this structure, we designed, and fabricated polymer loop brushes using polymer single crystals with desired surface functionality and controlled chain folding. Compared with reported loop brushes fabricated using triblock copolymers, the present loop bushes have precise loop sizes, loop grafting density, and well controlled tethering locations on the solid surface. Atomic force microscopy-based force spectroscopy measurements using a polymer chain coated probe reveal that the adhesion force are significantly enhanced on the loop brush surface as compared with its single-strand counterpart. This study directly shows the effect of polymer brush conformation on their properties, and suggests a promising strategy for advanced polymer surface design.

An active one-particle microrheometer: incorporating magnetic tweezers to total internal reflection microscopy.

PubMed

Gong, Xiangjun; Hua, Li; Wu, Chi; Ngai, To

2013-03-01

We present a novel microrheometer by incorporating magnetic tweezers in the total internal reflection microscopy (TIRM) that enables measuring of viscoelastic properties of materials near solid surface. An evanescent wave generated by a solid∕liquid interface in the TIRM is used as the incident light source in the microrheometer. When a probe particle (of a few micrometers diameter) moves near the interface, it can interact with the evanescent field and reflect its position with respect to the interface by the scattered light intensity. The exponential distance dependence of the evanescent field, on the one hand, makes this technique extremely sensitive to small changes from z-fluctuations of the probe (with a resolution of several nanometers), and on the other, it does not require imaging of the probe with high lateral resolution. Another distinct advantage is the high sensitivity in determining the z position of the probe in the absence of any labeling. The incorporated magnetic tweezers enable us to effectively manipulate the distance of the embedded particle from the interface either by a constant or an oscillatory force. The force ramp is easy to implement through a coil current ramp. In this way, the local viscous and elastic properties of a given system under different confinements can therefore be measured by resolving the near-surface particle motion. To test the feasibility of applying this microrheology to soft materials, we measured the viscoelastic properties of sucrose and poly(ethylene glycol) solutions and compared the results to bulk rheometry. In addition, we applied this technique in monitoring the structure and properties of deformable microgel particles near the flat surface.

Solid-phase single molecule biosensing using dual-color colocalization of fluorescent quantum dot nanoprobes

NASA Astrophysics Data System (ADS)

Liu, Jianbo; Yang, Xiaohai; Wang, Kemin; Wang, Qing; Liu, Wei; Wang, Dong

2013-10-01

The development of solid-phase surface-based single molecule imaging technology has attracted significant interest during the past decades. Here we demonstrate a sandwich hybridization method for highly sensitive detection of a single thrombin protein at a solid-phase surface based on the use of dual-color colocalization of fluorescent quantum dot (QD) nanoprobes. Green QD560-modified thrombin binding aptamer I (QD560-TBA I) were deposited on a positive poly(l-lysine) assembled layer, followed by bovine serum albumin blocking. It allowed the thrombin protein to mediate the binding of the easily detectable red QD650-modified thrombin binding aptamer II (QD650-TBA II) to the QD560-TBA I substrate. Thus, the presence of the target thrombin can be determined based on fluorescent colocalization measurements of the nanoassemblies, without target amplification or probe separation. The detection limit of this assay reached 0.8 pM. This fluorescent colocalization assay has enabled single molecule recognition in a separation-free detection format, and can serve as a sensitive biosensing platform that greatly suppresses the nonspecific adsorption false-positive signal. This method can be extended to other areas such as multiplexed immunoassay, single cell analysis, and real time biomolecule interaction studies.The development of solid-phase surface-based single molecule imaging technology has attracted significant interest during the past decades. Here we demonstrate a sandwich hybridization method for highly sensitive detection of a single thrombin protein at a solid-phase surface based on the use of dual-color colocalization of fluorescent quantum dot (QD) nanoprobes. Green QD560-modified thrombin binding aptamer I (QD560-TBA I) were deposited on a positive poly(l-lysine) assembled layer, followed by bovine serum albumin blocking. It allowed the thrombin protein to mediate the binding of the easily detectable red QD650-modified thrombin binding aptamer II (QD650-TBA II) to the QD560-TBA I substrate. Thus, the presence of the target thrombin can be determined based on fluorescent colocalization measurements of the nanoassemblies, without target amplification or probe separation. The detection limit of this assay reached 0.8 pM. This fluorescent colocalization assay has enabled single molecule recognition in a separation-free detection format, and can serve as a sensitive biosensing platform that greatly suppresses the nonspecific adsorption false-positive signal. This method can be extended to other areas such as multiplexed immunoassay, single cell analysis, and real time biomolecule interaction studies. Electronic supplementary information (ESI) available: Absorbance and fluorescence spectra of quantum dot nanoprobes, electrophoresis analysis, and experimental setup for fluorescence imaging with dual channels. See DOI: 10.1039/c3nr03291d

Laser Driven Compression Equations of State and Hugoniot Pressure Measurements in Thick Solid Metallic Targets at ˜0.17-13 TW/cm2

NASA Astrophysics Data System (ADS)

Remo, John L.

2010-10-01

An electro-optic laser probe was developed to obtain parameters for high energy density equations of state (EoS), Hugoniot pressures (PH), and strain rates for high energy density laser irradiation intensity, I, experiments at ˜170 GW/cm2 (λ = 1064 nm) to ˜13 TW/cm2 (λ = 527 nm) on Al, Cu, Ti, Fe, Ni metal targets in a vacuum. At I ˜7 TW/cm2 front surface plasma pressures and temperatures reached 100's GPa and over two million K. Rear surface PH ranged from 7-120 GPa at average shock wave transit velocities 4.2-8.5 km/s, depending on target thickness and I. A surface plasma compression ˜100's GPa generated an impulsive radial expanding shock wave causing compression, rarefactions, and surface elastic and plastic deformations depending on I. A laser/fiber optic system measured rear surface shock wave emergence and particle velocity with ˜3 GHz resolution by monitoring light deflection from diamond polished rear surfaces of malleable metallic targets, analogous to an atomic force microscope. Target thickness, ˜0.5-2.9 mm, prevented front surface laser irradiation penetration, due to low radiation skin depth, from altering rear surface reflectivity (refractive index). At ˜10 TW electromagnetic plasma pulse noise generated from the target chamber overwhelmed detector signals. Pulse frequency analysis using Moebius loop antennae probed transient noise characteristics. Average shock (compression) and particle (rear surface displacement) velocity measurements determined rear surface PH and GPa) EoS that are compared with gas guns.

MICRO- AND NANOSCALE MEASUREMENT METHODS FOR PHASE CHANGE HEAT TRANSFER ON PLANAR AND STRUCTURED SURFACES

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

Buongiorno, J; Cahill, DG; Hidrovo, CH

2014-07-23

In this opinion piece, we discuss recent advances in experimental methods for characterizing phase change heat transfer. We begin with a survey of techniques for high-resolution measurements of temperature and heat flux at the solid surface and in the working fluid. Next, we focus on diagnostic tools for boiling heat transfer and describe techniques for visualizing the temperature and velocity fields, as well as measurements at the single bubble level. Finally, we discuss techniques to probe the kinetics of vapor formation within a few molecular layers of the interface. We conclude with our outlook for future progress in experimental methodsmore » for phase change heat transfer.« less

And There Was Light: Prospects for the Creation of Micro- and Nanostructures through Maskless Photolithography.

PubMed

Rühe, J

2017-09-26

In photolithographic processes, the light inducing the photochemical reactions is confined to a small volume, which enables direct writing of micro- and nanoscale features onto solid surfaces without the need of a predefined photomask. The direct writing process can be used to generate topographic patterns through photopolymerization or photo-cross-linking or can be employed to use light to generate chemical patterns on the surface with high spatial control, which would make such processes attractive for bioapplications. The prospects of maskless photolithography technologies with a focus on two-photon lithography and scanning-probe-based photochemical processes based on scanning near-field optical microscopy or beam pen lithography are discussed.

A colorimetric turn-on optical chemosensor for Cu2+ ions and its application as solid state sensor

NASA Astrophysics Data System (ADS)

Pannipara, Mehboobali; Al-Sehemi, Abdullah G.; Assiri, Mohammed; Kalam, Abul

2018-05-01

We report a novel coumarin based optical chemosensor (Probe 1) for the selective and sensitive detection of Cu2+ ions in aqueous medium. The addition of Cu2+ ions to Probe 1 shows distinct color change from light yellow to pinkish red color under visible light with the sensing limit of 1.54 μM. Moreover, practical utility of Probe 1 as solid state optical sensor (test paper, TLC plates) for sensing Cu2+ has been demonstrated by instantaneous "naked eye" response.

Computer Simulation of the Forces Acting on a Submerged Polystyrene Probe as it Approaches the Succinonitrile Melt-Solid Interface

NASA Technical Reports Server (NTRS)

Bune, Andris V.; Kaukler, William; Whitaker, Ann (Technical Monitor)

2001-01-01

A Modeling approach to simulate both mesoscale and microscopic forces acting in a typical AFM experiment is presented. A mesoscale level interaction between the cantilever tip and the sample surface is primarily described by the balance of attractive Van der Waals and repulsive forces. Ultimately, the goal is to measure the forces between a particle and the crystal-melt interface. Two modes of AFM operation are considered in this paper - a stationary and a "tapping" one. The continuous mechanics approach to model tip-surface interaction is presented. At microscopic levels, tip contamination and details of tip-surface interaction are modeled using a molecular dynamics approach for the case of polystyrene - succinonitrile contact. Integration of the mesoscale model with a molecular dynamic model is discussed.

Predicting Organic Cation Sorption Coefficients: Accounting for Competition from Sorbed Inorganic Cations Using a Simple Probe Molecule.

PubMed

Jolin, William C; Goyetche, Reaha; Carter, Katherine; Medina, John; Vasudevan, Dharni; MacKay, Allison A

2017-06-06

With the increasing number of emerging contaminants that are cationic at environmentally relevant pH values, there is a need for robust predictive models of organic cation sorption coefficients (K d ). Current predictive models fail to account for the differences in the identity, abundance, and affinity of surface-associated inorganic exchange ions naturally present at negatively charged receptor sites on environmental solids. To better understand how organic cation sorption is influenced by surface-associated inorganic exchange ions, sorption coefficients of 10 organic cations (including eight pharmaceuticals and two simple probe organic amines) were determined for six homoionic forms of the aluminosilicate mineral, montmorillonite. Organic cation sorption coefficients exhibited consistent trends for all compounds across the various homoionic clays with sorption coefficients (K d ) decreasing as follows: K d Na + > K d NH 4 + ≥ K d K + > K d Ca 2+ ≥ K d Mg 2+ > K d Al 3+ . This trend for competition between organic cations and exchangeable inorganic cations is consistent with the inorganic cation selectivity sequence, determined for exchange between inorganic ions. Such consistent trends in competition between organic and inorganic cations suggested that a simple probe cation, such as phenyltrimethylammonium or benzylamine, could capture soil-to-soil variations in native inorganic cation identity and abundance for the prediction of organic cation sorption to soils and soil minerals. Indeed, sorption of two pharmaceutical compounds to 30 soils was better described by phenyltrimethylammonium sorption than by measures of benzylamine sorption, effective cation exchange capacity alone, or a model from the literature (Droge, S., and Goss, K. Environ. Sci. Technol. 2013, 47, 14224). A hybrid approach integrating structural scaling factors derived from this literature model of organic cation sorption, along with phenyltrimethylammonium K d values, allowed for estimation of K d values for more structurally complex organic cations to homoionic montmorillonites and to heteroionic soils (mean absolute error of 0.27 log unit). Accordingly, we concluded that the use of phenyltrimethylammonium as a probe compound was a promising means to account for the identity, affinity, and abundance of natural exchange ions in the prediction of organic cation sorption coefficients for environmental solids.

Development of Active DNA Control Technique for DNA Sequencer With a Solid-state Nanopore

NASA Astrophysics Data System (ADS)

Akahori, Rena; Harada, Kunio; Goto, Yusuke; Yanagi, Itaru; Yokoi, Takahide; Oura, Takeshi; Shibahara, Masashi; Takeda, Ken-Ichi

We have developed a technique that can control the arbitrary speeds of DNA passing through a solid-state nanopore of a DNA sequencer. For this active DNA control technique, we used a DNA-immobilized Si probe, larger than the membrane with a nanopore, and used a piezoelectric actuator and stepper motor to drive the probe. This probe enables a user to adjust the relative position between the nanopore and DNA immobilized on the probe without the need for precise lateral control. In this presentation, we demonstrate how DNA (block copolymer ([(dT)25-(dC)25-(dA)50]m)), immobilized on the probe, slid through a nanopore and was pulled out using the active DNA control technique. As the DNA-immobilized probe was being pulled out, we obtained various ion-current signal levels corresponding to the number of different nucleotides in a single strand of DNA.

Solid phase sequencing of biopolymers

DOEpatents

Cantor, Charles; Koster, Hubert

2010-09-28

This invention relates to methods for detecting and sequencing target nucleic acid sequences, to mass modified nucleic acid probes and arrays of probes useful in these methods, and to kits and systems which contain these probes. Useful methods involve hybridizing the nucleic acids or nucleic acids which represent complementary or homologous sequences of the target to an array of nucleic acid probes. These probes comprise a single-stranded portion, an optional double-stranded portion and a variable sequence within the single-stranded portion. The molecular weights of the hybridized nucleic acids of the set can be determined by mass spectroscopy, and the sequence of the target determined from the molecular weights of the fragments. Nucleic acids whose sequences can be determined include DNA or RNA in biological samples such as patient biopsies and environmental samples. Probes may be fixed to a solid support such as a hybridization chip to facilitate automated molecular weight analysis and identification of the target sequence.

In situ analysis of capacity fade in thin-film anodes for high performance Li-ion all-solid-state batteries

NASA Astrophysics Data System (ADS)

Leite, Marina S.; Gong, Chen; Ruzmetov, Dmitry; Talin, A. Alec

There is still a pressing need to understand how the solid-interfaces in Li-ion all-solid-batteries form, including their chemical composition and electrical characteristics. In order to resolve the origin of the degradation mechanism in Al anodes, we combine in situ scanning electron microscopy in ultra-high vacuum with electrochemical cycling, in addition to ex situ characterization of the morphological, chemical, and electrical changes of the Al anodes upon lithiation. An AlLi alloy capped by a stable Al-Li-O is formed on the top surface of the anode, trapping Li, which results in the capacity fade, from 48.0 to 41.5 μ.Ah/cm2 in two cycles. The addition of a Cu capping layer is insufficient to prevent the device degradation because of the fast Li diffusion within Al. Yet, Si present extremely stable cycling: >92% of capacity retention after 100 cycles, with average Coulombic efficiency of 98%. Our in situ measurements represent a new platform for probing the real-time degradation of electrodes in all-solid-state batteries for energy storage devices.

High-yield synthesis of vaterite microparticles in gypsum suspension system via ultrasonic probe vibration/magnetic stirring

NASA Astrophysics Data System (ADS)

Wang, Bo; Pan, Zihe; Cheng, Huaigang; Chen, Zuliang; Cheng, Fangqin

2018-06-01

Vaterite-type calcium carbonate particles have some unique properties such as high hydrophilicity, large surface areas, and hierarchical structures consisting of primary vaterite particles in comparison with calcite or aragonite-type polymorphs. In this paper, gypsum (CaSO4·2H2O) suspension is used to synthesize micro-sized vaterite CaCO3 through magnetic stirring (MS) and ultrasonic probe vibration (UPV) methods. The effects of ammonia concentration, CO2 flow rate, solid-liquid ratio on the gypsum carbonation process, mineral phase composition, morphology and particle size distribution of CaCO3 are investigated. The results show that the carbonation process is significantly influenced by ammonia concentration, CO2 flow rate and ultrasound. Comparing with magnetic stirring, ultrasonic probe vibration take less time to reach the complete carbonate reaction. Gypsum is transformed to vaterite with the conversion rate about ∼95% when the mole ratio of NH4+/Ca2+ is 2.4 otherwise the carbonation reaction was uncompleted with gypsum residues left. Comparing with MS method, the UPV method resulted in smaller size and narrower size distribution of as-prepared microparticles and approximately 80% reduction of the particle size was achieved. It is established that increasing the solid-liquid ratio resulted in larger particle size in MS system and smaller particle size in UPV system. Increasing CO2 flow rate caused the particle size decreased in MS system and increased in UPV system.

High-resolution measurements of the spatial and temporal evolution of megagauss magnetic fields created in intense short-pulse laser-plasma interactions

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

Chatterjee, Gourab, E-mail: gourab@tifr.res.in; Singh, Prashant Kumar; Adak, Amitava

A pump-probe polarimetric technique is demonstrated, which provides a complete, temporally and spatially resolved mapping of the megagauss magnetic fields generated in intense short-pulse laser-plasma interactions. A normally incident time-delayed probe pulse reflected from its critical surface undergoes a change in its ellipticity according to the magneto-optic Cotton-Mouton effect due to the azimuthal nature of the ambient self-generated megagauss magnetic fields. The temporal resolution of the magnetic field mapping is typically of the order of the pulsewidth, limited by the laser intensity contrast, whereas a spatial resolution of a few μm is achieved by this optical technique. High-harmonics of themore » probe can be employed to penetrate deeper into the plasma to even near-solid densities. The spatial and temporal evolution of the megagauss magnetic fields at the target front as well as at the target rear are presented. The μm-scale resolution of the magnetic field mapping provides valuable information on the filamentary instabilities at the target front, whereas probing the target rear mirrors the highly complex fast electron transport in intense laser-plasma interactions.« less

Probing of exopolysaccharides with green fluorescence protein-labeled carbohydrate-binding module in Escherichia coli biofilms and flocs induced by bcsB overexpression.

PubMed

Nguyen, Minh Hong; Ojima, Yoshihiro; Sakka, Makiko; Sakka, Kazuo; Taya, Masahito

2014-10-01

Polysaccharides are major structural constituents to develop the three-dimensional architecture of Escherichia coli biofilms. In this study, confocal laser scanning microscopy was applied in combination with a fluorescent probe to analyze the location and arrangement of exopolysaccharide (EPSh) in microcolonies of E. coli K-12 derived strains, formed as biofilms on solid surfaces and flocs in the liquid phase. For this purpose, a novel fluorescent probe was constructed by conjugating a carbohydrate-binding module 3, from Paenibacillus curdlanolyticus, with the green fluorescence protein (GFP-CBM3). The GFP-CBM3 fused protein exhibited strong affinity to microcrystalline cellulose. Moreover, GFP-CBM3 specifically bound to cell-dense microcolonies in the E. coli biofilms, and to their flocs induced by bcsB overexpression. Therefore, the fused protein presents as a novel marker for EPSh produced by E. coli cells. Overexpression of bcsB was associated with abundant EPSh production and enhanced E. coli biofilm formation, which was similarly detectable by GFP-CBM3 probing. Copyright © 2014 The Society for Biotechnology, Japan. Published by Elsevier B.V. All rights reserved.

Interfacial friction and adhesion of cross-linked polymer thin films swollen with linear chains.

PubMed

Zhang, Qing; Archer, Lynden A

2007-07-03

The preparation and interfacial properties of a new type of tethered, thin-film lubricant coating are presented. These coatings are composed of three components: a dense self-assembled monolayer (SAM) underlayer that presents reactive vinyl groups at its surface; a cross-linked polydimethylsiloxane (PDMS) overlayer that is covalently tethered to the SAM; and free, mobile linear PDMS chains dispersed in the network. We investigate the influence of the molecular weight (Ms) and concentration of the free PDMS chains on the structure and equilibrium swelling properties of the cross-linked films. Using a bead-probe lateral force microscopy measurement technique, we also quantify the interfacial friction and adhesion characteristics of surfaces functionalized with these coatings. We find that both the volume fraction and the molecular weight of free PDMS molecules in the coatings influence their interfacial friction and adhesion properties. For example, the addition of short PDMS chains in dry, cross-linked PDMS thin films yields tethered surface coatings with ultralow friction coefficients (mu = 5.2 x 10(-3)). An analysis based on classical lubrication theory suggests that the reduction in friction force produced by free polymer is a consequence of the gradual separation of asperities on opposing surfaces and the consequent substitution of solid-solid friction by viscous drag of the free polymer chains in the network.

BIOPHYSICAL PROPERTIES OF NUCLEIC ACIDS AT SURFACES RELEVANT TO MICROARRAY PERFORMANCE.

PubMed

Rao, Archana N; Grainger, David W

2014-04-01

Both clinical and analytical metrics produced by microarray-based assay technology have recognized problems in reproducibility, reliability and analytical sensitivity. These issues are often attributed to poor understanding and control of nucleic acid behaviors and properties at solid-liquid interfaces. Nucleic acid hybridization, central to DNA and RNA microarray formats, depends on the properties and behaviors of single strand (ss) nucleic acids (e.g., probe oligomeric DNA) bound to surfaces. ssDNA's persistence length, radius of gyration, electrostatics, conformations on different surfaces and under various assay conditions, its chain flexibility and curvature, charging effects in ionic solutions, and fluorescent labeling all influence its physical chemistry and hybridization under assay conditions. Nucleic acid (e.g., both RNA and DNA) target interactions with immobilized ssDNA strands are highly impacted by these biophysical states. Furthermore, the kinetics, thermodynamics, and enthalpic and entropic contributions to DNA hybridization reflect global probe/target structures and interaction dynamics. Here we review several biophysical issues relevant to oligomeric nucleic acid molecular behaviors at surfaces and their influences on duplex formation that influence microarray assay performance. Correlation of biophysical aspects of single and double-stranded nucleic acids with their complexes in bulk solution is common. Such analysis at surfaces is not commonly reported, despite its importance to microarray assays. We seek to provide further insight into nucleic acid-surface challenges facing microarray diagnostic formats that have hindered their clinical adoption and compromise their research quality and value as genomics tools.

BIOPHYSICAL PROPERTIES OF NUCLEIC ACIDS AT SURFACES RELEVANT TO MICROARRAY PERFORMANCE

PubMed Central

Rao, Archana N.; Grainger, David W.

2014-01-01

Both clinical and analytical metrics produced by microarray-based assay technology have recognized problems in reproducibility, reliability and analytical sensitivity. These issues are often attributed to poor understanding and control of nucleic acid behaviors and properties at solid-liquid interfaces. Nucleic acid hybridization, central to DNA and RNA microarray formats, depends on the properties and behaviors of single strand (ss) nucleic acids (e.g., probe oligomeric DNA) bound to surfaces. ssDNA’s persistence length, radius of gyration, electrostatics, conformations on different surfaces and under various assay conditions, its chain flexibility and curvature, charging effects in ionic solutions, and fluorescent labeling all influence its physical chemistry and hybridization under assay conditions. Nucleic acid (e.g., both RNA and DNA) target interactions with immobilized ssDNA strands are highly impacted by these biophysical states. Furthermore, the kinetics, thermodynamics, and enthalpic and entropic contributions to DNA hybridization reflect global probe/target structures and interaction dynamics. Here we review several biophysical issues relevant to oligomeric nucleic acid molecular behaviors at surfaces and their influences on duplex formation that influence microarray assay performance. Correlation of biophysical aspects of single and double-stranded nucleic acids with their complexes in bulk solution is common. Such analysis at surfaces is not commonly reported, despite its importance to microarray assays. We seek to provide further insight into nucleic acid-surface challenges facing microarray diagnostic formats that have hindered their clinical adoption and compromise their research quality and value as genomics tools. PMID:24765522

Atmospheric electromagnetic pulse propagation effects from thick targets in a terawatt laser target chamber.

PubMed

Remo, John L; Adams, Richard G; Jones, Michael C

2007-08-20

Generation and effects of atmospherically propagated electromagnetic pulses (EMPs) initiated by photoelectrons ejected by the high density and temperature target surface plasmas from multiterawatt laser pulses are analyzed. These laser radiation pulse interactions can significantly increase noise levels, thereby obscuring data (sometimes totally) and may even damage sensitive probe and detection instrumentation. Noise effects from high energy density (approximately multiterawatt) laser pulses (approximately 300-400 ps pulse widths) interacting with thick approximately 1 mm) metallic and dielectric solid targets and dielectric-metallic powder mixtures are interpreted as transient resonance radiation associated with surface charge fluctuations on the target chamber that functions as a radiating antenna. Effective solutions that minimize atmospheric EMP effects on internal and proximate electronic and electro-optical equipment external to the system based on systematic measurements using Moebius loop antennas, interpretations of signal periodicities, and dissipation indicators determining transient noise origin characteristics from target emissions are described. Analytic models for the effect of target chamber resonances and associated noise current and temperature in a probe diode laser are described.

Atmospheric electromagnetic pulse propagation effects from thick targets in a terawatt laser target chamber

NASA Astrophysics Data System (ADS)

Remo, John L.; Adams, Richard G.; Jones, Michael C.

2007-08-01

Generation and effects of atmospherically propagated electromagnetic pulses (EMPs) initiated by photoelectrons ejected by the high density and temperature target surface plasmas from multiterawatt laser pulses are analyzed. These laser radiation pulse interactions can significantly increase noise levels, thereby obscuring data (sometimes totally) and may even damage sensitive probe and detection instrumentation. Noise effects from high energy density (approximately multiterawatt) laser pulses (˜300-400 ps pulse widths) interacting with thick (˜1 mm) metallic and dielectric solid targets and dielectric-metallic powder mixtures are interpreted as transient resonance radiation associated with surface charge fluctuations on the target chamber that functions as a radiating antenna. Effective solutions that minimize atmospheric EMP effects on internal and proximate electronic and electro-optical equipment external to the system based on systematic measurements using Moebius loop antennas, interpretations of signal periodicities, and dissipation indicators determining transient noise origin characteristics from target emissions are described. Analytic models for the effect of target chamber resonances and associated noise current and temperature in a probe diode laser are described.

Atmospheric electromagnetic pulse propagation effects from thick targets in a terawatt laser target chamber

DOE PAGES

Remo, John L.; Adams, Richard G.; Jones, Michael C.

2007-08-16

Generation and effects of atmospherically propagated electromagnetic pulses (EMPs) initiated by photoelectrons ejected by the high density and temperature target surface plasmas from multiterawatt laser pulses are analyzed. These laser radiation pulse interactions can significantly increase noise levels, thereby obscuring data (sometimes totally) and may even damage sensitive probe and detection instrumentation. Noise effects from high energy density (approximately multiterawatt) laser pulses (~300–400 ps pulse widths) interacting with thick (~1 mm) metallic and dielectric solid targets and dielectric–metallic powder mixtures are interpreted as transient resonance radiation associated with surface charge fluctuations on the target chamber that functions as a radiatingmore » antenna. Effective solutions that minimize atmospheric EMP effects on internal and proximate electronic and electro-optical equipment external to the system based on systematic measurements using Moebius loop antennas, interpretations of signal periodicities, and dissipation indicators determining transient noise origin characteristics from target emissions are described. Analytic models for the effect of target chamber resonances and associated noise current and temperature in a probe diode laser are described.« less

Measurement of contact-line dissipation in a nanometer-thin soap film

NASA Astrophysics Data System (ADS)

Guo, Shuo; Lee, Chun Huen; Sheng, Ping; Tong, Penger

2015-01-01

We report a direct measurement of the friction coefficient ξc of two fluctuating contact lines formed on a fiber surface when a long glass fiber intersects the two water-air interfaces of a thin soap film. The glass fiber of diameter d in the range of 0.4-4 μ m and length 100-300 μ m is glued onto the front end of a rectangular cantilever used for atomic force microscopy. As a sensitive mechanical resonator, the hanging fiber probe can accurately measure a minute change of its viscous damping caused by the soap film. By measuring the broadening of the resonant peak of the hanging fiber probe with varying viscosity η of the soap film and different surface treatments of the glass fiber, we confirm that the contact line dissipation obeys a universal scaling law, ξc=α π d η , where the coefficient α =1.1 ±0.3 is insensitive to the change of liquid-solid contact angle. The experimental result is in good agreement with the numerical result based on the phase field model under the generalized Navier boundary conditions.

Measurement of contact-line dissipation in a nanometer-thin soap film.

PubMed

Guo, Shuo; Lee, Chun Huen; Sheng, Ping; Tong, Penger

2015-01-01

We report a direct measurement of the friction coefficient ξ(c) of two fluctuating contact lines formed on a fiber surface when a long glass fiber intersects the two water-air interfaces of a thin soap film. The glass fiber of diameter d in the range of 0.4-4 μm and length 100-300 μm is glued onto the front end of a rectangular cantilever used for atomic force microscopy. As a sensitive mechanical resonator, the hanging fiber probe can accurately measure a minute change of its viscous damping caused by the soap film. By measuring the broadening of the resonant peak of the hanging fiber probe with varying viscosity η of the soap film and different surface treatments of the glass fiber, we confirm that the contact line dissipation obeys a universal scaling law, ξ(c)=απdη, where the coefficient α=1.1±0.3 is insensitive to the change of liquid-solid contact angle. The experimental result is in good agreement with the numerical result based on the phase field model under the generalized Navier boundary conditions.

CONFERENCE NOTE: European Optical Society, Topical Meeting Optical Metrology and Nanotechnology, Engelberg, Switzerland, 27 30 March 1994

NASA Astrophysics Data System (ADS)

1993-01-01

This meeting, organized by the Paul Scherrer Institute's Department of Applied Solid State Physics, will be held from 27 30 March 1994 at the Hotel Regina-Titlis, Engelberg, Switzerland. The aim is to bring together scientists from two important fields of current research and increasing industrial relevance. Optical metrology is a traditional discipline of applied optics which reached the nanometre scale a long time ago. Nanotechnology is setting new limits and represents a major challenge to metrology, as well as offering new opportunities to optics. The meeting is intended to help define a common future for optical metrology and nanotechnology. Topics to be covered include: nanometre position control and measuring techniques ultrahigh precision interferometry scanning probe microscopy (AFM, SNOM, etc.) surface modification by scanning probe methods precision surface fabrication and characterization nanolithography micro-optics, diffractive optics components, including systems and applications subwavelength optical structures synthetic optical materials structures and technologies for X-ray optics. For further information please contact: Jens Gobrecht (Secretary), Paul Scherrer Institute, CH-5232 Villigen-PSI, Switzerland.Tel. (41)56992529; Fax (41) 5698 2635.

Couplings

NASA Astrophysics Data System (ADS)

Stošić, Dušan; Auroux, Aline

Basic principles of calorimetry coupled with other techniques are introduced. These methods are used in heterogeneous catalysis for characterization of acidic, basic and red-ox properties of solid catalysts. Estimation of these features is achieved by monitoring the interaction of various probe molecules with the surface of such materials. Overview of gas phase, as well as liquid phase techniques is given. Special attention is devoted to coupled calorimetry-volumetry method. Furthermore, the influence of different experimental parameters on the results of these techniques is discussed, since it is known that they can significantly influence the evaluation of catalytic properties of investigated materials.

The birth and evolution of surface science: Child of the union of science and technology

PubMed Central

Duke, C. B.

2003-01-01

This article is an account of the birth and evolution of surface science as an interdisciplinary research area. Surface science emanated from the confluence of concepts and tools in physics and chemistry with technological innovations that made it possible to determine the structure and properties of surfaces and interfaces and the dynamics of chemical reactions at surfaces. The combination in the 1960s and 1970s of ultra-high-vacuum (i.e., P < 10−7 Pascal or 10−9 Torr) technology with the recognition that electrons in the energy range from 50 to 500 eV exhibited inelastic collision mean free paths of the order of a few angstroms fostered an explosion of activity. The results were a reformulation of the theory of electron solid scattering, the nearly universal use of electron spectroscopies for surface characterization, the rise of surface science as an independent interdisciplinary research area, and the emergence of the American Vacuum Society (AVS) as a major international scientific society. The rise of microelectronics in the 1970s and 1980s resulted in huge increases in computational power. These increases enabled more complex experiments and the utilization of density functional theory for the quantitative prediction of surface structure and dynamics. Development of scanning-probe microscopies in the 1990s led to atomic-resolution images of macroscopic surfaces and interfaces as well as videos of atoms moving about on surfaces during growth and diffusion. Scanning probes have since brought solid–liquid interfaces into the realm of atomic-level surface science, expanding its scope to more complex systems, including fragile biological materials and processes. PMID:12651946

Combined IR-Raman vs vibrational sum-frequency heterospectral correlation spectroscopy

NASA Astrophysics Data System (ADS)

Roy, Sandra; Beutier, Clémentine; Hore, Dennis K.

2018-06-01

Vibrational sum-frequency generation spectroscopy is a valuable probe of surface structure, particularly when the same molecules are present in one of the adjacent bulk solid or solution phases. As a result of the non-centrosymmetric requirement of SFG, the signal generated is a marker of the extent to which the molecules are ordered in an arrangement that breaks the up-down symmetry at the surface. In cases where the accompanying changes in the bulk are of interest in understanding and interpreting the surface structure, simultaneous analysis of the bulk IR absorption or bulk Raman scattering is helpful, and may be used in heterospectral surface-bulk two-dimensional correlation. We demonstrate that, in such cases, generating a new type of bulk spectrum that combines the IR and Raman amplitudes is a better candidate than the individual IR and Raman spectra for the purpose of correlation with the SFG signal.

Characterization of ozone decomposition in a soil slurry: kinetics and mechanism.

PubMed

Lim, Hyung-Nam; Choi, Hechul; Hwang, Tae-Moon; Kang, Joon-Wun

2002-01-01

A series of soil slurry experiments were performed in a carefully conceived reactor set-up to investigate the characteristics of the catalytic decomposition of ozone on a sand and iron surface. Real time on-line monitoring of ozone in the reaction module was possible using flow injection analysis coupled with a computer-controlled UV detector and data acquisition system. The effects of the soil media and size, ozone dosage, pH and p-CBA as a probe compound were examined at the given experimental conditions. Two apparent phases existed, and ozone instantaneously decomposed within one second in the first phase. These were defined as the instantaneous ozone demand (ID) phase, and the relatively slow decay stage. The interactions of ozone with the soil organic matter (SOM) and metal oxides were attributed mostly to the instantaneous decomposition of ozone. From the probe (p-CBA) experiments, 60-68% of total p-CBA removal occurred during the ID phase. The generation of hydroxyl radicals (OH.) was demonstrated and was closely related with metal oxides as well as SOM. Metal oxides in soil surface were considered to have relatively faster reaction rate with ozone and provide more favorable reactive sites to generate higher amount of OH. than SOM. Even at one-tenth concentration of the sands, a goethite-induced catalytic reaction outfitted the removal rate ofp-CBA among all the soils tested. More than 40% of total p-CBA removal occurred on the soil surface. It was inferred that the radical reaction with the probe compound seemed to take place not only on the soil surface but also in the solid-liquid interface. Ozone decomposition and the reaction between OH. and p-CBA appeared to be independent of any change in pH.

Characterization of laser-driven shock waves in solids using a fiber optic pressure probe.

PubMed

Cranch, Geoffrey A; Lunsford, Robert; Grün, Jacob; Weaver, James; Compton, Steve; May, Mark; Kostinski, Natalie

2013-11-10

Measurement of laser-driven shock wave pressure in solid blocks of polymethyl methacrylate is demonstrated using fiber optic pressure probes. Three probes based on a fiber Fabry-Perot, fiber Bragg grating, and interferometric fiber tip sensor are tested and compared. Shock waves are generated using a high-power laser focused onto a thin foil target placed in close proximity to the test blocks. The fiber Fabry-Perot sensor appears capable of resolving the shock front with a rise time of 91 ns. The peak pressure is estimated, using a separate shadowgraphy measurement, to be 3.4 GPa.

Anisotropic high-harmonic generation in bulk crystals

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

You, Yong Sing; Reis, David A.; Ghimire, Shambhu

2016-11-21

The microscopic valence electron density determines the optical, electronic, structural and thermal properties of materials. However, current techniques for measuring this electron charge density are limited: for example, scanning tunnelling microscopy is confined to investigations at the surface, and electron diffraction requires very thin samples to avoid multiple scattering. Therefore, an optical method is desirable for measuring the valence charge density of bulk materials. Since the discovery of high-harmonic generation (HHG) in solids, there has been growing interest in using HHG to probe the electronic structure of solids. Here, using single-crystal MgO, we demonstrate that high-harmonic generation in solids ismore » sensitive to interatomic bonding. We find that harmonic efficiency is enhanced (diminished) for semi-classical electron trajectories that connect (avoid) neighbouring atomic sites in the crystal. Finally, these results indicate the possibility of using materials’ own electrons for retrieving the interatomic potential and thus the valence electron density, and perhaps even wavefunctions, in an all-optical setting.« less

Cassini First Radio Science Observations of Titan's Atmosphere and Surface

NASA Astrophysics Data System (ADS)

Marouf, Essam A.; Flasar, F. M.; French, R. G.; Kliore, A. J.; Nagy, A. F.; Rappaport, N. J.; Schinder, P. J.; McGhee, C. A.; Simpson, R.; Anabtawi, A.; Asmar, S.; Barbinis, E.; Goltz, G.; Fleischman, D.; Kahan, D.; Rochblatt, D.

2006-09-01

The first two Cassini radio occultations of Titan's atmosphere occurred on March 18 (T12) and May 20 (T14), 2006. The atmosphere was probed on the ingress and egress sides, yielding observations at four mid-southern latitudes. Titan's surface was also probed using bistatic-scattering during the inbound period on T12 and the inbound and outbound periods on T14. In all cases, quasi-monochromatic S-, X-, and Ka-bands RCP signals (13, 3.6, and 0.94 cm-wavelength, respectively) were transmitted from Cassini. Both the RCP and LCP signal components were observed at multiple ground receiving stations of the NASA/DSN. Demanding spacecraft maneuvers to point the Cassini high-gain antenna to virtual Earth during the occultations, and to track the specular region on Titan's surface during the bistatic observations were successfully implemented. For the first time ever, quasi-specular bistatic scattering surface echo is detected on both the inbound and outbound T14 observations. Although weak, an X-band RCP and LCP reflected spectral components are clearly detectable. Their total power ratio determines the refractive index of the regions probed and its likely nature (liquid vs solid). The echo appears consistent with reflection from localized hydrocarbon liquid regions embedded in mostly nonspecularly reflecting terrain. The atmospheric refracted S and X signals were tracked down to Titan's surface. The Ka signal was consistently extinguished by atmospheric absorption at about 10 km above the surface. Observed changes of signal frequency is used to recover the refractivity profiles of the neutral atmosphere, hence determine the corresponding temperature-pressure profiles assuming 100% N2 composition. Changes of signal strength, corrected to remove refractive defocusing, reveals both small-scale and large-scale effects. The former is likely due to gravity waves, turbulence, and layers. The latter exhibits remarkable wavelength dependence and is likely caused by dispersive N2-N2 collision-induced gaseous absorption, although additional extinction mechanisms may also be responsible.

The surface chemical reactivity of particles and its impact on human health

NASA Astrophysics Data System (ADS)

Setyan, A.; Sauvain, J. J.; Riediker, M.; Guillemin, M.; Rossi, M. J.

2017-12-01

The chemical composition of the particle-air interface is the gateway to chemical reactions of gases with condensed phase particles. It is of prime importance to understand the reactivity of particles and their interaction with surrounding gases, biological membranes, and solid supports. We used a Knudsen flow reactor to quantify functional groups on the surface of a few selected particle types. This technique is based on a heterogeneous titration reaction between a probe gas and a specific functional group on the particle surface. Six probe gases have been selected for the identification and quantification of important functional groups: N(CH3)3 for the titration of acidic sites, NH2OH for the detection of carbonyl functions (aldehydes and ketones) and/or oxidized sites owing to its strong reducing properties, CF3COOH and HCl for basic sites of different strength, O3 and NO2 for oxidizable groups. We also studied the kinetics of the reactions between particles and probe gases (uptake coefficient γ0). We tested the surface chemical composition and oxidation states of laboratory-generated aerosols (3 amorphous carbons, 2 flame soots, 2 Diesel particles, 2 secondary organic aerosols [SOA], 4 multiwall carbon nanotubes [MWCNT], 3 TiO2, and 2 metal salts) and of aerosols sampled in several bus depots. The sampling of particles in the bus depots was accompanied by the collection of urine samples of mechanics working full-time in these bus depots, and the quantification of 8-hydroxy-2'-deoxyguanosine, a biomarker of oxidative stress. The increase in oxidative stress biomarker levels over a working day was correlated (p<0.05) with the number of olefinic and/or PAH sites on the surface of particles sampled at the bus depots, obtained from O3 uptakes, as well as with the initial uptake coefficient (γ0) of five probe gases used in the field. This correlation with γ0 suggests the idea of competing pathways occurring at the interface of the aerosol particles between the generation of reactive oxygen species (ROS) responsible for oxidative stress and cellular antioxidants.

"Artificial lymphatic system": a new approach to reduce interstitial hypertension and increase blood flow, pH and pO2 in solid tumors.

PubMed

DiResta, G R; Lee, J; Healey, J H; Levchenko, A; Larson, S M; Arbit, E

2000-05-01

A mechanical drainage system, the "artificial lymphatic system" (ALS), consisting of a vacuum source and drain, is evaluated for its ability to aspirate the interstitial fluids responsible for the elevated interstitial fluid pressure (IFP) observed in solid tumors. IFP, pH, and pO2 radial profiles were measured before and after aspiration using wick-in-needle (WIN) probes, needle pH and oxygen electrodes, respectively. Laser Doppler flowmetry measured temporal changes in blood flow rate (BFR) at the tumor surface during aspiration. The WIN probe and IFP profile data were analyzed using numerical simulation and distributed mathematical models, respectively. The model parameter, P(E), reflecting central tumor IFP, was reduced from 15.3 to 5.7 mm Hg in neuroblastoma and from 13.3 to 12.1 mm Hg in Walker 256, respectively, following aspiration. The simulation demonstrated that spatial averaging inherent in WIN measurements reduced the calculated magnitude of the model parameter changes. IFP was significantly lower (p<0.05), especially in regions surrounding the drain, and BFR was significantly higher (p<0.05) following 25 and 45 min of aspiration, respectively; pH and pO2 profiles increased following aspiration. The experimental and mathematical findings suggest that ALS aspiration may be a viable way of reducing IFP and increasing BFR, pO2, and pH and should enhance solid tumor chemo and radiation therapy.

Aspheric surface measurement using capacitive probes

NASA Astrophysics Data System (ADS)

Tao, Xin; Yuan, Daocheng; Li, Shaobo

2017-02-01

With the application of aspheres in optical fields, high precision and high efficiency aspheric surface metrology becomes a hot research topic. We describe a novel method of non-contact measurement of aspheric surface with capacitive probe. Taking an eccentric spherical surface as the object of study, the averaging effect of capacitive probe measurement and the influence of tilting the capacitive probe on the measurement results are investigated. By comparing measurement results from simultaneous measurement of the capacitive probe and contact probe of roundness instrument, this paper indicates the feasibility of using capacitive probes to test aspheric surface and proposes the compensation method of measurement error caused by averaging effect and the tilting of the capacitive probe.

Exploring the Electronic Landscape at Interfaces and Junctions in Semiconductor Nanowire Devices with Subsurface Local Probing of Carrier Dynamics

NASA Astrophysics Data System (ADS)

McGuckin, Terrence

The solid state devices that are pervasive in our society, are based on building blocks composed of interfaces between materials and junctions that manipulate how charge carriers behave in a device. As the dimensions of these devices are reduced to the nanoscale, surfaces and interfaces play a larger role in the behavior of carriers in devices and must be thoroughly investigated to understand not only the material properties but how these materials interact. Separating the effects of these different building blocks is a challenge, as most testing methods measure the performance of the whole device. Semiconductor nanowires represent an excellent test system to explore the limits of size and novel device structures. The behavior of charge carriers in semiconductor nanowire devices under operational conditions is investigated using local probing technique electron beam induced current (EBIC). The behavior of locally excited carriers are driven by the forces of drift, from electric fields within a device at junctions, surfaces, contacts and, applied voltage bias, and diffusion. This thesis presents the results of directly measuring these effects spatially with nanometer resolution, using EBIC in Ge, Si, and complex heterostructure GaAs/AlGaAs nanowire devices. Advancements to the EBIC technique, have pushed the resolution from tens of nanometers down to 1 to 2 nanometers. Depth profiling and tuning of the interaction volume allows for the separating the signal originating from the surface and the interior of the nanowire. Radial junctions and variations in bands can now be analyzed including core/shell hetero-structures. This local carrier probing reveals a number of surprising behaviors; Most notably, directly imaging the evolution of surface traps filling with electrons causing bandbending at the surface of Ge nanowires that leads to an enhancement in the charge separation of electrons and holes, and extracting different characteristic lengths from GaAs and AlGaAs in core/shell nanowires. For new and emerging solid state materials, understanding charge carrier dynamics is crucial to designing functional devices. Presented here are examples of the wide application of EBIC, and its variants, through imaging domains in ferroelectric materials, local electric fields and defects in 2D semiconductor material MoS2, and gradients in doping profiles of solar cells. Measuring the local behavior of carrier dynamics, EBIC has the potential to be a key metrology technique in correlative microscopy, enabling a deeper understanding of materials and how they interact within devices.

On the dynamics of water molecules at the protein solute interfaces.

PubMed

Bernini, A; Spiga, O; Ciutti, A; Chiellini, S; Menciassi, N; Venditti, V; Niccolai, N

2004-10-01

Proteins, with the large variety of chemical groups they present at their molecular surface, are a class of molecules which can be very informative on most of the possible solute-solvent interactions. Hen egg white lysozyme has been used as a probe to investigate the complex solvent dynamics occurring at the protein surface, by analysing the results obtained from Nuclear Magnetic Resonance, X-ray diffractometry and Molecular Dynamics simulations. A consistent overall picture for the dynamics of water molecules close to the protein is obtained, suggesting that a rapid exchange occurs, in a picosecond timescale, among all the possible hydration surface sites both in solution and the solid state, excluding the possibility that solvent molecules can form liquid-crystal-like supramolecular adducts, which have been proposed as a molecular basis of 'memory of water'.

Effect of air confinement on thermal contact resistance in nanoscale heat transfer

NASA Astrophysics Data System (ADS)

Pratap, Dheeraj; Islam, Rakibul; Al-Alam, Patricia; Randrianalisoa, Jaona; Trannoy, Nathalie

2018-03-01

Here, we report a detailed analysis of thermal contact resistance (R c) of nano-size contact formed between a Wollaston wire thermal probe and the used samples (fused silica and titanium) as a function of air pressure (from 1 Pa to 105 Pa). Moreover, we suggest an analytical model using experimental data to extract R c. We found that for both samples, the thermal contact resistance decreases with increasing air pressure. We also showed that R c strongly depends on the thermal conductivity of materials keeping other parameters the same, such as roughness of the probe and samples, as well as the contact force. We provide a physical explanation of the R c trend with pressure and thermal conductivity of the materials: R c is ascribed to the heat transfer through solid-solid (probe-sample) contact and confined air at nanoscale cavities, due to the rough nature of the materials in contact. The contribution of confined air on heat transfer through the probe sample contact is significant at atmospheric pressure but decreases as the pressure decreases. In vacuum, only the solid-solid contact contributes to R c. In addition, theoretical calculations using the well-known acoustic and diffuse mismatch models showed a high thermal conductivity material that exhibits high heat transmission and consequently low R c, supporting our findings.

STM, SECPM, AFM and Electrochemistry on Single Crystalline Surfaces

PubMed Central

Wolfschmidt, Holger; Baier, Claudia; Gsell, Stefan; Fischer, Martin; Schreck, Matthias; Stimming, Ulrich

2010-01-01

Scanning probe microscopy (SPM) techniques have had a great impact on research fields of surface science and nanotechnology during the last decades. They are used to investigate surfaces with scanning ranges between several 100 μm down to atomic resolution. Depending on experimental conditions, and the interaction forces between probe and sample, different SPM techniques allow mapping of different surface properties. In this work, scanning tunneling microscopy (STM) in air and under electrochemical conditions (EC-STM), atomic force microscopy (AFM) in air and scanning electrochemical potential microscopy (SECPM) under electrochemical conditions, were used to study different single crystalline surfaces in electrochemistry. Especially SECPM offers potentially new insights into the solid-liquid interface by providing the possibility to image the potential distribution of the surface, with a resolution that is comparable to STM. In electrocatalysis, nanostructured catalysts supported on different electrode materials often show behavior different from their bulk electrodes. This was experimentally and theoretically shown for several combinations and recently on Pt on Au(111) towards fuel cell relevant reactions. For these investigations single crystals often provide accurate and well defined reference and support systems. We will show heteroepitaxially grown Ru, Ir and Rh single crystalline surface films and bulk Au single crystals with different orientations under electrochemical conditions. Image studies from all three different SPM methods will be presented and compared to electrochemical data obtained by cyclic voltammetry in acidic media. The quality of the single crystalline supports will be verified by the SPM images and the cyclic voltammograms. Furthermore, an outlook will be presented on how such supports can be used in electrocatalytic studies. PMID:28883327

Solid phase sequencing of double-stranded nucleic acids

DOEpatents

Fu, Dong-Jing; Cantor, Charles R.; Koster, Hubert; Smith, Cassandra L.

2002-01-01

This invention relates to methods for detecting and sequencing of target double-stranded nucleic acid sequences, to nucleic acid probes and arrays of probes useful in these methods, and to kits and systems which contain these probes. Useful methods involve hybridizing the nucleic acids or nucleic acids which represent complementary or homologous sequences of the target to an array of nucleic acid probes. These probe comprise a single-stranded portion, an optional double-stranded portion and a variable sequence within the single-stranded portion. The molecular weights of the hybridized nucleic acids of the set can be determined by mass spectroscopy, and the sequence of the target determined from the molecular weights of the fragments. Nucleic acids whose sequences can be determined include nucleic acids in biological samples such as patient biopsies and environmental samples. Probes may be fixed to a solid support such as a hybridization chip to facilitate automated determination of molecular weights and identification of the target sequence.

Flexible high-temperature pH probe

DOEpatents

Bielawski, John C.; Outwater, John O.; Halbfinger, George P.

2003-04-22

A flexible pH probe device is provided for use in hot water and other high temperature environments up to about 590.degree. F. The pH probe includes a flexible, inert tubular probe member, an oxygen anion conducting, solid state electrolyte plug located at the distal end of the tubular member, oxide powder disposed at the distal end of the tubular member; a metal wire extending along the tubular member and having a distal end in contact with the oxide powder so as to form therewith an internal reference electrode; and a compression fitting forming a pressure boundary seal around a portion of the tubular member remote from the distal end thereof. Preferably, the tubular member is made of polytetrafluoroethylene, and the solid state electrolyte plug is made of stabilized zirconia. The flexibility of the probe member enables placement of the electrode into the area of interest, including around corners, into confined areas and the like.

Investigating nearby exoplanets via interstellar radar

NASA Astrophysics Data System (ADS)

Scheffer, Louis K.

2014-01-01

Interstellar radar is a potential intermediate step between passive observation of exoplanets and interstellar exploratory missions. Compared with passive observation, it has the traditional advantages of radar astronomy. It can measure surface characteristics, determine spin rates and axes, provide extremely accurate ranges, construct maps of planets, distinguish liquid from solid surfaces, find rings and moons, and penetrate clouds. It can do this even for planets close to the parent star. Compared with interstellar travel or probes, it also offers significant advantages. The technology required to build such a radar already exists, radar can return results within a human lifetime, and a single facility can investigate thousands of planetary systems. The cost, although too high for current implementation, is within the reach of Earth's economy.

Pluto's Radius

NASA Astrophysics Data System (ADS)

Young, Eliot F.; Young, L. A.; Buie, M.

2007-10-01

The size of Pluto has been difficult to measure. Stellar occultations by Pluto have not yet probed altitudes lower than 1198 km, assuming the clear atmosphere model of Elliot, Person and Qu (2003). Differential refraction by Pluto's atmosphere attenuates the light from an occulted star to a level that is indistinguishable from the zero-level baseline long before Pluto's solid surface is a factor. Since Charon has no detectable atmosphere, its radius was well determined from a stellar occultation in 2005 (Gulbis et al. 2006, Sicardy et al. 2006). Combined with the mutual event photometry (Charon transited Pluto every 6.38 days between 1986 through 1992) - for which differential refraction is a negligible effect - the well-known radius of Charon translates into a more accurate radius for Pluto's solid surface. Our preliminary solid radius estimate for Pluto is 1161 km. We will discuss error bars and the correlations of this determination with Pluto albedo maps. We will also discuss the implications for Pluto's thermal profile, surface temperature and pressure, and constraints on the presence of a haze layer. This work is funded by NASA's Planetary Astronomy program. References Elliot, J.L., Person, M.J., & Qu, S. 2003, "Analysis of Stellar Occultation Data. II. Inversion, with Application to Pluto and Triton." AJ, 126, 1041. Gulbis, A.A.S. et al. 2006, "Charon's radius and atmospheric constraints from observations of a stellar occultation." Nature, 49, 48. Sicardy, B. et al. 2006, "Charon's size and an upper limit on its atmosphere from a stellar occultation." Nature, 49, 52.

Plasma Immersion Ion Implantation with Solid Targets for Space and Aerospace Applications

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

Oliveira, R. M.; Goncalves, J. A. N.; Ueda, M.

2009-01-05

This paper describes successful results obtained by a new type of plasma source, named as Vaporization of Solid Targets (VAST), for treatment of materials for space and aerospace applications, by means of plasma immersion ion implantation and deposition (PIII and D). Here, the solid element is vaporized in a high pressure glow discharge, being further ionized and implanted/deposited in a low pressure cycle, with the aid of an extra electrode. First experiments in VAST were run using lithium as the solid target. Samples of silicon and aluminum alloy (2024) were immersed into highly ionized lithium plasma, whose density was measuredmore » by a double Langmuir probe. Measurements performed with scanning electron microscopy (SEM) showed clear modification of the cross-sectioned treated silicon samples. X-ray photoelectron spectroscopy (XPS) analysis revealed that lithium was implanted/deposited into/onto the surface of the silicon. Implantation depth profiles may vary according to the condition of operation of VAST. One direct application of this treatment concerns the protection against radiation damage for silicon solar cells. For the case of the aluminum alloy, X-ray diffraction analysis indicated the appearance of prominent new peaks. Surface modification of A12024 by lithium implantation/deposition can lower the coefficient of friction and improve the resistance to fatigue of this alloy. Recently, cadmium was vaporized and ionized in VAST. The main benefit of this element is associated with the improvement of corrosion resistance of metallic substrates. Besides lithium and cadmium, VAST allows to performing PIII and D with other species, leading to the modification of the near-surface of materials for distinct purposes, including applications in the space and aerospace areas.« less

Perceiving the vertical distances of surfaces by means of a hand-held probe.

PubMed

Chan, T C; Turvey, M T

1991-05-01

Nine experiments were conducted on the haptic capacity of people to perceive the distances of horizontal surfaces solely on the basis of mechanical stimulation resulting from contacting the surfaces with a vertically held rod. Participants touched target surfaces with rods inside a wooden cabinet and reported the perceived surface location with an indicator outside the cabinet. The target surface, rod, and the participant's hand were occluded, and the sound produced in exploration was muffled. Properties of the probe (length, mass, moment of inertia, center of mass, and shape) were manipulated, along with surface distance and the method and angle of probing. Results suggest that for the most common method of probing, namely, tapping, perceived vertical distance is specific to a particular relation among the rotational inertia of the probe, the distance of the point of contact with the surface from the probe's center of percussion, and the inclination at contact of the probe to the surface. They also suggest that the probe length and the distance probed are independently perceivable. The results were discussed in terms of information specificity versus percept-percept coupling and parallels between selective attention in haptic and visual perception.

Monolayer Contact Doping of Silicon Surfaces and Nanowires Using Organophosphorus Compounds

PubMed Central

Hazut, Ori; Agarwala, Arunava; Subramani, Thangavel; Waichman, Sharon; Yerushalmi, Roie

2013-01-01

Monolayer Contact Doping (MLCD) is a simple method for doping of surfaces and nanostructures1. MLCD results in the formation of highly controlled, ultra shallow and sharp doping profiles at the nanometer scale. In MLCD process the dopant source is a monolayer containing dopant atoms. In this article a detailed procedure for surface doping of silicon substrate as well as silicon nanowires is demonstrated. Phosphorus dopant source was formed using tetraethyl methylenediphosphonate monolayer on a silicon substrate. This monolayer containing substrate was brought to contact with a pristine intrinsic silicon target substrate and annealed while in contact. Sheet resistance of the target substrate was measured using 4 point probe. Intrinsic silicon nanowires were synthesized by chemical vapor deposition (CVD) process using a vapor-liquid-solid (VLS) mechanism; gold nanoparticles were used as catalyst for nanowire growth. The nanowires were suspended in ethanol by mild sonication. This suspension was used to dropcast the nanowires on silicon substrate with a silicon nitride dielectric top layer. These nanowires were doped with phosphorus in similar manner as used for the intrinsic silicon wafer. Standard photolithography process was used to fabricate metal electrodes for the formation of nanowire based field effect transistor (NW-FET). The electrical properties of a representative nanowire device were measured by a semiconductor device analyzer and a probe station. PMID:24326774

Implications of contamination and surface area ratios for Langmuir probe diagnostics on CubeSats

NASA Astrophysics Data System (ADS)

Suresh, P.; Swenson, C.

2009-12-01

Theories describing the current collected by a biased probe under various conditions are necessary for such observation to be used to accurately determine plasma properties. Langmuir probes are routinely used on spacecraft to measure plasma parameters such as density, temperature, and vehicle charging. The collected current is a function of the potential between the surrounding plasma and probe surface. There have been both observations of and concepts for unaccounted variations of this potential which limit the application of Langmuir probe theory for determining plasma properties. These variations occur due to spatial variations of the work function across the probe surface due to non-uniformity of the crystalline surface properties and surface contamination of the probe. Currently we do not have theoretical expressions which consider these factors as first principles in their derivation. In the event of these surface potential variations, the analysis of the plasma using the currently available theories of the Langmuir probe yield erroneous results. We present a theory which models the current as a function of the surface potential variations. Another consideration for Langmuir probes on CubeSats is the ratio of the probe area to the return current collection area. If the area ratio is unfavorable this can also lead to erroneous results in the interpretation of observations. A mathematical formulation of the current collected by the probe for contaminated surfaces is presented and compared with data from a Langmuir probe flown on a sounding rocket mission. The implications of using Langmuir probes on CubeSats given the engineering limitations of probe cleanliness and area ratios are reviewed.

'Incremental thermocouple probe' for testing insulation erosion on a rocket motor

NASA Technical Reports Server (NTRS)

Gould, Reginald J.

1993-01-01

An incremental thermocouple probe was developed to measure insulation erosion during a solid rocket motor firing. The probe's new and unique design is described along with its theory of operation. Data from an actual firing are reported which show that the probe's performance greatly exceeded predictions and present technology as a temperature measurement device and as an event gage.

Characterization of laser-driven shock waves in solids using a fiber optic pressure probe

DOE PAGES

Cranch, Geoffrey A.; Lunsford, Robert; Grun, Jacob; ...

2013-11-08

Measurement of laser-driven shock wave pressure in solid blocks of polymethyl methacrylate is demonstrated using fiber optic pressure probes. Three probes based on a fiber Fabry–Perot, fiber Bragg grating, and interferometric fiber tip sensor are tested and compared. Shock waves are generated using a high-power laser focused onto a thin foil target placed in close proximity to the test blocks. The fiber Fabry–Perot sensor appears capable of resolving the shock front with a rise time of 91 ns. As a result, the peak pressure is estimated, using a separate shadowgraphy measurement, to be 3.4 GPa.

Enhanced biocompatibility of neural probes by integrating microstructures and delivering anti-inflammatory agents via microfluidic channels

NASA Astrophysics Data System (ADS)

Liu, Bin; Kim, Eric; Meggo, Anika; Gandhi, Sachin; Luo, Hao; Kallakuri, Srinivas; Xu, Yong; Zhang, Jinsheng

2017-04-01

Objective. Biocompatibility is a major issue for chronic neural implants, involving inflammatory and wound healing responses of neurons and glial cells. To enhance biocompatibility, we developed silicon-parylene hybrid neural probes with open architecture electrodes, microfluidic channels and a reservoir for drug delivery to suppress tissue responses. Approach. We chronically implanted our neural probes in the rat auditory cortex and investigated (1) whether open architecture electrode reduces inflammatory reaction by measuring glial responses; and (2) whether delivery of antibiotic minocycline reduces inflammatory and tissue reaction. Four weeks after implantation, immunostaining for glial fibrillary acid protein (astrocyte marker) and ionizing calcium-binding adaptor molecule 1 (macrophages/microglia cell marker) were conducted to identify immunoreactive astrocyte and microglial cells, and to determine the extent of astrocytes and microglial cell reaction/activation. A comparison was made between using traditional solid-surface electrodes and newly-designed electrodes with open architecture, as well as between deliveries of minocycline and artificial cerebral-spinal fluid diffused through microfluidic channels. Main results. The new probes with integrated micro-structures induced minimal tissue reaction compared to traditional electrodes at 4 weeks after implantation. Microcycline delivered through integrated microfluidic channels reduced tissue response as indicated by decreased microglial reaction around the neural probes implanted. Significance. The new design will help enhance the long-term stability of the implantable devices.

The Detection of Protein via ZnO Resonant Raman Scattering Signal

NASA Astrophysics Data System (ADS)

Shan, Guiye; Yang, Guoliang; Wang, Shuang; Liu, Yichun

2008-03-01

Detecting protein with high sensitivity and specificity is essential for disease diagnostics, drug screening and other application. Semiconductor nanoparticles show better properties than organic dye molecules when used as markers for optical measurements. We used ZnO nanoparticles as markers for detecting protein in resonant Raman scattering measurements. The highly sensitive detection of proteins was achieved by an antibody-based sandwich assay. A probe for the target protein was constructed by binding the ZnO/Au nanoparticles to a primary antibody by eletrostatic interaction between Au and the antibody. A secondary antibody, which could be specifically recognized by target protein, was attached to a solid surface. The ZnO/Au-antibody probe could specifically recognize and bind to the complex of the target protein and secondary antibody. Our measurements using the resonant Raman scattering signal of ZnO nanoparticles showed good selectivity and sensitivity for the target protein.

Nanometer-scale mapping of irreversible electrochemical nucleation processes on solid Li-ion electrolytes

NASA Astrophysics Data System (ADS)

Kumar, Amit; Arruda, Thomas M.; Tselev, Alexander; Ivanov, Ilia N.; Lawton, Jamie S.; Zawodzinski, Thomas A.; Butyaev, Oleg; Zayats, Sergey; Jesse, Stephen; Kalinin, Sergei V.

2013-04-01

Electrochemical processes associated with changes in structure, connectivity or composition typically proceed via new phase nucleation with subsequent growth of nuclei. Understanding and controlling reactions requires the elucidation and control of nucleation mechanisms. However, factors controlling nucleation kinetics, including the interplay between local mechanical conditions, microstructure and local ionic profile remain inaccessible. Furthermore, the tendency of current probing techniques to interfere with the original microstructure prevents a systematic evaluation of the correlation between the microstructure and local electrochemical reactivity. In this work, the spatial variability of irreversible nucleation processes of Li on a Li-ion conductive glass-ceramics surface is studied with ~30 nm resolution. An increased nucleation rate at the boundaries between the crystalline AlPO4 phase and amorphous matrix is observed and attributed to Li segregation. This study opens a pathway for probing mechanisms at the level of single structural defects and elucidation of electrochemical activities in nanoscale volumes.

Nanometer-scale mapping of irreversible electrochemical nucleation processes on solid Li-ion electrolytes.

PubMed

Kumar, Amit; Arruda, Thomas M; Tselev, Alexander; Ivanov, Ilia N; Lawton, Jamie S; Zawodzinski, Thomas A; Butyaev, Oleg; Zayats, Sergey; Jesse, Stephen; Kalinin, Sergei V

2013-01-01

Electrochemical processes associated with changes in structure, connectivity or composition typically proceed via new phase nucleation with subsequent growth of nuclei. Understanding and controlling reactions requires the elucidation and control of nucleation mechanisms. However, factors controlling nucleation kinetics, including the interplay between local mechanical conditions, microstructure and local ionic profile remain inaccessible. Furthermore, the tendency of current probing techniques to interfere with the original microstructure prevents a systematic evaluation of the correlation between the microstructure and local electrochemical reactivity. In this work, the spatial variability of irreversible nucleation processes of Li on a Li-ion conductive glass-ceramics surface is studied with ~30 nm resolution. An increased nucleation rate at the boundaries between the crystalline AlPO4 phase and amorphous matrix is observed and attributed to Li segregation. This study opens a pathway for probing mechanisms at the level of single structural defects and elucidation of electrochemical activities in nanoscale volumes.

Nanometer-scale mapping of irreversible electrochemical nucleation processes on solid Li-ion electrolytes

PubMed Central

Kumar, Amit; Arruda, Thomas M.; Tselev, Alexander; Ivanov, Ilia N.; Lawton, Jamie S.; Zawodzinski, Thomas A.; Butyaev, Oleg; Zayats, Sergey; Jesse, Stephen; Kalinin, Sergei V.

2013-01-01

Electrochemical processes associated with changes in structure, connectivity or composition typically proceed via new phase nucleation with subsequent growth of nuclei. Understanding and controlling reactions requires the elucidation and control of nucleation mechanisms. However, factors controlling nucleation kinetics, including the interplay between local mechanical conditions, microstructure and local ionic profile remain inaccessible. Furthermore, the tendency of current probing techniques to interfere with the original microstructure prevents a systematic evaluation of the correlation between the microstructure and local electrochemical reactivity. In this work, the spatial variability of irreversible nucleation processes of Li on a Li-ion conductive glass-ceramics surface is studied with ~30 nm resolution. An increased nucleation rate at the boundaries between the crystalline AlPO4 phase and amorphous matrix is observed and attributed to Li segregation. This study opens a pathway for probing mechanisms at the level of single structural defects and elucidation of electrochemical activities in nanoscale volumes. PMID:23563856

Exploring Ultrafast Structural Dynamics for Energetic Enhancement or Disruption

DTIC Science & Technology

2016-03-01

it. In a pump -push/ dump probe experiment, a secondary laser pulse (push/ dump ) is used after the initial perturbation due to the pump pulse. The...increased. The pump -push/ dump probe technique is a difficult experiment that requires a highly stable laser source. Ultrafast pump -probe experiments...decomposition of solids. Journal of Applied Physics. 2001;89:4156–4166. 17. Kee TW. Femtosecond pump -push-probe and pump - dump -probe spectroscopy of

Near infrared lasers in flow cytometry.

PubMed

Telford, William G

2015-07-01

Technology development in flow cytometry has closely tracked laser technology, the light source that flow cytometers almost exclusively use to excite fluorescent probes. The original flow cytometers from the 1970s and 1980s used large water-cooled lasers to produce only one or two laser lines at a time. Modern cytometers can take advantage of the revolution in solid state laser technology to use almost any laser wavelength ranging from the ultraviolet to the near infrared. Commercial cytometers can now be equipped with many small solid state lasers, providing almost any wavelength needed for cellular analysis. Flow cytometers are now equipped to analyze 20 or more fluorescent probes simultaneously, requiring multiple laser wavelengths. Instrument developers are now trying to increase this number by designing fluorescent probes that can be excited by laser wavelength at the "edges" of the visible light range, in the near ultraviolet and near-infrared region. A variety of fluorescent probes have been developed that excite with violet and long wavelength ultraviolet light; however, the near-infrared range (660-800 nm) has yet seen only exploitation in flow cytometry. Fortunately, near-infrared laser diodes and other solid state laser technologies appropriate for flow cytometry have been in existence for some time, and can be readily incorporated into flow cytometers to accelerate fluorescent probe development. The near infrared region represents one of the last "frontiers" to maximize the number of fluorescent probes that can be analyzed by flow cytometry. In addition, near infrared fluorescent probes used in biomedical tracking and imaging could also be employed for flow cytometry with the correct laser wavelengths. This review describes the available technology, including lasers, fluorescent probes and detector technology optimal for near infrared signal detection. Published by Elsevier Inc.

Dual-Frequency Bistatic Radar Probing of Mars: Potential and Pitfalls for Depth Sounding at Centimeter Wavelengths

NASA Astrophysics Data System (ADS)

Simpson, R. A.; Tyler, G. L.; Paetzold, M.; Haeusler, B.; Asmar, S. W.

2009-12-01

Early spacecraft-to-Earth bistatic radar (BSR) probing of Mars' surface emphasized measurement of rms surface slopes on scales of centimeters to a few meters, information of particular interest to the design and deployment of landers and rovers. Shorter wavelengths yielded higher values, consistent with fractal models in which surface texture becomes rougher as the measuring instrument senses more detail. Although Mars Express (MEX) has found the smoothest extraterrestrial solid surface yet observed by radar (0.17 deg rms in the north polar region), its antenna pattern typically illuminates only part of the scattering surface, making rms slope determination difficult. With careful calibration, however, the ratio of echo power in its two orthogonal polarizations can be used to infer the dielectric constant of the surface material from the Fresnel reflection coefficients. Early results showed larger dielectric constant at 12.6 cm than 3.6 cm, consistent with materials which become more densely packed at depth; as the data collection continued, regional variations became apparent. More puzzling, are cases in which the derived dielectric constant is 30 percent larger at the shorter wavelength, suggesting a centimeter of crust (invisible at 12.6 cm wavelength) overlying less dense regolith below. Duricrust layers have been inferred in some of these areas from thermal measurements; and a layer of gravel, stripped of finer particles, could produce similar effects. Earth-to-spacecraft BSR could improve measurement sensitivity by factors of 100-1000; spacecraft-to-spacecraft experiments could improve surface coverage. All three configurations, including the conventional 'downlink' experiments now being conducted, can provide basic information on surface structure to depths of a few centimeters.

Probing the surface of γ-Al2O3 by oxygen-17 dynamic nuclear polarization enhanced solid-state NMR spectroscopy.

PubMed

Li, Wenzheng; Wang, Qiang; Xu, Jun; Aussenac, Fabien; Qi, Guodong; Zhao, Xingling; Gao, Pan; Wang, Chao; Deng, Feng

2018-06-14

γ-Al2O3 is an important catalyst and catalyst support of industrial interest. Its acid/base characteristics are correlated to the surface structure, which has always been an issue of concern. In this work, the complex (sub-)surface oxygen species on surface-selectively labelled γ-Al2O3 were probed by 17O dynamic nuclear polarization surface-enhanced NMR spectroscopy (DNP-SENS). Direct 17O MAS and indirect 1H-17O cross-polarization (CP)/MAS DNP experiments enable observation of the (sub-)surface bare oxygen species and hydroxyl groups. In particular, a two-dimensional (2D) 17O 3QMAS DNP spectrum was for the first time achieved for γ-Al2O3, in which two O(Al)4 and one O(Al)3 bare oxygen species were identified. The 17O isotropic chemical shifts (δcs) vary from 56.7 to 81.0 ppm and the quadrupolar coupling constants (CQ) range from 0.6 to 2.5 MHz for the three oxygen species. The coordinatively unsaturated O(Al)3 species is characterized by a higher field chemical shift (56.7 ppm) and the largest CQ value (2.5 MHz) among these oxygen sites. 2D 1H → 17O HETCOR DNP experiments allow us to discriminate three bridging (Aln)-μ2-OH and two terminal (Aln)-μ1-OH hydroxyl groups. The structural features of the bare oxygen species and hydroxyl groups are similar for the γ-Al2O3 samples isotopically labelled by 17O2 gas or H217O. The results presented here show that the combination of surface-selective labelling and DNP-SENS is an effective approach for characterizing oxides with complex surface species.

In situ, simultaneous thermal imaging and infrared molecular emission studies of solid oxide fuel cell electrodes

NASA Astrophysics Data System (ADS)

Kirtley, J. D.; Qadri, S. N.; Steinhurst, D. A.; Owrutsky, J. C.

2016-12-01

Various in situ probes of solid oxide fuel cells (SOFCs) have advanced recently to provide detailed, real time data regarding materials and chemical processes that relate to device performance and degradation. These techniques offer insights into complex fuel chemistry at the anode in particular, especially in the context of model predictions. However, cell-to-cell variations can hinder mechanistic interpretations of measurements from separate, independent techniques. The present study describes an in situ technique that for the first time simultaneously measures surface temperature changes using near infrared thermal imaging and gas species using Fourier-transform infrared emission spectra at the anodes of operating SOFCs. Electrolyte-supported SOFCs with Ni-based anodes are operated at 700 °C with internal, dry-reformed methane at 75% maximum current and at open circuit voltage (OCV) while electrochemical and optical measurements are collected. At OCV, more cooling is observed coincident with more CO reforming products. Under load, CO decreases while the anode cools less, especially near the current collectors. The extent of cooling is more sensitive to polarization for electrolyte-supported cells because their anodes are thinner relative to anode-supported cells. This study exemplifies how this duplex technique can be a useful probe of electrochemical processes in SOFCs.

Coupled diffusion and mechanics in battery electrodes

NASA Astrophysics Data System (ADS)

Eshghinejad, Ahmadreza

We are living in a world with continuous production and consumption of energy. The energy production in the past decades has started to move away from petrochemical sources toward sustainable sources such as solar, wind and geothermal. Also, the energy consumption is further adapting to the sustainable sources. For instance, in recent years electric vehicles are growing fast that can consume sustainable electric energy stored in their batteries. In this direction, in order to further move toward sustainable energy, materials are becoming increasingly important for storing electric energy. Although, currently the technologies such as Li-ion batteries and solid-oxide fuel cells are commercially available for energy applications, improvements are crucial for the next generation of many other technologies producing or consuming sustainable energies. A critical aspect of the electrochemical activities involved in energy storage technologies such as Li-ion batteries and solid-oxide fuel cells is the diffusion of ions into the electrode materials. This process ultimately governs various functional properties of the batteries such as capacity and charging/discharging rates. The first goal of this dissertation is to develop mathematical tools to analyze the ionic diffusion and investigate its coupling with mechanics in electrodes. For this purpose, a thermodynamics-based modeling framework is developed and numerically solved using two numerical methods to analyze ionic diffusion in heterogeneous and structured electrodes. The next goal of this dissertation is to develop and analyze characterization techniques to probe the electrochemical processes at the nano-scale. To this end, the mathematical models are first employed to model a previously developed Atomic Force Microscopy based technique to probe local electrochemical activities called Electrochemical Strain Microscopy (ESM). This method probes the activities by inducing AC electric field to perturb ionic activities and measuring the surface vibrations. Different aspects of this technique are analyzed and the limitations are discussed. Such limitations moves the dissertation toward development of a new technique for probing the electrochemical activities, to overcome the previous limitations, called Scanning Thermo-ionic Microscopy (STIM). In this method, the local activities are probed by inducing AC temperature oscillations to perturb ionic activities and measuring the surface vibrations. The principle mathematical analysis of the coupled governing equations and the method of probing electrochemical activities are discussed in detail. Also, the method is implemented into the AFM hardware/software and the STIM response is confirmed using experiments on LiFePO4 and Sm-doped Ceria as well-known battery and fuel cell electrodes. The STIM method provides a clean method for analyzing energy storage materials and designing novel nano-structured materials for improved performance. Finally, conclusion of the presented work is discussed in the last chapter and the future works to continue the development of the modeling and experiments are listed.

The effect of probe choice and solution conditions on the apparent photoreactivity of dissolved organic matter.

PubMed

Maizel, Andrew C; Remucal, Christina K

2017-08-16

Excited triplet states of dissolved organic matter ( 3 DOM) are quantified directly with the species-specific probes trans,trans-hexadienoic acid (HDA) and 2,4,6-trimethylphenol (TMP), and indirectly with the singlet oxygen ( 1 O 2 ) probe furfuryl alcohol (FFA). Although previous work suggests that these probe compounds may be sensitive to solution conditions, including dissolved organic carbon concentration ([DOC]) and pH, and may quantify different 3 DOM subpopulations, the probes have not been systematically compared. Therefore, we quantify the apparent photoreactivity of diverse environmental waters using HDA, TMP, and FFA. By conducting experiments under ambient [DOC] and pH, with standardized [DOC] and pH, and with solid phase extraction isolates, we demonstrate that much of the apparent dissimilarity in photochemical measurements is attributable to solution conditions, rather than intrinsic differences in 3 DOM production. In general, apparent quantum yields (Φ 1 O 2 ≥ Φ 3 DOM,TMP ≫ Φ 3 DOM,HDA ) and pseudo-steady state concentrations ([ 1 O 2 ] ss > [ 3 DOM] ss,TMP > [ 3 DOM] ss,HDA ) show consistent relationships in all waters under standardized conditions. However, intrinsic differences in 3 DOM photoreactivity are apparent between DOM from diverse sources, as seen in the higher Φ 1 O 2 and lower Φ 3 DOM,TMP of wastewater effluents compared with oligotrophic lakes. Additionally, while conflicting trends in photoreactivity are observed under ambient conditions, all probes observe quantum yields increasing from surface wetlands to terrestrially influenced waters to oligotrophic lakes under standardized conditions. This work elucidates how probe selection and solution conditions influence the apparent photoreactivity of environmental waters and confirms that 3 DOM or 1 O 2 probes cannot be used interchangeably in waters that vary in [DOC], pH, or DOM source.

Real-time single-molecule observations of proteins at the solid-liquid interface

NASA Astrophysics Data System (ADS)

Langdon, Blake Brianna

Non-specific protein adsorption to solid surfaces is pervasive and observed across a broad spectrum of applications including biomaterials, separations, pharmaceuticals, and biosensing. Despite great interest in and considerable literature dedicated to the phenomena, a mechanistic understanding of this complex phenomena is lacking and remains controversial, partially due to the limits of ensemble-averaging techniques used to study it. Single-molecule tracking (SMT) methods allow us to study distinct protein dynamics (e.g. adsorption, desorption, diffusion, and intermolecular associations) on a molecule-by-molecule basis revealing the protein population and spatial heterogeneity inherent in protein interfacial behavior. By employing single-molecule total internal reflection fluorescence microscopy (SM-TIRFM), we have developed SMT methods to directly observe protein interfacial dynamics at the solid-liquid interface to build a better mechanistic understanding of protein adsorption. First, we examined the effects of surface chemistry (e.g. hydrophobicity, hydrogen-bonding capacity), temperature, and electrostatics on isolated protein desorption and interfacial diffusion for fibrinogen (Fg) and bovine serum albumin (BSA). Next, we directly and indirectly probed the effects of protein-protein interactions on interfacial desorption, diffusion, aggregation, and surface spatial heterogeneity on model and polymeric thin films. These studies provided many useful insights into interfacial protein dynamics including the following observations. First, protein adsorption was reversible, with the majority of proteins desorbing from all surface chemistries within seconds. Isolated protein-surface interactions were relatively weak on both hydrophobic and hydrophilic surfaces (apparent desorption activation energies of only a few kBT). However, proteins could dynamically and reversibly associate at the interface, and these interfacial associations led to proteins remaining on the surface for longer time intervals. Surface chemistry and surface spatial heterogeneity (i.e. surface sites with different binding strengths) were shown to influence adsorption, desorption, and interfacial protein-protein associations. For example, faster protein diffusion on hydrophobic surfaces increased protein-protein associations and, at higher protein surface coverage, led to proteins remaining on hydrophobic surfaces longer than on hydrophilic surfaces. Ultimately these studies suggested that surface properties (chemistry, heterogeneity) influence not only protein-surface interactions but also interfacial mobility and protein-protein associations, implying that surfaces that better control protein adsorption can be designed by accounting for these processes.

Monitoring solute interactions with poly(ethylene oxide)-modified colloidal silica nanoparticles via fluorescence anisotropy decay.

PubMed

Tleugabulova, Dina; Duft, Andy M; Brook, Michael A; Brennan, John D

2004-01-06

The fluorescence-based nanosize metrology approach, proposed recently by Geddes and Birch (Geddes, C. D.; Birch, D. J. S. J. Non-Cryst. Solids 2000, 270, 191), was used to characterize the extent of binding of a fluorescent cationic solute, rhodamine 6G (R6G), to the surface of silica particles after modification of the surface with the hydrophilic polymer poly(ethylene oxide) (PEO) of various molecular weights. The measurement of the rotational dynamics of R6G in PEO solutions showed the absence of strong interactions between R6G and PEO chains in water and the ability of the dye to sense the presence of polymer clusters in 30 wt % solutions. Time-resolved anisotropy decays of polymer-modified Ludox provided direct evidence for distribution of the dye between bound and free states, with the bound dye showing two decay components: a nanosecond decay component that is consistent with local motions of bound probes and a residual anisotropy component due to slow rotation of large silica particles. The data showed that the dye was strongly adsorbed to unmodified silica nanoparticles, to the extent that less than 1% of the dye was present in the surrounding aqueous solution. Addition of PEO blocked the adsorption of the dye to a significant degree, with up to 50% of the probe being present in the aqueous solution for Ludox samples containing 30 wt % of low molecular weight PEO. The addition of such agents also decreased the value and increased the fractional contribution of the nanosecond rotational correlation time, suggesting that polymer adsorption altered the degree of local motion of the bound probe. Atomic force microscopy imaging studies provided no evidence for a change in the particle size upon surface modification but did suggest interparticle aggregation after polymer adsorption. Thus, this redistribution of the probe is interpreted as being due to coverage of particles with the polymer, resulting in lower adsorption of R6G to the silica. The data clearly show the power of time-resolved fluorescence anisotropy decay measurements for probing the modification of silica surfaces and suggest that this method should prove useful in characterization of new chromatographic stationary phases and nanocomposite materials.

Colloidal silica films for high-capacity DNA arrays

NASA Astrophysics Data System (ADS)

Glazer, Marc Irving

The human genome project has greatly expanded the amount of genetic information available to researchers, but before this vast new source of data can be fully utilized, techniques for rapid, large-scale analysis of DNA and RNA must continue to develop. DNA arrays have emerged as a powerful new technology for analyzing genomic samples in a highly parallel format. The detection sensitivity of these arrays is dependent on the quantity and density of immobilized probe molecules. We have investigated substrates with a porous, "three-dimensional" surface layer as a means of increasing the surface area available for the synthesis of oligonucleotide probes, thereby increasing the number of available probes and the amount of detectable bound target. Porous colloidal silica films were created by two techniques. In the first approach, films were deposited by spin-coating silica colloid suspensions onto flat glass substrates, with the pores being formed by the natural voids between the solid particles (typically 23nm pores, 35% porosity). In the second approach, latex particles were co-deposited with the silica and then pyrolyzed, creating films with larger pores (36 nm), higher porosity (65%), and higher surface area. For 0.3 mum films, enhancements of eight to ten-fold and 12- to 14-fold were achieved with the pure silica films and the films "templated" with polymer latex, respectively. In gene expression assays for up to 7,000 genes using complex biological samples, the high-capacity films provided enhanced signals and performed equivalently or better than planar glass on all other functional measures, confirming that colloidal silica films are a promising platform for high-capacity DNA arrays. We have also investigated the kinetics of hybridization on planar glass and high-capacity substrates. Adsorption on planar arrays is similar to ideal Langmuir-type adsorption, although with an "overshoot" at high solution concentration. Hybridization on high-capacity films is controlled by traditional adsorption (ka) and desorption (kd) coefficients, as well as morphology factors and transient binding interactions between the target and probes. The strength of the transient probe/target binding interactions are on the order of 5--7 DNA base pairs, which suggests the formation of nucleation or other metastable complexes, rather than fully-zippered duplexes.

Probing the effects of surface hydrophobicity and tether orientation on antibody-antigen binding

NASA Astrophysics Data System (ADS)

Bush, Derek B.; Knotts, Thomas A.

2017-04-01

Antibody microarrays have the potential to revolutionize molecular detection for many applications, but their current use is limited by poor reliability, and efforts to change this have not yielded fruitful results. One difficulty which limits the rational engineering of next-generation devices is that little is known, at the molecular level, about the antibody-antigen binding process near solid surfaces. Atomic-level structural information is scant because typical experimental techniques (X-ray crystallography and NMR) cannot be used to image proteins bound to surfaces. To overcome this limitation, this study uses molecular simulation and an advanced, experimentally validated, coarse-grain, protein-surface model to compare fab-lysozyme binding in bulk solution and when the fab is tethered to hydrophobic and hydrophilic surfaces. The results show that the tether site in the fab, as well as the surface hydrophobicity, significantly impacts the binding process and suggests that the optimal design involves tethering fabs upright on a hydrophilic surface. The results offer an unprecedented, molecular-level picture of the binding process and give hope that the rational design of protein-microarrays is possible.

CO2 sorption on surface-modified carbonaceous support: Probing the influence of the carbon black microporosity and surface polarity

NASA Astrophysics Data System (ADS)

Gargiulo, Valentina; Alfè, Michela; Ammendola, Paola; Raganati, Federica; Chirone, Riccardo

2016-01-01

The use of solid sorbents is a convenient option in post-combustion CO2 capture strategies. Sorbents selection is a key point because the materials are required to be both low-cost and versatile in typical post-combustion conditions in order to guarantee an economically advantageous overall process. This work compares strategies to tailor the chemico-physical features of carbon black (CB) by surface-modification and/or coating with a CO2-sorbent phase. The influence of the CB microporosity, enhanced by chemical/thermal treatments, is also taken into account. Three CB surface modifications are performed and compared: (i) oxidation and functionalization with amino-groups, (ii) coating with iron oxides and (iii) impregnation with an ionic liquid (IL). The CO2 capture performance is evaluated on the basis of the breakthrough curves measured at atmospheric pressure and room temperature in a lab-scale fixed bed micro-reactor. Most of tested solids adsorb a CO2 amount significantly higher than a 13X zeolite and DARCO FGD (Norit) activated carbon (up to 4 times more in the best case). The sorbents bearing basic functionalities (amino-groups and IL) exhibit the highest CO2 sorption capacity. The use of a microporous carbonaceous support limits the accessibility of CO2 toward the adsorbing phase (IL or FM) lowering the number of accessible binding sites for CO2.

Observation of NMR noise from solid samples.

PubMed

Schlagnitweit, Judith; Dumez, Jean-Nicolas; Nausner, Martin; Jerschow, Alexej; Elena-Herrmann, Bénédicte; Müller, Norbert

2010-11-01

We demonstrate that proton NMR noise signals, i.e. NMR spectra without excitation by radio frequency, can be obtained from solid samples. Experimental results are shown for static and magic-angle spinning conditions. In addition, a tuning procedure based on the probes' NMR noise characteristics and similar to the one described previously for liquids probes can also be used to optimize signal-to-noise ratios in ¹H-MAS experiments. Copyright © 2010 Elsevier Inc. All rights reserved.

Analysis of non-contact and contact probe-to-sample thermal exchange for quantitative measurements of thin film and nanostructure thermal conductivity by the scanning hot probe method

NASA Astrophysics Data System (ADS)

Wilson, Adam A.

The ability to measure thermal properties of thin films and nanostructured materials is an important aspect of many fields of academic study. A strategy especially well-suited for nanoscale investigations of these properties is the scanning hot probe technique, which is unique in its ability to non-destructively interrogate the thermal properties with high resolution, both laterally as well as through the thickness of the material. Strategies to quantitatively determine sample thermal conductivity depend on probe calibration. State of the art calibration strategies assume that the area of thermal exchange between probe and sample does not vary with sample thermal conductivity. However, little investigation has gone into determining whether or not that assumption is valid. This dissertation provides a rigorous study into the probe-to-sample heat transfer through the air gap at diffusive distances for a variety of values of sample thermal conductivity. It is demonstrated that the thermal exchange radius and gap/contact thermal resistance varies with sample thermal conductivity as well as tip-to-sample clearance in non-contact mode. In contact mode, it is demonstrated that higher thermal conductivity samples lead to a reduction in thermal exchange radius for Wollaston probe tips. Conversely, in non-contact mode and in contact mode for sharper probe tips where air contributes the most to probe-to-sample heat transfer, the opposite trend occurs. This may be attributed to the relatively strong solid-to-solid conduction occurring between probe and sample for the Wollaston probes. A three-dimensional finite element (3DFE) model was developed to investigate how the calibrated thermal exchange parameters vary with sample thermal conductivity when calibrating the probe via the intersection method in non-contact mode at diffusive distances. The 3DFE model was then used to explore the limits of sensitivity of the experiment for a range of simulated experimental conditions. It is determined that, when operating the scanning hot probe technique in air at standard temperature and pressure using Wollaston probes, the technique is capable of measuring, within 20% uncertainty, samples with values of thermal conductivity up to 10 Wm-1K-1 in contact mode and up to 2 Wm-1K-1 in non-contact mode. By increasing the thermal conductivity of the probe's surroundings (i.e. changing air to a more conductive gas), sensitivity in non-contact mode to sample thermal conductivity is improved, which suggests potential for future investigations using non-contact scanning hot probe to measure thermal conductivity of higher thermal conductivity samples. The ability of the technique to differentiate thin films from the substrate is investigated, and the sensitivity of the technique to thin films and samples with anisotropic properties is explored. The models (both analytical and finite element) developed and reported in this dissertation lead to the ability to measure samples which, by the standard procedure before this work, were unable to be accurately measured. While other techniques failed to be able to successfully interrogate the film thermal conductivity of a full set of double-wall carbon nanotubes infused into polymers, the methods developed in this work allowed non-contact scanning hot probe measurements to be successfully performed to obtain the film thermal conductivity for each sample. Finite element simulations accounting for the anisotropy of these thin film on sample materials show similar trends with independently measured in-plane thermal conductivity for the only two (of five) samples in the set which were successfully able to be measured by the independent technique. Investigations in contact mode with high resolution Pd probes, whose probe-to-sample clearance is difficult to control in a repeatable fashion, show that surface roughness affects the thermal contact resistance. This can lead to values of reported sample thermal conductivity which are misleading, when using the standard calibrated thermal exchange parameters on samples with significantly different surface roughness than the calibration samples. This affect was taken into account to report sample thermal conductivity of Bi2Te3 nanoflakes.

(99m)Tc-amitrole as a novel selective imaging probe for solid tumor: In silico and preclinical pharmacological study.

PubMed

Essa, B M; Sakr, T M; Khedr, Mohammed A; El-Essawy, F A; El-Mohty, A A

2015-08-30

Lactoperoxidase (LPO) inhibitors are very selective for solid tumor due to their high binding affinity to the LPO enzyme. A computational study was used to select top-ranked LPO inhibitor (alone and in complex with (99m)Tc) with high in silico affinity. The novel prepared (99m)Tc-amitrole complex demonstrated both in silico and in vivo high affinity toward solid tumors.(99m)Tc-amitrole was radio-synthesized with a high radiochemical yield (89.7±3.25). It showed in vitro stability for up to 6h. Its preclinical evaluation in solid tumor-bearing mice showed high retention and biological accumulation in solid tumor cells with a high Target/Non-Target (T/NT) ratio equal to 4.9 at 60min post-injection. The data described previously could recommend (99m)Tc-amitrole as potential targeting scintigraphic probe for solid tumor imaging. Copyright © 2015 Elsevier B.V. All rights reserved.

Toward a solid-phase nucleic acid hybridization assay within microfluidic channels using immobilized quantum dots as donors in fluorescence resonance energy transfer.

PubMed

Chen, Lu; Algar, W Russ; Tavares, Anthony J; Krull, Ulrich J

2011-01-01

The optical properties and surface area of quantum dots (QDs) have made them an attractive platform for the development of nucleic acid biosensors based on fluorescence resonance energy transfer (FRET). Solid-phase assays based on FRET using mixtures of immobilized QD-oligonucleotide conjugates (QD biosensors) have been developed. The typical challenges associated with solid-phase detection strategies include non-specific adsorption, slow kinetics of hybridization, and sample manipulation. The new work herein has considered the immobilization of QD biosensors onto the surfaces of microfluidic channels in order to address these challenges. Microfluidic flow can be used to dynamically control stringency by adjustment of the potential in an electrokinetic-based microfluidics environment. The shearing force, Joule heating, and the competition between electroosmotic and electrophoretic mobilities allow the optimization of hybridization conditions, convective delivery of target to the channel surface to speed hybridization, amelioration of adsorption, and regeneration of the sensing surface. Microfluidic flow can also be used to deliver (for immobilization) and remove QD biosensors. QDs that were conjugated with two different oligonucleotide sequences were used to demonstrate feasibility. One oligonucleotide sequence on the QD was available as a linker for immobilization via hybridization with complementary oligonucleotides located on a glass surface within a microfluidic channel. A second oligonucleotide sequence on the QD served as a probe to transduce hybridization with target nucleic acid in a sample solution. A Cy3 label on the target was excited by FRET using green-emitting CdSe/ZnS QD donors and provided an analytical signal to explore this detection strategy. The immobilized QDs could be removed under denaturing conditions by disrupting the duplex that was used as the surface linker and thus allowed a new layer of QD biosensors to be re-coated within the channel for re-use of the microfluidic chip.

Laser-based linear and nonlinear guided elastic waves at surfaces (2D) and wedges (1D).

PubMed

Hess, Peter; Lomonosov, Alexey M; Mayer, Andreas P

2014-01-01

The characteristic features and applications of linear and nonlinear guided elastic waves propagating along surfaces (2D) and wedges (1D) are discussed. Laser-based excitation, detection, or contact-free analysis of these guided waves with pump-probe methods are reviewed. Determination of material parameters by broadband surface acoustic waves (SAWs) and other applications in nondestructive evaluation (NDE) are considered. The realization of nonlinear SAWs in the form of solitary waves and as shock waves, used for the determination of the fracture strength, is described. The unique properties of dispersion-free wedge waves (WWs) propagating along homogeneous wedges and of dispersive wedge waves observed in the presence of wedge modifications such as tip truncation or coatings are outlined. Theoretical and experimental results on nonlinear wedge waves in isotropic and anisotropic solids are presented. Copyright © 2013 Elsevier B.V. All rights reserved.

A Novel Method for Rapid Hybridization of DNA to a Solid Support

PubMed Central

Pettersson, Erik; Ahmadian, Afshin; Ståhl, Patrik L.

2013-01-01

Here we present a novel approach entitled Magnetic Forced Hybridization (MFH) that provides the means for efficient and direct hybridization of target nucleic acids to complementary probes immobilized on a glass surface in less than 15 seconds at ambient temperature. In addition, detection is carried out instantly since the beads become visible on the surface. The concept of MFH was tested for quality control of array manufacturing, and was combined with a multiplex competitive hybridization (MUCH) approach for typing of Human Papilloma Virus (HPV). Magnetic Forced Hybridization of bead-DNA constructs to a surface achieves a significant reduction in diagnostic testing time. In addition, readout of results by visual inspection of the unassisted eye eliminates the need for additional expensive instrumentation. The method uses the same set of beads throughout the whole process of manipulating and washing DNA constructs prior to detection, as in the actual detection step itself. PMID:23950946

Shallow Heavily Doped n++ Germanium by Organo-Antimony Monolayer Doping.

PubMed

Alphazan, Thibault; Díaz Álvarez, Adrian; Martin, François; Grampeix, Helen; Enyedi, Virginie; Martinez, Eugénie; Rochat, Névine; Veillerot, Marc; Dewitte, Marc; Nys, Jean-Philippe; Berthe, Maxime; Stiévenard, Didier; Thieuleux, Chloé; Grandidier, Bruno

2017-06-14

Functionalization of Ge surfaces with the aim of incorporating specific dopant atoms to form high-quality junctions is of particular importance for the development of solid-state devices. In this study, we report the shallow doping of Ge wafers with a monolayer doping strategy that is based on the controlled grafting of Sb precursors and the subsequent diffusion of Sb into the wafer upon annealing. We also highlight the key role of citric acid in passivating the surface before its reaction with the Sb precursors and the benefit of a protective SiO 2 overlayer that enables an efficient incorporation of Sb dopants with a concentration higher than 10 20 cm -3 . Microscopic four-point probe measurements and photoconductivity experiments show the full electrical activation of the Sb dopants, giving rise to the formation of an n++ Sb-doped layer and an enhanced local field-effect passivation at the surface of the Ge wafer.

Neutron reflectivity measurement of protein A-antibody complex at the solid-liquid interface.

PubMed

Mazzer, Alice R; Clifton, Luke A; Perevozchikova, Tatiana; Butler, Paul D; Roberts, Christopher J; Bracewell, Daniel G

2017-05-26

Chromatography is a ubiquitous unit operation in the purification of biopharmaceuticals yet few studies have addressed the biophysical characterisation of proteins at the solution-resin interface. Chromatography and other adsorption and desorption processes have been shown to induce protein aggregation which is undesirable in biopharmaceutical products. In order to advance understanding of how adsorption processes might impact protein stability, neutron reflectivity was used to characterise the structure of adsorbed immunoglobulin G (IgG) on model surfaces. In the first model system, IgG was adsorbed directly to silica and demonstrated a side-on orientation with high surface contact. A maximum dimension of 60Å in the surface normal direction and high density surface coverage were observed under pH 4.1 conditions. In chromatography buffers, pH was found to influence IgG packing density and orientation at the solid-liquid interface. In the second model system, which was designed to mimic an affinity chromatography surface, protein A was attached to a silica surface to produce a configuration representative of a porous glass chromatography resin. Interfacial structure was probed during sequential stages from ligand attachment, through to IgG binding and elution. Adsorbed IgG structures extended up to 250Å away from the surface and showed dependence on surface blocking strategies. The data was suggestive of two IgG molecules bound to protein A with a somewhat skewed orientation and close proximity to the silica surface. The findings provide insight into the orientation of adsorbed antibody structures under conditions encountered during chromatographic separations. Copyright © 2017 The Author(s). Published by Elsevier B.V. All rights reserved.

Biofilm formation and potential for iron cycling in serpentinization-influenced groundwater of the Zambales and Coast Range ophiolites.

PubMed

Meyer-Dombard, D'Arcy R; Casar, Caitlin P; Simon, Alexander G; Cardace, Dawn; Schrenk, Matthew O; Arcilla, Carlo A

2018-05-01

Terrestrial serpentinizing systems harbor microbial subsurface life. Passive or active microbially mediated iron transformations at alkaline conditions in deep biosphere serpentinizing ecosystems are understudied. We explore these processes in the Zambales (Philippines) and Coast Range (CA, USA) ophiolites, and associated surface ecosystems by probing the relevance of samples acquired at the surface to in situ, subsurface ecosystems, and the nature of microbe-mineral associations in the subsurface. In this pilot study, we use microcosm experiments and batch culturing directed at iron redox transformations to confirm thermodynamically based predictions that iron transformations may be important in subsurface serpentinizing ecosystems. Biofilms formed on rock cores from the Zambales ophiolite on surface and in-pit associations, confirming that organisms from serpentinizing systems can form biofilms in subsurface environments. Analysis by XPS and FTIR confirmed that enrichment culturing utilizing ferric iron growth substrates produced reduced, magnetic solids containing siderite, spinels, and FeO minerals. Microcosms and enrichment cultures supported organisms whose near relatives participate in iron redox transformations. Further, a potential 'principal' microbial community common to solid samples in serpentinizing systems was identified. These results indicate collectively that iron redox transformations should be more thoroughly and universally considered when assessing the function of terrestrial subsurface ecosystems driven by serpentinization.

AFM fluid delivery/liquid extraction surface sampling/electrostatic spray cantilever probe

DOEpatents

Van Berkel, Gary J.

2015-06-23

An electrospray system comprises a liquid extraction surface sampling probe. The probe comprises a probe body having a liquid inlet and a liquid outlet, and having a liquid extraction tip. A solvent delivery conduit is provided for receiving solvent liquid from the liquid inlet and delivering the solvent liquid to the liquid extraction tip. An open liquid extraction channel extends across an exterior surface of the probe body from the liquid extraction tip to the liquid outlet. An electrospray emitter tip is in liquid communication with the liquid outlet of the liquid extraction surface sampling probe. A system for analyzing samples, a liquid junction surface sampling system, and a method of analyzing samples are also disclosed.

Acoustic Probe for Solid-Gas-Liquid Suspension

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

Tavlarides, L.L.; Sangani, Ashok

The primary objective of the research project during the first funding period was to develop an acoustic probe to measure volume percent solids in solid-liquid slurries in the presence of small amounts of gas bubbles. This problem was addressed because of the great need for a non-invasive, accurate and reliable method for solids monitoring in liquid slurries in the presence of radiolytically generated gases throughout the DOE complex. These measurements are necessary during mobilization of salts and sediments in tanks, transport of these slurries in transfer lines to processing facilities across a site, and, in some instances, during high levelmore » waste processing. Although acoustic probes have been commonly used for monitoring flows in single-phase fluids (McLeod, 1967), their application to monitor two-phase mixtures has not yet fully realized its potential. A number of investigators in recent years have therefore been involved in developing probes for measuring the volume fractions in liquid solid suspensions (Atkinson and Kytomaa, 1993; Greenwood et al., 1993; Martin et al., 1995) and in liquid-liquid suspensions (Bonnet and Tavlarides, 1987; Tavlarides and Bonnet, 1988, Yi and Tavlarides, 1990; Tsouris and Tavlarides, 1993, Tsouris et al., 1995). In particular, Atkinson and Kytomaa (1993) showed that the acoustic technique can be used to determine both the velocity and the volume fraction of solids while Martin et al. (1995) and Spelt et al. (1999) showed that the acoustic probe can also be used to obtain information on the size distribution of the particles. In a recent testing of in-line slurry monitors with radioactive slurries suspended with Pulsair Mixers (Hylton & Bayne, 1999), an acoustic probe did not compare well with other instruments most probably due to presence of entrained gases and improper acoustic frequency range of interrogation. The work of the investigators cited has established the potential of the acoustic probe for characterizing/monitoring two-phase flows in relatively ideal, well-characterized suspensions. Two major factors which we judge has prevented its wide-spread use in the processing industry, particularly for dilute suspensions, is careful selection of the frequency range for interrogation and quantification and removal of the noise introduced by bubbles from the acoustic signal obtained from the suspension. Our research during the first funding period to develop an acoustic probe for solid-gas liquid suspensions has resulted in a theory, supported by our experiments, to describe small amplitude dilute suspensions (Norato, 1999, Spelt et al., 1999, Spelt et al., 2001). The theory agrees well with experimental data of sound attenuation up to 45 {approx}01% suspensions of 0.11 and 77 micron radius polystyrene particles in water and 0.4 to 40 vol %, suspensions of 32 micron soda-lime glass particles in water. Also, analyses of our attenuation experiments for solid-gas liquid experiments suggest the theory can be applied to correct for signal interference due to the presence of bubbles over a selected frequency range to permit determination of the solid-liquid volume fraction. Further, we show experimentally that a reliable linear dependency of weight percent solids with attenuation is obtained for low weight fractions at high frequencies of interrogation where bubble interference is minimal. There was a collaborative effort during the first funding period with the Pacific Northwest National Laboratories in that Dr. Margaret Greenwood was a co-investigator on the project. Dr. Greenwood provided a high level of experimental knowledge and techniques on ultrasound propagation, measurement and data processing. During the second funding period the slurry test loop at Oak Ridge National Laboratories under the direction of Mr. Tom Hylton will be employed to demonstrate the measurement capabilities of the prototype acoustic monitor.« less

In-line gas chromatographic apparatus for measuring the hydrophobic micropore volume (HMV) and contaminant transformation in mineral micropores.

PubMed

Cheng, Hefa; Reinhard, Martin

2010-07-15

Desorption of hydrophobic organic compounds from micropores is characteristically slow compared to surface adsorption and partitioning. The slow-desorbing mass of a hydrophobic probe molecule can be used to calculate the hydrophobic micropore volume (HMV) of microporous solids. A gas chromatographic apparatus is described that allows characterization of the sorbed mass with respect to the desorption rate. The method is demonstrated using a dealuminated zeolite and an aquifer sand as the model and reference sorbents, respectively, and trichloroethylene (TCE) as the probe molecule. A glass column packed with the microporous sorbent is coupled directly to a gas chromatograph that is equipped with flame ionization and electron capture detectors. Sorption and desorption of TCE on the sorbent was measured by sampling the influent and effluent of the column using a combination of switching and injection valves. For geosorbents, the HMV is quantified based on Gurvitsch's rule from the mass of TCE desorbed at a rate that is characteristic for micropores. Instrumental requirements, design considerations, hardware details, detector calibration, performance, and data analysis are discussed along with applications. The method is novel and complements traditional vacuum gravimetric and piezometric techniques, which quantify the total pore volume under vacuum conditions. The HMV is more relevant than the total micropore volume for predicting the fate and transport of organic contaminants in the subsurface. Sorption in hydrophobic micropores strongly impacts the mobility of organic contaminants, and their chemical and biological transformations. The apparatus can serve as a tool for characterizing microporous solids and investigating contaminant-solid interactions. 2010 Elsevier B.V. All rights reserved.

Insights into electrode/electrolyte interfacial processes and the effect of nanostructured cobalt oxides loading on graphene-based hybrids by scanning electrochemical microscopy

NASA Astrophysics Data System (ADS)

Gupta, Sanju; Carrizosa, Sara B.

2016-12-01

Nanostructured cobalt oxide polymorphs (CoO and Co3O4) deposited via electrodeposition allowed optimal loading on supercapacitive graphene nanosheets producing a set of graphene-based hybrids namely, CoO/GO, CoO/ErGO, Co3O4/GO, Co3O4/rGO, and Co3O4/ErGO, as pseudocapacitive electrochemical electrodes. We gained fundamental insights into the complex physicochemical interfacial processes at electrode surfaces and electrode/electrolyte (or solid/liquid) interfaces by scanning electrochemical microscopy operating in the feedback probe approach and imaging modes while monitoring and mapping the redox probe (re)activity behavior. We determined the various experimental descriptors including diffusion coefficient, electron transfer rate, and electroactive site distribution on electrodes. We emphasize the interplay of (1) heterogeneous basal and edge plane active sites, (2) graphene surface functional moieties (conducting/semiconducting), and (3) crystalline spinel cobalt oxides (semiconducting/insulating) coated graphene, reinforcing the available electron density of states in the vicinity of the Fermi level contributing to higher electroactivity, faster interfacial diffusion, and shorter distances for electron transfer, facilitated through molecular and chemical bridges obtained by electrodeposition as compared with the physical deposition.

Tuning the ultrafast photodissociation dynamics of CH3Br on ultrathin MgO films by reducing the layer thickness to the 2D limit

NASA Astrophysics Data System (ADS)

Vaida, Mihai E.; Bernhardt, Thorsten M.

2017-11-01

The femtosecond-laser induced photodissociation of CH3Br adsorbed at sub-monolayer coverage on a solid surface was investigated by time-resolved pump-probe mass spectrometry. To tune the interaction of the CH3Br molecules with the substrate, an Mo(1 0 0) surface was covered with ultrathin insulating MgO layers of variable thickness. By gradually decreasing the magnesia layer thickness to the 2D limit the photodissociation dynamics observed by detection of the methyl fragment indicates an energetic lowering of the relevant methyl bromide excited states due to the increasing spatial proximity of the metallic support. Potential orientational effects of the methyl bromide adsorption geometry are also considered.

Tailoring bifunctional hybrid organic–inorganic nanoadsorbents by the choice of functional layer composition probed by adsorption of Cu2+ ions

PubMed Central

Tomina, Veronika V; Melnyk, Inna V; Zub, Yuriy L; Kareiva, Aivaras; Vaclavikova, Miroslava; Kessler, Vadim G

2017-01-01

Spherical silica particles with bifunctional (≡Si(CH2)3NH2/≡SiCH3, ≡Si(CH2)3NH2/≡Si(CH2)2(CF2)5CF3) surface layers were produced by a one-step approach using a modified Stöber method in three-component alkoxysilane systems, resulting in greatly increased contents of functional components. The content of functional groups and thermal stability of the surface layers were analyzed by diffuse reflectance infrared Fourier transform (DRIFT) spectroscopy, and 13C and 29Si solid-state NMR spectroscopy revealing their composition and organization. The fine chemical structure of the surface in the produced hybrid adsorbent particles and the ligand distribution were further investigated by electron paramagnetic resonance (EPR) and electron spectroscopy of diffuse reflectance (ESDR) spectroscopy using Cu2+ ion coordination as a probe. The composition and structure of the emerging surface complexes were determined and used to provide an insight into the molecular structure of the surfaces. It was demonstrated that the introduction of short hydrophobic (methyl) groups improves the kinetic characteristics of the samples during the sorption of copper(II) ions and promotes fixation of aminopropyl groups on the surface of silica microspheres. The introduction of long hydrophobic (perfluoroctyl) groups changes the nature of the surface, where they are arranged in alternately hydrophobic/hydrophilic patches. This makes the aminopropyl groups huddled and less active in the sorption of metal cations. The size and aggregation/morphology of obtained particles was optimized controlling the synthesis conditions, such as concentrations of reactants, basicity of the medium, and the process temperature. PMID:28243572

Brønsted acid sites based on penta-coordinated aluminum species

NASA Astrophysics Data System (ADS)

Wang, Zichun; Jiang, Yijiao; Lafon, Olivier; Trébosc, Julien; Duk Kim, Kyung; Stampfl, Catherine; Baiker, Alfons; Amoureux, Jean-Paul; Huang, Jun

2016-12-01

Zeolites and amorphous silica-alumina (ASA), which both provide Brønsted acid sites (BASs), are the most extensively used solid acid catalysts in the chemical industry. It is widely believed that BASs consist only of tetra-coordinated aluminum sites (AlIV) with bridging OH groups in zeolites or nearby silanols on ASA surfaces. Here we report the direct observation in ASA of a new type of BAS based on penta-coordinated aluminum species (AlV) by 27Al-{1H} dipolar-mediated correlation two-dimensional NMR experiments at high magnetic field under magic-angle spinning. Both BAS-AlIV and -AlV show a similar acidity to protonate probe molecular ammonia. The quantitative evaluation of 1H and 27Al sites demonstrates that BAS-AlV co-exists with BAS-AlIV rather than replaces it, which opens new avenues for strongly enhancing the acidity of these popular solid acids.

Test data from small solid propellant rocket motor plume measurements (FA-21)

NASA Technical Reports Server (NTRS)

Hair, L. M.; Somers, R. E.

1976-01-01

A program is described for obtaining a reliable, parametric set of measurements in the exhaust plumes of solid propellant rocket motors. Plume measurements included pressures, temperatures, forces, heat transfer rates, particle sampling, and high-speed movies. Approximately 210,000 digital data points and 15,000 movie frames were acquired. Measurements were made at points in the plumes via rake-mounted probes, and on the surface of a large plate impinged by the exhaust plume. Parametric variations were made in pressure altitude, propellant aluminum loading, impinged plate incidence angle and distance from nozzle exit to plate or rake. Reliability was incorporated by continual use of repeat runs. The test setup of the various hardware items is described along with an account of test procedures. Test results and data accuracy are discussed. Format of the data presentation is detailed. Complete data are included in the appendix.

Shock wave as a probe of flux-dimited thermal transport in laser-heated solids

NASA Astrophysics Data System (ADS)

Smith, K.; Forsman, A.; Chiu, G.

1996-11-01

Laser-generated shock waves in solids result from the ablation of the target material. Where radiation transport is negligible, the ablation process is dominated by electron thermal conduction. This offers an opportunity to probe the degree of transport inhibition (compared with classical heat flow) for steep temperature gradients in a dense plasma. Using a 1-dimensional hydrodynamic code, we have examined the effect of flux-limited thermal conduction on the amplitude of the resulting shock wave.

Kinetic nanofriction: a mechanism transition from quasi-continuous to ballistic-like Brownian regime

PubMed Central

2012-01-01

Surface diffusion of mobile adsorbates is not only the key to control the rate of dynamical processes on solid surfaces, e.g. epitaxial growth, but also of fundamental importance for recent technological applications, such as nanoscale electro-mechanical, tribological, and surface probing devices. Though several possible regimes of surface diffusion have been suggested, the nanoscale surface Brownian motion, especially in the technologically important low friction regimes, remains largely unexplored. Using molecular dynamics simulations, we show for the first time, that a C60 admolecule on a graphene substrate exhibits two distinct regimes of nanoscale Brownian motion: a quasi-continuous and a ballistic-like. A crossover between these two regimes is realized by changing the temperature of the system. We reveal that the underlying physical origin for this crossover is a mechanism transition of kinetic nanofriction arising from distinctive ways of interaction between the admolecule and the graphene substrate in these two regimes due to the temperature change. Our findings provide insight into surface mass transport and kinetic friction control at the nanoscale. PMID:22353343

Optical second-harmonic diffraction study of anisotropic surface diffusion: CO on Ni(110)

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

Xiao, X.; Zhu, X.D.; Daum, W.

We describe in detail a technique using optical second-harmonic (SH) diffraction from a one-dimensional laser-induced monolayer grating to probe surface diffusion of adsorbates and its anisotropy on a solid surface. The case of CO on Ni(110) is used as a demonstration. The two orthogonal and independent diffusion tensor components along (1{bar 1}0) and (001) are measured, exhibiting a strong anisotropy in both the activation energy {ital E}{sub diff} and the preexponential factor {ital D}{sub 0} in the diffusion coefficients. A compensation effect between {ital E}{sub diff} and {ital D}{sub 0} is observed. In comparison with CO/Ni(111) and CO/Ni(100), our resultmore » suggests that the Ni(110) surface seen by CO is much smoother than Ni(111) and Ni(100). Both advantages and limitations of the present technique are mentioned and possible complications in the data analysis are discussed.« less

Rapid ultrasensitive single particle surface-enhanced Raman spectroscopy using metallic nanopores.

PubMed

Cecchini, Michael P; Wiener, Aeneas; Turek, Vladimir A; Chon, Hyangh; Lee, Sangyeop; Ivanov, Aleksandar P; McComb, David W; Choo, Jaebum; Albrecht, Tim; Maier, Stefan A; Edel, Joshua B

2013-10-09

Nanopore sensors embedded within thin dielectric membranes have been gaining significant interest due to their single molecule sensitivity and compatibility of detecting a large range of analytes, from DNA and proteins, to small molecules and particles. Building on this concept we utilize a metallic Au solid-state membrane to translocate and rapidly detect single Au nanoparticles (NPs) functionalized with 589 dye molecules using surface-enhanced resonance Raman spectroscopy (SERRS). We show that, due to the plasmonic coupling between the Au metallic nanopore surface and the NP, signal intensities are enhanced when probing analyte molecules bound to the NP surface. Although not single molecule, this nanopore sensing scheme benefits from the ability of SERRS to provide rich vibrational information on the analyte, improving on current nanopore-based electrical and optical detection techniques. We show that the full vibrational spectrum of the analyte can be detected with ultrahigh spectral sensitivity and a rapid temporal resolution of 880 μs.

Remote laser evaporative molecular absorption spectroscopy

NASA Astrophysics Data System (ADS)

Hughes, Gary B.; Lubin, Philip; Cohen, Alexander; Madajian, Jonathan; Kulkarni, Neeraj; Zhang, Qicheng; Griswold, Janelle; Brashears, Travis

2016-09-01

We describe a novel method for probing bulk molecular and atomic composition of solid targets from a distant vantage. A laser is used to melt and vaporize a spot on the target. With sufficient flux, the spot temperature rises rapidly, and evaporation of surface materials occurs. The melted spot creates a high-temperature blackbody source, and ejected material creates a plume of surface materials in front of the spot. Molecular and atomic absorption occurs as the blackbody radiation passes through the ejected plume. Bulk molecular and atomic composition of the surface material is investigated by using a spectrometer to view the heated spot through the ejected plume. The proposed method is distinct from current stand-off approaches to composition analysis, such as Laser-Induced Breakdown Spectroscopy (LIBS), which atomizes and ionizes target material and observes emission spectra to determine bulk atomic composition. Initial simulations of absorption profiles with laser heating show great promise for Remote Laser-Evaporative Molecular Absorption (R-LEMA) spectroscopy. The method is well-suited for exploration of cold solar system targets—asteroids, comets, planets, moons—such as from a spacecraft orbiting the target. Spatial composition maps could be created by scanning the surface. Applying the beam to a single spot continuously produces a borehole or trench, and shallow subsurface composition profiling is possible. This paper describes system concepts for implementing the proposed method to probe the bulk molecular composition of an asteroid from an orbiting spacecraft, including laser array, photovoltaic power, heating and ablation, plume characteristics, absorption, spectrometry and data management.

Surface plasmon resonance based fiber optic detection of chlorine utilizing polyvinylpyrolidone supported zinc oxide thin films.

PubMed

Tabassum, Rana; Gupta, Banshi D

2015-03-21

A highly sensitive chlorine sensor for an aqueous medium is fabricated using an optical fiber surface plasmon resonance (OFSPR) system. An OFSPR-based chlorine sensor is designed with a multilayer-type platform by zinc oxide (ZnO) and polyvinylpyrollidone (PVP) film morphology manipulations. Among all the methodologies of transduction reported in the field of solid state chemical and biochemical sensing, our attention is focused on the Kretschmann configuration optical fiber sensing technique using the mechanism of surface plasmon resonance. The optical fiber surface plasmon resonance (SPR) chlorine sensor is developed using a multimode optical fiber with the PVP-supported ZnO film deposited over a silver-coated unclad core of the fiber. A spectral interrogation mode of operation is used to characterize the sensor. In an Ag/ZnO/PVP multilayer system, the absorption of chlorine in the vicinity of the sensing region is performed by the PVP layer and the zinc oxide layer enhances the shift in resonance wavelength. It is, experimentally, demonstrated that the SPR wavelength shifts nonlinearly towards the red side of the visible region with an increase in the chlorine concentration in an aqueous medium while the sensitivity of the sensor decreases linearly with an increase in the chlorine concentration. As the proposed sensor utilizes an optical fiber, it possesses the additional advantages of fiber such as less signal degradation, less susceptibility to electromagnetic interference, possibility of remote sensing, probe miniaturization, probe re-usability, online monitoring, small size, light weight and low cost.

Thin-film fiber optic hydrogen and temperature sensor system

DOEpatents

Nave, Stanley E.

1998-01-01

The invention discloses a sensor probe device for monitoring of hydrogen gas concentrations and temperatures by the same sensor probe. The sensor probe is constructed using thin-film deposition methods for the placement of a multitude of layers of materials sensitive to hydrogen concentrations and temperature on the end of a light transparent lens located within the sensor probe. The end of the lens within the sensor probe contains a lens containing a layer of hydrogen permeable material which excludes other reactive gases, a layer of reflective metal material that forms a metal hydride upon absorbing hydrogen, and a layer of semi-conducting solid that is transparent above a temperature dependent minimum wavelength for temperature detection. The three layers of materials are located at the distal end of the lens located within the sensor probe. The lens focuses light generated by broad-band light generator and connected by fiber-optics to the sensor probe, onto a reflective metal material layer, which passes through the semi-conducting solid layer, onto two optical fibers located at the base of the sensor probe. The reflected light is transmitted over fiberoptic cables to a spectrometer and system controller. The absence of electrical signals and electrical wires in the sensor probe provides for an elimination of the potential for spark sources when monitoring in hydrogen rich environments, and provides a sensor free from electrical interferences.

Thin-film fiber optic hydrogen and temperature sensor system

DOEpatents

Nave, S.E.

1998-07-21

The invention discloses a sensor probe device for monitoring of hydrogen gas concentrations and temperatures by the same sensor probe. The sensor probe is constructed using thin-film deposition methods for the placement of a multitude of layers of materials sensitive to hydrogen concentrations and temperature on the end of a light transparent lens located within the sensor probe. The end of the lens within the sensor probe contains a lens containing a layer of hydrogen permeable material which excludes other reactive gases, a layer of reflective metal material that forms a metal hydride upon absorbing hydrogen, and a layer of semi-conducting solid that is transparent above a temperature dependent minimum wavelength for temperature detection. The three layers of materials are located at the distal end of the lens located within the sensor probe. The lens focuses light generated by broad-band light generator and connected by fiber-optics to the sensor probe, onto a reflective metal material layer, which passes through the semi-conducting solid layer, onto two optical fibers located at the base of the sensor probe. The reflected light is transmitted over fiber optic cables to a spectrometer and system controller. The absence of electrical signals and electrical wires in the sensor probe provides for an elimination of the potential for spark sources when monitoring in hydrogen rich environments, and provides a sensor free from electrical interferences. 3 figs.

Scanning Surface Potential Microscopy of Spore Adhesion on Surfaces

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

Lee, Ida; Chung, Eunhyea; Kweon, Hyojin

2012-01-01

The adhesion of spores of Bacillus anthracis - the cause of anthrax and a likely biological threat - to solid surfaces is an important consideration in cleanup after an accidental or deliberate release. However, because of safety concerns, directly studying B. anthracis spores with advanced instrumentation is problematic. As a first step, we are examining the electrostatic potential of Bacillus thuringiensis (Bt), which is a closely related species that is often used as a simulant to study B. anthracis. Scanning surface potential microscopy (SSPM), also known as Kelvin probe force microscopy (KPFM), was used to investigate the influence of relativemore » humidity (RH) on the surface electrostatic potential of Bt that had adhered to silica, mica, or gold substrates. AFM/SSPM side-by-side images were obtained separately in air, at various values of RH, after an aqueous droplet with spores was applied on each surface and allowed to dry before measurements. In the SSPM images, a negative potential on the surface of the spores was observed compared with that of the substrates. The surface potential decreased as the humidity increased. Spores were unable to adhere to a surface with an extremely negative potential, such as mica.« less

Understanding Intense Laser Interactions with Solid Density Plasma

DTIC Science & Technology

2017-01-04

obtain the time-dependent diffraction efficiency. Further improvements may lead to femtosecond temporal resolution, with negligible pump-probe jitter...with negligible pump-probe jitter being possible with future laser- wakefield-accelerator ultrafast-electron-diffraction schemes. Distribution

Water: a responsive small molecule.

PubMed

Shultz, Mary Jane; Vu, Tuan Hoang; Meyer, Bryce; Bisson, Patrick

2012-01-17

Unique among small molecules, water forms a nearly tetrahedral yet flexible hydrogen-bond network. In addition to its flexibility, this network is dynamic: bonds are formed or broken on a picosecond time scale. These unique features make probing the local structure of water challenging. Despite the challenges, there is intense interest in developing a picture of the local water structure due to water's fundamental importance in many fields of chemistry. Understanding changes in the local network structure of water near solutes likely holds the key to unlock problems from analyzing parameters that determine the three dimensional structure of proteins to modeling the fate of volatile materials released into the atmosphere. Pictures of the local structure of water are heavily influenced by what is known about the structure of ice. In hexagonal I(h) ice, the most stable form of solid water under ordinary conditions, water has an equal number of donor and acceptor bonds; a kind of symmetry. This symmetric tetrahedral coordination is only approximately preserved in the liquid. The most obvious manifestation of this altered tetrahedral bonding is the greater density in the liquid compared with the solid. Formation of an interface or addition of solutes further modifies the local bonding in water. Because the O-H stretching frequency is sensitive to the environment, vibrational spectroscopy provides an excellent probe for the hydrogen-bond structure in water. In this Account, we examine both local interactions between water and small solutes and longer range interactions at the aqueous surface. Locally, the results suggest that water is not a symmetric donor or acceptor, but rather has a propensity to act as an acceptor. In interactions with hydrocarbons, action is centered at the water oxygen. For soluble inorganic salts, interaction is greater with the cation than the anion. The vibrational spectrum of the surface of salt solutions is altered compared with that of neat water. Studies of local salt-water interactions suggest that the picture of the local water structure and the ion distribution at the surface deduced from the surface vibrational spectrum should encompass both ions of the salt.

Spatially resolved observation of crystal-face-dependent catalysis by single turnover counting

NASA Astrophysics Data System (ADS)

Roeffaers, Maarten B. J.; Sels, Bert F.; Uji-I, Hiroshi; de Schryver, Frans C.; Jacobs, Pierre A.; de Vos, Dirk E.; Hofkens, Johan

2006-02-01

Catalytic processes on surfaces have long been studied by probing model reactions on single-crystal metal surfaces under high vacuum conditions. Yet the vast majority of industrial heterogeneous catalysis occurs at ambient or elevated pressures using complex materials with crystal faces, edges and defects differing in their catalytic activity. Clearly, if new or improved catalysts are to be rationally designed, we require quantitative correlations between surface features and catalytic activity-ideally obtained under realistic reaction conditions. Transmission electron microscopy and scanning tunnelling microscopy have allowed in situ characterization of catalyst surfaces with atomic resolution, but are limited by the need for low-pressure conditions and conductive surfaces, respectively. Sum frequency generation spectroscopy can identify vibrations of adsorbed reactants and products in both gaseous and condensed phases, but so far lacks sensitivity down to the single molecule level. Here we adapt real-time monitoring of the chemical transformation of individual organic molecules by fluorescence microscopy to monitor reactions catalysed by crystals of a layered double hydroxide immersed in reagent solution. By using a wide field microscope, we are able to map the spatial distribution of catalytic activity over the entire crystal by counting single turnover events. We find that ester hydrolysis proceeds on the lateral {1010} crystal faces, while transesterification occurs on the entire outer crystal surface. Because the method operates at ambient temperature and pressure and in a condensed phase, it can be applied to the growing number of liquid-phase industrial organic transformations to localize catalytic activity on and in inorganic solids. An exciting opportunity is the use of probe molecules with different size and functionality, which should provide insight into shape-selective or structure-sensitive catalysis and thus help with the rational design of new or more productive heterogeneous catalysts.

Probing surface hydrogen bonding and dynamics by natural abundance, multidimensional, 17O DNP-NMR spectroscopy

DOE PAGES

Perras, Frederic A.; Chaudhary, Umesh; Slowing, Igor I.; ...

2016-05-06

Dynamic nuclear polarization (DNP)-enhanced solid-state nuclear magnetic resonance (SSNMR) spectroscopy is increasingly being used as a tool for the atomic-level characterization of surface sites. DNP surface-enhanced SSNMR spectroscopy of materials has, however, been limited to studying relatively receptive nuclei, and the particularly rare 17O nuclide, which is of great interest for materials science, has not been utilized. We demonstrate that advanced 17O SSNMR experiments can be performed on surface species at natural isotopic abundance using DNP. We use 17O DNP surface-enhanced 2D SSNMR to measure 17O{ 1H} HETCOR spectra as well as dipolar oscillations on a series of thermally treatedmore » mesoporous silica nanoparticle samples having different pore diameters. These experiments allow for a nonintrusive and unambiguous characterization of hydrogen bonding and dynamics at the surface of the material; no other single experiment can give such details about the interactions at the surface. Lastly, our data show that, upon drying, strongly hydrogen-bonded surface silanols, whose motions are greatly restricted by the interaction when compared to lone silanols, are selectively dehydroxylated.« less

Method for making a hot wire anemometer and product thereof

NASA Technical Reports Server (NTRS)

Milkulla, V. (Inventor)

1977-01-01

A hot wire anemometer probe is described that includes a ceramic body supporting two conductive rods parallel to each other. The body has a narrow edge surface from which the rods protrude. A probe wire is welded to the rods and extends along the edge surface. A ceramic adhesive is used to secure the probe wire to the surface so that the probe wire is rigid. A method for fabricating the probe is also described in which the body is molded and precisely shaped by machining techniques before the probe wires are installed.

Real-time thermal imaging of solid oxide fuel cell cathode activity in working condition.

PubMed

Montanini, Roberto; Quattrocchi, Antonino; Piccolo, Sebastiano A; Amato, Alessandra; Trocino, Stefano; Zignani, Sabrina C; Faro, Massimiliano Lo; Squadrito, Gaetano

2016-09-01

Electrochemical methods such as voltammetry and electrochemical impedance spectroscopy are effective for quantifying solid oxide fuel cell (SOFC) operational performance, but not for identifying and monitoring the chemical processes that occur on the electrodes' surface, which are thought to be strictly related to the SOFCs' efficiency. Because of their high operating temperature, mechanical failure or cathode delamination is a common shortcoming of SOFCs that severely affects their reliability. Infrared thermography may provide a powerful tool for probing in situ SOFC electrode processes and the materials' structural integrity, but, due to the typical design of pellet-type cells, a complete optical access to the electrode surface is usually prevented. In this paper, a specially designed SOFC is introduced, which allows temperature distribution to be measured over all the cathode area while still preserving the electrochemical performance of the device. Infrared images recorded under different working conditions are then processed by means of a dedicated image processing algorithm for quantitative data analysis. Results reported in the paper highlight the effectiveness of infrared thermal imaging in detecting the onset of cell failure during normal operation and in monitoring cathode activity when the cell is fed with different types of fuels.

Polymer coating behavior of Rayleigh-SAW resonators with gold electrode structure for gas sensor applications.

PubMed

Avramov, Ivan D; Länge, Kerstin; Rupp, Swen; Rapp, Bastian; Rapp, Michael

2007-01-01

Results from systematic polymer coating experiments on surface acoustic wave (SAW) resonators and coupled resonator filters (CRF) on ST-cut quartz with a corrosion-proof electrode structure entirely made of gold (Au) are presented and compared with data from similar SAW devices using aluminium (Al) electrodes. The recently developed Au devices are intended to replace their earlier Al counterparts in sensor systems operating in highly reactive chemical gas environments. Solid parylene C and soft poly[chlorotrifluoroethylene-co-vinylidene fluoride] (PCFV) polymer films are deposited under identical conditions onto the surface of Al and Au devices. The electrical performance of the Parylene C coated devices is monitored online during film deposition. The PCVF coated devices are evaluated after film deposition. The experimental data show that the Au devices can stand up to 40% thicker solid films for the same amount of loss increase than the Al devices and retain better resonance and phase characteristics. The frequency sensitivities of Au and Al devices to parylene C deposition are nearly identical. After coating with soft PCFV sensing film, the Au devices provide up to two times higher gas sensitivity when probed with cooling agent, octane, or tetrachloroethylene.

Paper-based solid-phase multiplexed nucleic acid hybridization assay with tunable dynamic range using immobilized quantum dots as donors in fluorescence resonance energy transfer.

PubMed

Noor, M Omair; Krull, Ulrich J

2013-08-06

A multiplexed solid-phase nucleic acid hybridization assay on a paper-based platform is presented using multicolor immobilized quantum dots (QDs) as donors in fluorescence resonance energy transfer (FRET). The surface of paper was modified with imidazole groups to immobilize two types of QD-probe oligonucleotide conjugates that were assembled in solution. Green-emitting QDs (gQDs) and red-emitting QDs (rQDs) served as donors with Cy3 and Alexa Fluor 647 (A647) acceptors. The gQD/Cy3 FRET pair served as an internal standard, while the rQD/A647 FRET pair served as a detection channel, combining the control and analytical test zones in one physical location. Hybridization of dye-labeled oligonucleotide targets provided the proximity for FRET sensitized emission from the acceptor dyes, which served as an analytical signal. Hybridization assays in the multicolor format provided a limit of detection of 90 fmol and an upper limit of dynamic range of 3.5 pmol. The use of an array of detection zones was designed to provide improved analytical figures of merit compared to that which could be achieved on one type of array design in terms of relative concentration of multicolor QDs. The hybridization assays showed excellent resistance to nonspecific adsorption of oligonucleotides. Selectivity of the two-plex hybridization assay was demonstrated by single nucleotide polymorphism (SNP) detection at a contrast ratio of 50:1. Additionally, it is shown that the use of preformed QD-probe oligonucleotide conjugates and consideration of the relative number density of the two types of QD-probe conjugates in the two-color assay format is advantageous to maximize assay sensitivity and the upper limit of dynamic range.

Probing mass-transport and binding inhomogeneity in macromolecular interactions by molecular interferometric imaging

NASA Astrophysics Data System (ADS)

Zhao, Ming; Wang, Xuefeng; Nolte, David

2009-02-01

In solid-support immunoassays, the transport of target analyte in sample solution to capture molecules on the sensor surface controls the detected binding signal. Depletion of the target analyte in the sample solution adjacent to the sensor surface leads to deviations from ideal association, and causes inhomogeneity of surface binding as analyte concentration varies spatially across the sensor surface. In the field of label-free optical biosensing, studies of mass-transport-limited reaction kinetics have focused on the average response on the sensor surface, but have not addressed binding inhomogeneities caused by mass-transport limitations. In this paper, we employ Molecular Interferometric Imaging (MI2) to study mass-transport-induced inhomogeneity of analyte binding within a single protein spot. Rabbit IgG binding to immobilized protein A/G was imaged at various concentrations and under different flow rates. In the mass-transport-limited regime, enhanced binding at the edges of the protein spots was caused by depletion of analyte towards the center of the protein spots. The magnitude of the inhomogeneous response was a function of analyte reaction rate and sample flow rate.

Art By Don Davis Artist's concept of one of the probes on the hot surface of Venus. Although the

NASA Technical Reports Server (NTRS)

1977-01-01

Art By Don Davis Artist's concept of one of the probes on the hot surface of Venus. Although the probes were not designed to withstand impact, there was a chance that one might survive and transmit some data from the surface. A small probe did survive and transmitted data for 67 minutes.

Simultaneous surface and depth neural activity recording with graphene transistor-based dual-modality probes.

PubMed

Du, Mingde; Xu, Xianchen; Yang, Long; Guo, Yichuan; Guan, Shouliang; Shi, Jidong; Wang, Jinfen; Fang, Ying

2018-05-15

Subdural surface and penetrating depth probes are widely applied to record neural activities from the cortical surface and intracortical locations of the brain, respectively. Simultaneous surface and depth neural activity recording is essential to understand the linkage between the two modalities. Here, we develop flexible dual-modality neural probes based on graphene transistors. The neural probes exhibit stable electrical performance even under 90° bending because of the excellent mechanical properties of graphene, and thus allow multi-site recording from the subdural surface of rat cortex. In addition, finite element analysis was carried out to investigate the mechanical interactions between probe and cortex tissue during intracortical implantation. Based on the simulation results, a sharp tip angle of π/6 was chosen to facilitate tissue penetration of the neural probes. Accordingly, the graphene transistor-based dual-modality neural probes have been successfully applied for simultaneous surface and depth recording of epileptiform activity of rat brain in vivo. Our results show that graphene transistor-based dual-modality neural probes can serve as a facile and versatile tool to study tempo-spatial patterns of neural activities. Copyright © 2018 Elsevier B.V. All rights reserved.

Eddy-Current Inspection of Ball Bearings

NASA Technical Reports Server (NTRS)

Bankston, B.

1985-01-01

Custom eddy-current probe locates surface anomalies. Low friction air cushion within cone allows ball to roll easily. Eddy current probe reliably detects surface and near-surface cracks, voids, and material anomalies in bearing balls or other spherical objects. Defects in ball surface detected by probe displayed on CRT and recorded on strip-chart recorder.

Detection of influenza A virus subtypes using a solid-phase PCR microplate chip assay.

PubMed

Sun, Xin-Cheng; Wang, YunLong; Yang, Liping; Zhang, HuiRu

2015-01-01

A rapid and sensitive microplate chip based on solid PCR was developed to identify influenza A subtypes. A simple ultraviolet cross-linking method was used to immobilize DNA probes on pretreated microplates. Solid-phase PCR was proven to be a convenient method for influenza A screening. The sensitivity of the microplate chip was 10(-3) μg/mL for the enzymatic colorimetric method and 10(-4) μg/mL for the fluorescence method. The 10 sets of primers and probes for the microplate chip were highly specific and did not interfere with each other. These results suggest that the microplate chip based on solid PCR can be used to rapidly detect universal influenza A and its subtypes. This platform can also be used to detect other pathogenic microorganisms. Copyright © 2014 Elsevier B.V. All rights reserved.

Direct Sampling and Analysis from Solid Phase Extraction Cards using an Automated Liquid Extraction Surface Analysis Nanoelectrospray Mass Spectrometry System

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

Walworth, Matthew J; ElNaggar, Mariam S; Stankovich, Joseph J

Direct liquid extraction based surface sampling, a technique previously demonstrated with continuous flow and autonomous pipette liquid microjunction surface sampling probes, has recently been implemented as the Liquid Extraction Surface Analysis (LESA) mode on the commercially available Advion NanoMate chip-based infusion nanoelectrospray ionization system. In the present paper, the LESA mode was applied to the analysis of 96-well format custom solid phase extraction (SPE) cards, with each well consisting of either a 1 or 2 mm diameter monolithic hydrophobic stationary phase. These substrate wells were conditioned, loaded with either single or multi-component aqueous mixtures, and read out using the LESAmore » mode of a TriVersa NanoMate or a Nanomate 100 coupled to an ABI/Sciex 4000QTRAPTM hybrid triple quadrupole/linear ion trap mass spectrometer and a Thermo LTQ XL linear ion trap mass spectrometer. Extraction conditions, including extraction/nanoESI solvent composition, volume, and dwell times, were optimized in the analysis of targeted compounds. Limit of detection and quantitation as well as analysis reproducibility figures of merit were measured. Calibration data was obtained for propranolol using a deuterated internal standard which demonstrated linearity and reproducibility. A 10x increase in signal and cleanup of micromolar Angiotensin II from a concentrated salt solution was demonstrated. Additionally, a multicomponent herbicide mixture at ppb concentration levels was analyzed using MS3 spectra for compound identification in the presence of isobaric interferences.« less

Anionic magnetite nanoparticle conjugated with pyrrolidinyl peptide nucleic acid for DNA base discrimination

NASA Astrophysics Data System (ADS)

Khadsai, Sudarat; Rutnakornpituk, Boonjira; Vilaivan, Tirayut; Nakkuntod, Maliwan; Rutnakornpituk, Metha

2016-09-01

Magnetite nanoparticles (MNPs) were surface modified with anionic poly( N-acryloyl glycine) (PNAG) and streptavidin for specific interaction with biotin-conjugated pyrrolidinyl peptide nucleic acid (PNA). Hydrodynamic size ( D h) of PNAG-grafted MNPs varied from 334 to 496 nm depending on the loading ratio of the MNP to NAG in the reaction. UV-visible and fluorescence spectrophotometries were used to confirm the successful immobilization of streptavidin and PNA on the MNPs. About 291 pmol of the PNA/mg MNP was immobilized on the particle surface. The PNA-functionalized MNPs were effectively used as solid supports to differentiate between fully complementary and non-complementary/single-base mismatch DNA using the PNA probe. These novel anionic MNPs can be efficiently applicable for use as a magnetically guidable support for DNA base discrimination.

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

PubMed

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

2015-02-01

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

Phoenix's 'Dodo' Trench

NASA Technical Reports Server (NTRS)

2008-01-01

This image was taken by NASA's Phoenix Mars Lander's Robotic Arm Camera (RAC) on the ninth Martian day of the mission, or Sol 9 (June 3, 2008). The center of the image shows a trench informally called 'Dodo' after the second dig. 'Dodo' is located within the previously determined digging area, informally called 'Knave of Hearts.' The light square to the right of the trench is the Robotic Arm's Thermal and Electrical Conductivity Probe (TECP). The Robotic Arm has scraped to a bright surface which indicated the Arm has reached a solid structure underneath the surface, which has been seen in other images as well.

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.

Computationally Probing the Performance of Hybrid, Heterogeneous, and Homogeneous Iridium-Based Catalysts for Water Oxidation

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

García-Melchor, Max; Vilella, Laia; López, Núria

2016-04-29

An attractive strategy to improve the performance of water oxidation catalysts would be to anchor a homogeneous molecular catalyst on a heterogeneous solid surface to create a hybrid catalyst. The idea of this combined system is to take advantage of the individual properties of each of the two catalyst components. We use Density Functional Theory to determine the stability and activity of a model hybrid water oxidation catalyst consisting of a dimeric Ir complex attached on the IrO 2(110) surface through two oxygen atoms. We find that homogeneous catalysts can be bound to its matrix oxide without losing significant activity.more » Hence, designing hybrid systems that benefit from both the high tunability of activity of homogeneous catalysts and the stability of heterogeneous systems seems feasible.« less

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

NASA Technical Reports Server (NTRS)

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

2001-01-01

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

Highly Sensitive Detection of Target Biomolecules on Cell Surface Using Gold Nanoparticle Conjugated with Aptamer Probe

NASA Astrophysics Data System (ADS)

Kim, Hyonchol; Terazono, Hideyuki; Hayashi, Masahito; Takei, Hiroyuki; Yasuda, Kenji

2012-06-01

A method of gold nanoparticle (Au NP) labeling with backscattered electron (BE) imaging of field emission scanning electron microscopy (FE-SEM) was applied for specific detection of target biomolecules on a cell surface. A single-stranded DNA aptamer, which specifically binds to the target molecule on a human acute lymphoblastic leukemia cell, was conjugated with a 20 nm Au NP and used as a probe to label its target molecule on the cell. The Au NP probe was incubated with the cell, and the interaction was confirmed using BE imaging of FE-SEM through direct counting of the number of Au NPs attached on the target cell surface. Specific Au NP-aptamer probes were observed on a single cell surface and their spatial distributions including submicron-order localizations were also clearly visualized, whereas the nonspecific aptamer probes were not observed on it. The aptamer probe can be potentially dislodged from the cell surface with treatment of nucleases, indicating that Au NP-conjugated aptamer probes can be used as sensitive and reversible probes to label target biomolecules on cells.

A Modified Alderman-Grant Coil makes possible an efficient cross-coil probe for high field solid-state NMR of lossy biological samples

NASA Astrophysics Data System (ADS)

Grant, Christopher V.; Yang, Yuan; Glibowicka, Mira; Wu, Chin H.; Park, Sang Ho; Deber, Charles M.; Opella, Stanley J.

2009-11-01

The design, construction, and performance of a cross-coil double-resonance probe for solid-state NMR experiments on lossy biological samples at high magnetic fields are described. The outer coil is a Modified Alderman-Grant Coil (MAGC) tuned to the 1H frequency. The inner coil consists of a multi-turn solenoid coil that produces a B 1 field orthogonal to that of the outer coil. This results in a compact nested cross-coil pair with the inner solenoid coil tuned to the low frequency detection channel. This design has several advantages over multiple-tuned solenoid coil probes, since RF heating from the 1H channel is substantially reduced, it can be tuned for samples with a wide range of dielectric constants, and the simplified circuit design and high inductance inner coil provides excellent sensitivity. The utility of this probe is demonstrated on two electrically lossy samples of membrane proteins in phospholipid bilayers (bicelles) that are particularly difficult for conventional NMR probes. The 72-residue polypeptide embedding the transmembrane helices 3 and 4 of the Cystic Fibrosis Transmembrane Conductance Regulator (CFTR) (residues 194-241) requires a high salt concentration in order to be successfully reconstituted in phospholipid bicelles. A second application is to paramagnetic relaxation enhancement applied to the membrane-bound form of Pf1 coat protein in phospholipid bicelles where the resistance to sample heating enables high duty cycle solid-state NMR experiments to be performed.

Electro-Optic Surface Field Imaging System

DTIC Science & Technology

1989-06-01

ELECTRO - OPTIC SURFACE FIELD IMAGING SYSTEM L. E. Kingsley and W. R. Donaldson LABORATORY FOR LASER ENERGETICS University of Rochester 250 East...surface electric fields present during switch operation. The electro - optic , or Pockel’s effect, provides an extremely useful probe of surface electric...fields. Using the electro - optic effect, surface fields can be measured with an optical probe. This paper describes an electro - optic probe which is

Electrospray surface-enhanced Raman spectroscopy (ES-SERS) for probing surface chemical compositions of atmospherically relevant particles

NASA Astrophysics Data System (ADS)

Gen, Masao; Chan, Chak K.

2017-11-01

We present electrospray surface-enhanced Raman spectroscopy (ES-SERS) as a new approach to measuring the surface chemical compositions of atmospherically relevant particles. The surface-sensitive SERS is realized by electrospraying Ag nanoparticle aerosols over analyte particles. Spectral features at v(SO42-), v(C-H) and v(O-H) modes were observed from the normal Raman and SERS measurements of laboratory-generated supermicron particles of ammonium sulfate (AS), AS mixed with succinic acid (AS / SA) and AS mixed with sucrose (AS / sucrose). SERS measurements showed strong interaction (or chemisorption) between Ag nanoparticles and surface aqueous sulfate [SO42-] with [SO42-]AS / sucrose > [SO42-]AS / SA > [SO42-]AS. Enhanced spectra of the solid AS and AS / SA particles revealed the formation of surface-adsorbed water on their surfaces at 60 % relative humidity. These observations of surface aqueous sulfate and adsorbed water demonstrate a possible role of surface-adsorbed water in facilitating the dissolution of sulfate from the bulk phase into its water layer(s). Submicron ambient aerosol particles collected in Hong Kong exhibited non-enhanced features of black carbon and enhanced features of sulfate and organic matter (carbonyl group), indicating an enrichment of sulfate and organic matter on the particle surface.

Surface-enhanced Raman scattering (SERS) dosimeter and probe

DOEpatents

Vo-Dinh, Tuan

1995-01-01

A dosimeter and probe for measuring exposure to chemical and biological compounds is disclosed. The dosimeter or probe includes a collector which may be analyzed by surface-enhanced Raman spectroscopy. The collector comprises a surface-enhanced Raman scattering-active material having a coating applied thereto to improve the adsorption properties of the collector. The collector may also be used in automated sequential devises, in probe array devices.

Imaging thermal conductivity with nanoscale resolution using a scanning spin probe

DOE PAGES

Laraoui, Abdelghani; Aycock-Rizzo, Halley; Gao, Yang; ...

2015-11-20

The ability to probe nanoscale heat flow in a material is often limited by lack of spatial resolution. Here, we use a diamond-nanocrystal-hosted nitrogen-vacancy centre attached to the apex of a silicon thermal tip as a local temperature sensor. We apply an electrical current to heat up the tip and rely on the nitrogen vacancy to monitor the thermal changes the tip experiences as it is brought into contact with surfaces of varying thermal conductivity. By combining atomic force and confocal microscopy, we image phantom microstructures with nanoscale resolution, and attain excellent agreement between the thermal conductivity and topographic maps.more » The small mass and high thermal conductivity of the diamond host make the time response of our technique short, which we demonstrate by monitoring the tip temperature upon application of a heat pulse. Our approach promises multiple applications, from the investigation of phonon dynamics in nanostructures to the characterization of heterogeneous phase transitions and chemical reactions in various solid-state systems.« less

Contact of a spherical probe with a stretched rubber substrate

NASA Astrophysics Data System (ADS)

Frétigny, Christian; Chateauminois, Antoine

2017-07-01

We report on a theoretical and experimental investigation of the normal contact of stretched neo-Hookean substrates with rigid spherical probes. Starting from a published formulation of surface Green's function for incremental displacements on a prestretched, neo-Hookean, substrate [J. Mech. Phys. Solids 56, 2957 (2008), 10.1016/j.jmps.2008.07.002], a model is derived for both adhesive and nonadhesive contacts. The shape of the elliptical contact area together with the contact load and the contact stiffness are predicted as a function of the in-plane stretch ratios λx and λy of the substrate. The validity of this model is assessed by contact experiments carried out using an uniaxally stretched silicone rubber. For stretch ratio below about 1.25, a good agreement is observed between theory and experiments. Above this threshold, some deviations from the theoretical predictions are induced as a result of the departure of the mechanical response of the silicone rubber from the neo-Hokeean description embedded in the model.

Effects of Drying Process on an IgG1 Monoclonal Antibody Using Solid-State Hydrogen Deuterium Exchange with Mass Spectrometric Analysis (ssHDX-MS).

PubMed

Moussa, Ehab M; Wilson, Nathan E; Zhou, Qi Tony; Singh, Satish K; Nema, Sandeep; Topp, Elizabeth M

2018-01-03

Lyophilization and spray drying are widely used to manufacture solid forms of therapeutic proteins. Lyophilization is used to stabilize proteins vulnerable to degradation in solution, whereas spray drying is mainly used to prepare inhalation powders or as an alternative to freezing for storing bulk drug substance. Both processes impose stresses that may adversely affect protein structure, stability and bioactivity. Here, we compared lyophilization with and without controlled ice nucleation, and spray drying for their effects on the solid-state conformation and matrix interactions of a model IgG1 monoclonal antibody (mAb). Solid-state conformation and matrix interactions of the mAb were probed using solid-state hydrogen-deuterium exchange with mass spectrometric analysis (ssHDX-MS), and solid-state Fourier transform infrared (ssFTIR) and solid-state fluorescence spectroscopies. mAb conformation and/or matrix interactions were most perturbed in mannitol-containing samples and the distribution of states was more heterogeneous in sucrose and trehalose samples that were spray dried. The findings demonstrate the sensitivity of ssHDX-MS to changes weakly indicated by spectroscopic methods, and support the broader use of ssHDX-MS to probe formulation and process effects on proteins in solid samples.

Pinus sylvestris L. needle surface wettability parameters as indicators of atmospheric environment pollution impacts: Novel contact angle hysteresis methodology

NASA Astrophysics Data System (ADS)

Pogorzelski, Stanisław J.; Rochowski, Pawel; Szurkowski, Janusz

2014-02-01

An investigation of water contact angles (CAs), contact angle hysteresis (CAH) was carried out for 1-year to 4-year old needles (Pinus sylvestris) collected in urban (Gdansk) and rural (Karsin) locations using an original measuring technique based on the geometry of the drop on a vertical filament. Concentrations of air pollutants (SO2, NOx, C6H6, and suspended particular matter - SPM) currently considered to be most important in causing direct damage to vegetation were simultaneously monitored. A set of the surface wettability parameters: the apparent surface free energy γSV, adhesive film tension Π, work of adhesion WA, and spreading WS, were determined from CAH data using the approach developed by Chibowski (2003) to quantify the surface energetics of the needle substrata affected by aging and pollution impacts. This formalism relates the total apparent surface free energy of the solid γSV with only three measurable quantities: the surface tension of the probe liquid γLV and its advancing θA and receding θR contact angle hysteresis. Since CAH depends on the outermost wax layer surface roughness and spatial physicochemical heterogeneity of a solid surface, CA data were corrected using surface architecture profiles registered with confocal scanning laser microscopy. It was found that the roughness parameter r is significantly negatively correlated (R = -0.74) with the needle age (collected at Karsin). The needle surface aging process resulted in its surface hydrophilization (CA↓ and CAH↓ with γSV↑ and WA↑). A temporal evolution of the needles wettability was traced with the data point distribution in the 2D space of CAH plotted versus WS. The wettability parameters were closely correlated to pollutant concentrations as evidenced from Spearman's rank correlation procedure (R = 0.63-0.91; p < 0.05). The aim of the study was to validate the established CA methodology to create a new non-invasive, low-cost technique suitable for monitoring of structural changes at interfaces of biological systems.

Carbon nanotube enhanced label-free detection of microRNAs based on hairpin probe triggered solid-phase rolling-circle amplification

NASA Astrophysics Data System (ADS)

Tian, Qianqian; Wang, Ying; Deng, Ruijie; Lin, Lei; Liu, Yang; Li, Jinghong

2014-12-01

The detection of microRNAs (miRNAs) is imperative for gaining a better understanding of the functions of these biomarkers and has great potential for the early diagnosis of human disease. High sensitivity and selectivity for miRNA detection brings new challenges. Herein, an ultrasensitive protocol for electrochemical detection of miRNA is designed through carbon nanotube (CNT) enhanced label-free detection based on hairpin probe triggered solid-phase rolling-circle amplification (RCA). Traditionally, RCA, widely applied for signal enhancement in the construction of a variety of biosensors, has an intrinsic limitation of ultrasensitive detection, as it is difficult to separate the enzymes, templates, and padlock DNAs from the RCA products in the homogeneous solution. We purposely designed a solid-phase RCA strategy, using CNTs as the solid substrate, integrated with a hairpin structured probe to recognize target miRNA. In the presence of miRNA the stem-loop structure will be unfolded, triggering the CNT based RCA process. Due to the efficient blocking effect originating from the polymeric RCA products, the label-free assay of miRNA exhibits an ultrasensitive detection limit of 1.2 fM. Furthermore, the protocol possesses excellent specificity for resolving lung cancer-related let-7 family members which have only one-nucleotide variations. The high sensitivity and selectivity give the method great potential for applications in online diagnostics and in situ detection in long-term development.The detection of microRNAs (miRNAs) is imperative for gaining a better understanding of the functions of these biomarkers and has great potential for the early diagnosis of human disease. High sensitivity and selectivity for miRNA detection brings new challenges. Herein, an ultrasensitive protocol for electrochemical detection of miRNA is designed through carbon nanotube (CNT) enhanced label-free detection based on hairpin probe triggered solid-phase rolling-circle amplification (RCA). Traditionally, RCA, widely applied for signal enhancement in the construction of a variety of biosensors, has an intrinsic limitation of ultrasensitive detection, as it is difficult to separate the enzymes, templates, and padlock DNAs from the RCA products in the homogeneous solution. We purposely designed a solid-phase RCA strategy, using CNTs as the solid substrate, integrated with a hairpin structured probe to recognize target miRNA. In the presence of miRNA the stem-loop structure will be unfolded, triggering the CNT based RCA process. Due to the efficient blocking effect originating from the polymeric RCA products, the label-free assay of miRNA exhibits an ultrasensitive detection limit of 1.2 fM. Furthermore, the protocol possesses excellent specificity for resolving lung cancer-related let-7 family members which have only one-nucleotide variations. The high sensitivity and selectivity give the method great potential for applications in online diagnostics and in situ detection in long-term development. Electronic supplementary information (ESI) available: Preparation of the chemically modified multi-walled carbon nanotubes (CNTs), characterization of the CNTs and modified CNTs, preparation of the circular probe, gel electrophoresis of the RCA products, and DNA probes as noted in the text. See DOI: 10.1039/c4nr05243a

Structure analysis of the single-domain Si(111)4 × 1-In surface by μ-probe Auger electron diffraction and μ-probe reflection high energy electron diffraction

NASA Astrophysics Data System (ADS)

Nakamura, N.; Anno, K.; Kono, S.

1991-10-01

A single-domain Si(111)4 × 1-In surface has been studied by μ-probe reflection high-energy electron diffraction (RHEED) to elucidate the symmetry of the 4 × 1 surface. Azimuthal diffraction patterns of In MNN Auger electron have been obtained by a μ-probe Auger electron diffraction (AED) apparatus from the single-domain Si(111)4 × 1-In surface. On the basis of information from scanning tunneling microscopy [J. Microsc. 152 (1988) 727] and under the assumption that the 4 × 1 surface is composed of In-overlayers, the μ-probe AED patterns were kinematically analyzed to reach a concrete model of indium arrangement.

First-principles study of the Kondo physics of a single Pu impurity in a Th host

DOE PAGES

Zhu, Jian -Xin; Albers, R. C.; Haule, K.; ...

2015-04-23

Based on its condensed-matter properties, crystal structure, and metallurgy, which includes a phase diagram with six allotropic phases, plutonium is one of the most complicated pure elements in its solid state. Its anomalous properties, which are indicative of a very strongly correlated state, are related to its special position in the periodic table, which is at the boundary between the light actinides that have itinerant 5f electrons and the heavy actinides that have localized 5f electrons. As a foundational study to probe the role of local electronic correlations in Pu, we use the local-density approximation together with a continuous-time quantummore » Monte Carlo simulation to investigate the electronic structure of a single Pu atom that is either substitutionally embedded in the bulk and or adsorbed on the surface of a Th host. This is a simpler case than the solid phases of Pu metal. With the Pu impurity atom we have found a Kondo resonance peak, which is an important signature of electronic correlations, in the local density of states around the Fermi energy. We show that the peak width of this resonance is narrower for Pu atoms at the surface of Th than for those in the bulk due to a weakened Pu - 5f hybridization with the ligands at the surface.« less

Probing the interaction of U (VI) with phosphonate-functionalized mesoporous silica using solid-state NMR spectroscopy

DOE PAGES

Uribe, Eva C.; Mason, Harris E.; Shusterman, Jennifer A.; ...

2016-05-30

The fundamental interaction of U (VI) with diethylphosphatoethyl triethoxysilane functionalized SBA-15 mesoporous silica is studied by macroscopic batch experiments and solid-state NMR spectroscopy. DPTS-functionalized silica has been shown to extract U (VI) from nitric acid solutions at or above pH 3. Extraction is dependent on pH and ionic strength. Single-pulse 31P NMR on U (VI) contacted samples revealed that U (VI)only interacts with a fraction of the ligands present on the surface. At pH 4 the U (VI) extraction capacity of the material is limited to 27–37% of the theoretical capacity, based on ligand loading. We combined single pulse 31Pmore » NMR on U (VI)-contacted samples with batch studies to measure a ligand-to-metal ratio of approximately 2 : 1 at pH 3 and 4. Batch studies and cross-polarization NMR measurements reveal that U (VI) binds to deprotonated phosphonate and/or silanol sites. We use 31P– 31P DQ-DRENAR NMR studies to compare the average dipolar coupling between phosphorus spins for both U (VI)-complexed and non-complexed ligand environments. Furthermore, these measurements reveal that U (VI) extraction is not limited by inadequate surface distribution of ligands, but rather by low stability of the surface phosphonate complex.« less

Probing the interaction of U (VI) with phosphonate-functionalized mesoporous silica using solid-state NMR spectroscopy

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

Uribe, Eva C.; Mason, Harris E.; Shusterman, Jennifer A.

The fundamental interaction of U (VI) with diethylphosphatoethyl triethoxysilane functionalized SBA-15 mesoporous silica is studied by macroscopic batch experiments and solid-state NMR spectroscopy. DPTS-functionalized silica has been shown to extract U (VI) from nitric acid solutions at or above pH 3. Extraction is dependent on pH and ionic strength. Single-pulse 31P NMR on U (VI) contacted samples revealed that U (VI)only interacts with a fraction of the ligands present on the surface. At pH 4 the U (VI) extraction capacity of the material is limited to 27–37% of the theoretical capacity, based on ligand loading. We combined single pulse 31Pmore » NMR on U (VI)-contacted samples with batch studies to measure a ligand-to-metal ratio of approximately 2 : 1 at pH 3 and 4. Batch studies and cross-polarization NMR measurements reveal that U (VI) binds to deprotonated phosphonate and/or silanol sites. We use 31P– 31P DQ-DRENAR NMR studies to compare the average dipolar coupling between phosphorus spins for both U (VI)-complexed and non-complexed ligand environments. Furthermore, these measurements reveal that U (VI) extraction is not limited by inadequate surface distribution of ligands, but rather by low stability of the surface phosphonate complex.« less

Eddy current probe response to open and closed surface flaws

NASA Technical Reports Server (NTRS)

Auld, B. A.; Muennemann, F.; Winslow, D. K.

1981-01-01

A general analysis of eddy current response to certain types of open and closed surface flaws is presented for both standard low-frequency and ferromagnetic-resonance (FMR) probes. It is shown analytically that for two-dimensional and three-dimensional surface flaws interrogated by a uniform probe field, the crack opening sensitivity increases with the operating frequency of the probe, this behavior being due to the Faraday induction effect. Experiments with low-frequency probes operating at or below 1 MHz and with the FMR probe operating at approximately 1000 MHz confirm this increase of the crack mouth opening displacement for practical situations where the probe field is not uniform in the vicinity of the flaw.

The role of probe oxide in local surface conductivity measurements

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

Barnett, C. J.; Kryvchenkova, O.; Wilson, L. S. J.

2015-05-07

Local probe methods can be used to measure nanoscale surface conductivity, but some techniques including nanoscale four point probe rely on at least two of the probes forming the same low resistivity non-rectifying contact to the sample. Here, the role of probe shank oxide has been examined by carrying out contact and non-contact I V measurements on GaAs when the probe oxide has been controllably reduced, both experimentally and in simulation. In contact, the barrier height is pinned but the barrier shape changes with probe shank oxide dimensions. In non-contact measurements, the oxide modifies the electrostatic interaction inducing a quantummore » dot that alters the tunneling behavior. For both, the contact resistance change is dependent on polarity, which violates the assumption required for four point probe to remove probe contact resistance from the measured conductivity. This has implications for all nanoscale surface probe measurements and macroscopic four point probe, both in air and vacuum, where the role of probe oxide contamination is not well understood.« less

A strip-shield improves the efficiency of a solenoid coil in probes for high-field solid-state NMR of lossy biological samples.

PubMed

Wu, Chin H; Grant, Christopher V; Cook, Gabriel A; Park, Sang Ho; Opella, Stanley J

2009-09-01

A strip-shield inserted between a high inductance double-tuned solenoid coil and the glass tube containing the sample improves the efficiency of probes used for high-field solid-state NMR experiments on lossy aqueous samples of proteins and other biopolymers. A strip-shield is a coil liner consisting of thin copper strips layered on a PTFE (polytetrafluoroethylene) insulator. With lossy samples, the shift in tuning frequency is smaller, the reduction in Q, and RF-induced heating are all significantly reduced when the strip-shield is present. The performance of 800MHz (1)H/(15)N and (1)H/(13)C double-resonance probes is demonstrated on aqueous samples of membrane proteins in phospholipid bilayers.

Foldable polymers as probes

DOEpatents

Li, Alexander D. Q. [Pullman, WA; Wang, Wei [Pullman, WA

2007-07-03

Disclosed herein are novel probes, which can be used to detect and identify target molecules of interest in a sample. The disclosed probes can be used to monitor conformational changes induced by molecular recognition events in addition to providing signaling the presence and/or identity of a target molecule. Methods, including solid phase synthesis techniques, for making probe molecules that exhibit changes in their optical properties upon target molecule binding are described in the disclosure. Also disclosed herein are novel chromophore moieties, which have tailored fluorescent emission spectra.

Foldable polymers as probes

DOEpatents

Li, Alexander D. Q. [Pullman, WA; Wang, Wei [Pullman, WA

2009-07-07

Disclosed herein are novel probes, which can be used to detect and identify target molecules of interest in a sample. The disclosed probes can be used to monitor conformational changes induced by molecular recognition events in addition to providing signaling the presence and/or identity of a target molecule. Methods, including solid phase synthesis techniques, for making probe molecules that exhibit changes in their optical properties upon target molecule binding are described in the disclosure. Also disclosed herein are novel chromophore moieties, which have tailored fluorescent emission spectra.

Method and apparatus for staining immobilized nucleic acids

DOEpatents

Ramsey, J. Michael; Foote, Robert S.; Jacobson, Stephen C.

2000-01-01

A method for staining immobilized nucleic acids includes the steps of affixing DNA probes to a solid substrate, moving target DNA material into proximity with the DNA probes, whereby the target DNA hybridized with specific ones of the DNA probes, and moving a fluorescent dye into proximity with the hybridized target DNA, whereby the fluorescent dye binds to the hybridized DNA to enable subsequent detection of fluorescence.

Dual-probe near-field fiber head with gap servo control for data storage applications.

PubMed

Fang, Jen-Yu; Tien, Chung-Hao; Shieh, Han-Ping D

2007-10-29

We present a novel fiber-based near-field optical head consisting of a straw-shaped writing probe and a flat gap sensing probe. The straw-shaped probe with a C-aperture on the end face exhibits enhanced transmission by a factor of 3 orders of magnitude over a conventional fiber probe due to a hybrid effect that excites both propagation modes and surface plasmon waves. In the gap sensing probe, the spacing between the probe and the disk surface functions as an external cavity. The high sensitivity of the output power to the change in the gap width is used as a feedback control signal. We characterize and design the straw-shaped writing probe and the flat gap sensing probe. The dual-probe system is installed on a conventional biaxial actuator to demonstrate the capability of flying over a disk surface with nanometer position precision.

Development of novel edible luminescent nanoparticle sensors

NASA Astrophysics Data System (ADS)

Jalalian, Sanaz

This project has developed a novel class of edible hydrocolloid food nanosensors which are doped with luminescent chromophores and investigated whether they can be used to provide information about the local food matrix - temperature, oxygen concentration, and the presence of food-borne pathogens. The luminescence properties of the probes such as phosphorescence and fluorescence provide the sensor sensitivity to the food properties. Hydrocolloid nanoparticles were made from gelatin and starch with diameters ranging from 50 to ˜200 nm and labeled with food grade luminescent probes. The chromophore was covalently and non-covalently attached to the nanoparticle and the photophysical properties of the probe in the food system were studied. Temperature sensors were developed by using the phosphorescence sensitivity of a chromophore to temperature. Experiments with two different probes, namely erythrosine B labeled gelatin nanoparticles and phloxine B labeled gelatin nanoparticles have demonstrated that both probes can be effectively used as temperature sensors in liquid and solid food. The Van't Hoff plots of ln(IDF/IP) versus 1/T vary monotonically over a relatively wide temperature range and thus provide a basis for estimating temperature from measurements of phosphorescence and delayed fluorescence. The tests indicated that the presence of some ingredients such as tannin and anthocyanins in the composition of the food may prohibit the use of gelatin nanoparticle probes due to precipitation of gelatin nanoparticles. The luminescence quenching of the probe by oxygen was used to develop a nanoparticle sensor for oxygen. The results of experiments on liquid and solid food samples indicate that erythrosine B labeled gelatin nanoparticles can be used as a probe to detect the presence or absence of oxygen in some liquid foods. Precise control of oxygen concentration in solutions will pose a challenge as has been observed in this study. The probe did not work as an appropriate oxygen sensor in the case of solid food samples with low relative humidity. The use of gelatin nanoparticles as a sensor to detect the presence of food-borne pathogens requires a measurable change in the spectrum of fluorescence resonance energy transfer between two chromophores which was not observed in the tests.

Four-probe measurements with a three-probe scanning tunneling microscope.

PubMed

Salomons, Mark; Martins, Bruno V C; Zikovsky, Janik; Wolkow, Robert A

2014-04-01

We present an ultrahigh vacuum (UHV) three-probe scanning tunneling microscope in which each probe is capable of atomic resolution. A UHV JEOL scanning electron microscope aids in the placement of the probes on the sample. The machine also has a field ion microscope to clean, atomically image, and shape the probe tips. The machine uses bare conductive samples and tips with a homebuilt set of pliers for heating and loading. Automated feedback controlled tip-surface contacts allow for electrical stability and reproducibility while also greatly reducing tip and surface damage due to contact formation. The ability to register inter-tip position by imaging of a single surface feature by multiple tips is demonstrated. Four-probe material characterization is achieved by deploying two tips as fixed current probes and the third tip as a movable voltage probe.

Manganese-calcium intermixing facilitates heteroepitaxial growth at the (1014) calcite-water interface

DOE PAGES

Xu, Man; Riechers, Shawn L.; Ilton, Eugene S.; ...

2017-09-05

For this research, in situ atomic force microscopy (AFM) measurements were performed to probe surface precipitates that formed on the (10more » $$\\bar{1}$$4) surface of calcite (CaCO 3) single crystals following reaction with Mn2 +-bearing aqueous solutions. Three-dimensional epitaxial islands were observed to precipitate and grow on the surfaces. In situ time-sequenced measurements demonstrated that the growth rates were commensurate with those obtained for epitaxial islands formed on calcite crystals reacted with Cd2 +-bearing aqueous solutions of the same range in supersaturation with respect to the pure metal carbonate phase. This finding was unexpected as rhodochrosite (MnCO 3) and calcite display a 10% lattice mismatch, based on the area of their (10$$\\bar{1}$$4) surface unit cells, whereas the lattice mismatch is only 4% for otavite (CdCO 3) and calcite. Coatings of varying thicknesses were therefore synthesized by reacting calcite single crystals in calcite-equilibrated aqueous solutions with up to 250 μM MnCl 2. Ex situ X-ray photoelectron spectroscopy (XPS), scanning transmission electron microscopy (STEM), energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), X-ray reflectivity (XRR), and AFM measurements of the reacted crystals demonstrated the formation of an epitaxial (Mn,Ca)CO 3 solid solution. The epitaxial solid solution had a spatially complex composition, whereby the first few nanometers were rich in Ca and the Mn content increased with distance from the original calcite surface, culminating in a topmost region of almost pure MnCO 3 for the thickest coatings. The effective lattice mismatch was therefore much smaller than the nominal mismatch thus explaining the measured growth rates. Lastly, these findings highlight the strong influence played by the substrate on the composition of surface precipitates in aqueous conditions.« less

Surface-enhanced Raman scattering (SERS) dosimeter and probe

DOEpatents

Vo-Dinh, T.

1995-03-21

A dosimeter and probe for measuring exposure to chemical and biological compounds is disclosed. The dosimeter or probe includes a collector which may be analyzed by surface-enhanced Raman spectroscopy. The collector comprises a surface-enhanced Raman scattering-active material having a coating applied thereto to improve the adsorption properties of the collector. The collector may also be used in automated sequential devices, in probe array devices. 10 figures.

Surface-enhanced Raman scattering based nonfluorescent probe for multiplex DNA detection.

PubMed

Sun, Lan; Yu, Chenxu; Irudayaraj, Joseph

2007-06-01

To provide rapid and accurate detection of DNA markers in a straightforward, inexpensive, and multiplex format, an alternative surface-enhanced Raman scattering based probe was designed and fabricated to covalently attach both DNA probing sequence and nonfluorescent Raman tags to the surface of gold nanoparticles (DNA-AuP-RTag). The intensity of Raman signal of the probes could be controlled through the surface coverage of the nonfluorescent Raman tags (RTags). Detection sensitivity of these probes could be optimized by fine-tuning the amount of DNA molecules and RTags on the probes. Long-term stability of the DNA-AuP-RTag probes was found to be good (over 3 months). Excellent multiplexing capability of the DNA-AuP-RTag scheme was demonstrated by simultaneous identification of up to eight probes in a mixture. Detection of hybridization of single-stranded DNA to its complementary targets was successfully accomplished with a long-term goal to use nonfluorescent RTags in a Raman-based DNA microarray platform.

Surface-Enhanced Raman Scattering Based Nonfluorescent Probe for Multiplex DNA Detection

PubMed Central

Sun, Lan; Yu, Chenxu; Irudayaraj, Joseph

2008-01-01

To provide rapid and accurate detection of DNA markers in a straightforward, inexpensive and multiplex format, an alternative surface enhanced Raman scattering (SERS) based probe was designed and fabricated to covalently attach both DNA probing sequence and non-fluorescent Raman tags to the surface of gold nanoparticles (DNA-AuP-RTag). The intensity of Raman signal of the probes could be controlled through the surface coverage of the non-fluorescent Raman tags (RTags). Detection sensitivity of these probes could be optimized by fine-tuning the amount of DNA molecules and RTags on the probes. Long-term stability of the DNA-AuP-RTag probes was found to be good (over 3 months). Excellent multiplexing capability of the DNA-AuP-RTag scheme was demonstrated by simultaneous identification of up to eight probes in a mixture. Detection of hybridization of single-stranded DNA (ssDNA) to its complementary targets was successfully accomplished with a long-term goal to use non-fluorescent RTags in a Raman-based DNA microarray platform. PMID:17465531

Spatial Temperature Mapping within Polymer Nanocomposites Undergoing Ultrafast Photothermal Heating via Gold Nanorods

PubMed Central

Maity, Somsubhra; Wu, Wei-Chen; Xu, Chao; Tracy, Joseph B.; Gundogdu, Kenan; Bochinski, Jason R.; Clarke, Laura I.

2015-01-01

Heat emanates from gold nanorods (GNRs) under ultrafast optical excitation of the localized surface plasmon resonance. The steady state nanoscale temperature distribution formed within a polymer matrix embedded with GNRs undergoing pulsed femtosecond photothermal heating is determined experimentally using two independent ensemble optical techniques. Physical rotation of the nanorods reveals the average local temperature of the polymer melt in the immediate spatial volume surrounding them while fluorescence of homogeneously-distributed perylene molecules monitors temperature over sample regions at larger distances from the GNRs. Polarization-sensitive fluorescence measurements of the perylene probes provide an estimate of the average size of the quasi-molten region surrounding each nanorod (that is, the boundary between softened polymer and solid material as the temperature decreases radially away from each particle) and distinguishes the steady state temperature in the solid and melt regions. Combining these separate methods enables nanoscale spatial mapping of the average steady state temperature distribution caused by ultrafast excitation of the GNRs. These observations definitively demonstrate the presence of a steady-state temperature gradient and indicate that localized heating via the photothermal effect within materials enables nanoscale thermal manipulations without significantly altering the bulk sample temperature in these systems. These quantitative results are further verified by reorienting nanorods within a solid polymer nanofiber without inducing any morphological changes to the highly temperature-sensitive nanofiber surface. Temperature differences of 70 – 90 °C were observed over a distances of ~100 nm. PMID:25379775

Characterization of structural and electrostatic complexity in pentacene thin films by scanning probe microscopy

NASA Astrophysics Data System (ADS)

Puntambekar, Kanan Prakash

The advancement of organic electronics for applications in solar energy conversion, printed circuitry, displays, and solid-state lighting depends upon optimization of structure and properties for a variety of organic semiconductor interfaces. Organic semiconductor/insulator (O/I) and organic-metal (O/M) interfaces, in particular, are critical to the operation of organic thin film transistors (OTFTs) currently being developed for printed flexible electronics. Scanning probe microscopy (SPM) is a powerful tool to isolate and characterize the bottlenecks to charge transport at these interfaces. This thesis establishes a direct correlation between the structural disorder and electrical complexity at these interfaces, using various SPM based methods and discusses the implications of such complexity on device performance. To examine the O/M interfaces, surface potentials of operating pentacene TFTs with two different contact geometries (bottom or top) were mapped by Kelvin probe force microscopy (KFM). The surface potential distribution was used to isolate the potential drops at the source and drain contacts. Simultaneously obtained topography and surface potential maps elucidated the correlation between the morphology and contact resistance at the O/M interface; the bottom contact TFTs were observed to be contact limited at large gate voltages, while the top contact TFTs were not contact limited. A direct correlation between structural defects and electric potential variations at the pentacene and silicon dioxide, a common insulator, is demonstrated. Lateral force microscopy (LFM) generates striking images of the polycrystalline microstructure of a monolayer thick pentacene film, allowing clear visualization of the grain boundary network. Further more, surface potential wells localized at the grain boundaries were observed by KFM, suggesting that the grain boundaries may serve as charge carrier (hole) traps. Line dislocations were also revealed in the second monolayer by chemical etching and SPM and produce strong variations in the surface potential that must affect the interfacial charge conductance. Structural disorder at the O/I and O/M interfaces degrades both injection and transport of charge, and therefore needs to be minimized. Thus both visualization and correlation of structural and electrical complexity at these interfaces have important implications for understanding electrical transport in OTFTs and for defining strategies to improve device performance.

SUMMARY REPORT ON CORROSIVITY STUDIES IN COINCINERATION OF SEWAGE SLUDGE AND SOLID WASTE

EPA Science Inventory

Corrosion probe exposures were conducted in the Harrisburg, Pennsylvania Incinerator to determine the effects of burning low-chloride sewage sludge with municipal refuse. Probes having controlled temperature gradients were used to measure corrosion rates for exposure times up to ...

Compact endocavity diagnostic probes for nuclear radiation detection

DOEpatents

Cui, Yonggang; James, Ralph; Bolotnikov, Aleksey

2014-08-26

This invention relates to the field of radiation imaging. In particular, the invention relates to an apparatus and a method for imaging tissue or an inanimate object using a novel probe that has an integrated solid-state semiconductor detector and complete readout electronics circuitry.

Discrimination of three types of homopolymers in single-stranded DNA with solid-state nanopores through external control of the DNA motion.

PubMed

Akahori, Rena; Yanagi, Itaru; Goto, Yusuke; Harada, Kunio; Yokoi, Takahide; Takeda, Ken-Ichi

2017-08-22

To achieve DNA sequencing with solid-state nanopores, the speed of the DNA in the nanopore must be controlled to obtain sequence-specific signals. In this study, we fabricated a nanopore-sensing system equipped with a DNA motion controller. DNA strands were immobilized on a Si probe, and approach of this probe to the nanopore vicinity could be controlled using a piezo actuator and stepper motor. The area of the Si probe was larger than the area of the membrane, which meant that the immobilized DNA could enter the nanopore without the need for the probe to scan to determine the location of the nanopore in the membrane. We demonstrated that a single-stranded DNA could be inserted into and removed from a nanopore in our experimental system. The number of different ionic-current levels observed while DNA remained in the nanopore corresponded to the number of different types of homopolymers in the DNA.

An "Inefficient Fin" Non-Dimensional Parameter to Measure Gas Temperatures Efficiently

NASA Technical Reports Server (NTRS)

Lemieux, Patrick; Murray, William; Cooke, Terry; Gerhardt, James

2012-01-01

A gas containment vessel that is not in thermal equilibrium with the bulk gas can affect its temperature measurement. The physical nature of many gas dynamics experiments often makes the accurate measurement of temperature a challenge. The environment itself typically requires that the thermocouple be sheathed, both to protect the wires and hot junction of the instrument from their environment, and to provide a smooth, rigid surface for pressure sealing of the enclosure. However, that enclosure may also be much colder than the gas to be sensed, or vice-versa. Either way, the effect of such gradients is to potentially skew the temperature measurements themselves, since heat may then be conducted by the instrument. Thermocouple designers traditionally address this problem by insulating the sheath from the thermocouple leads and hot junction as much as possible. The thermocouple leads are typically packed in a ceramic powder inside the sheath, protecting them somewhat from temperature gradients along the sheath, but there is no effective mechanism to shield the sheath from the enclosure body itself. Standard practice dictates that thermocouples be used in installations that do not present large thermal gradients along the probe. If this conduction dominates heat transfer near the tip of the probe, then temperature measurements may be expected to be skewed. While the same problem may be experienced in the measurement of temperature at various points within a solid in a gradient, it tends to be aggravated in the measurements of gas temperature, since heat transfer dependent on convection is often less efficient than conduction along the thermocouple. The proposed solution is an inefficient fin thermocouple probe. Conventional wisdom suggests that in many experiments where gas flows through an enclosure (e.g., flow in pipe, manifold, nozzle, etc.), the thermocouple be introduced flush to the surface, so as not to interfere with the flow. In practice, however, many such experiments take place where the flow is already turbulent, so that a protruding thermocouple probe has a negligible effect on the flow characteristics. The key question then becomes just how far into the flow should a thermocouple protrude in order to properly sense the gas temperature at that point. Modeling the thermocouple as an "inefficient fin" directly addresses this question. The appropriate assumptions in this case are: one-dimensional conduction along the fin; steady-state, constant, and homogeneous thermal conductivity; negligible radiation; and a uniform, constant heat transfer coefficient over the probe surface. It is noted that the nature of the ceramic-filled probe makes the key assumption of homogeneous thermal conductivity that much more conservative.

ELECTRON TRANSFER MECHANISM AT THE SOLID-LIQUID INTERFACE OF PHYLLOSILICATES

EPA Science Inventory

Interfacial electron transfer processes on clay minerals have significant impact in natural environments and geochemical systems. Nitrobenzene was used as molecular probes to study the electron transfer mechanism at the solid-water interfaces of Fe-containing phyllosicates. For...

Surface Organometallic Chemistry of Supported Iridium(III) as a Probe for Organotransition Metal–Support Interactions in C–H Activation

DOE PAGES

Kaphan, David M.; Klet, Rachel C.; Perras, Frederic A.; ...

2018-05-11

Systematic study of the interactions between organometallic catalysts and metal oxide support materials is essential for the realization of rational design in heterogeneous catalysis. Herein we describe the stoichiometric and catalytic chemistry of a [Cp*(PMe 3)Ir(III)] complex chemisorbed on a variety of acidic metal oxides as a multifaceted probe for stereoelectronic communication between the support and organometallic center. Electrophilic bond activation was explored in the context of stoichiometric hydrogenolysis as well as catalytic H/D exchange. Further information was obtained from the observation of processes related to dynamic exchange between grafted organometallic species and those in solution. The supported organometallic speciesmore » were characterized by a variety of spectroscopic techniques including dynamic nuclear polarization-enhanced solid-state NMR spectroscopy, diffuse reflectance infrared Fourier transform spectroscopy, and X-ray absorption spectroscopy. Finally, strongly acidic modified metal oxides such as sulfated zirconia engender high levels of activity toward electrophilic bond activation of both sp 2 and sp 3 C–H bonds, including the rapid deuteration of methane at room temperature; however, the global trend for the supports studied here does not suggest a direct correlation between activity and surface Brønsted acidity.« less

Surface Organometallic Chemistry of Supported Iridium(III) as a Probe for Organotransition Metal–Support Interactions in C–H Activation

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

Kaphan, David M.; Klet, Rachel C.; Perras, Frederic A.

Systematic study of the interactions between organometallic catalysts and metal oxide support materials is essential for the realization of rational design in heterogeneous catalysis. Herein we describe the stoichiometric and catalytic chemistry of a [Cp*(PMe 3)Ir(III)] complex chemisorbed on a variety of acidic metal oxides as a multifaceted probe for stereoelectronic communication between the support and organometallic center. Electrophilic bond activation was explored in the context of stoichiometric hydrogenolysis as well as catalytic H/D exchange. Further information was obtained from the observation of processes related to dynamic exchange between grafted organometallic species and those in solution. The supported organometallic speciesmore » were characterized by a variety of spectroscopic techniques including dynamic nuclear polarization-enhanced solid-state NMR spectroscopy, diffuse reflectance infrared Fourier transform spectroscopy, and X-ray absorption spectroscopy. Finally, strongly acidic modified metal oxides such as sulfated zirconia engender high levels of activity toward electrophilic bond activation of both sp 2 and sp 3 C–H bonds, including the rapid deuteration of methane at room temperature; however, the global trend for the supports studied here does not suggest a direct correlation between activity and surface Brønsted acidity.« less

Combustion of solid carbon rods in zero and normal gravity. Ph.D. Thesis - Toledo Univ., Ohio

NASA Technical Reports Server (NTRS)

Spuckler, C. M.

1981-01-01

In order to investigate the mechanism of carbon combustion and to assess the importance of gravitational induced convection on the process, zero and normal gravity experiments were conducted in which spectroscopic carbon rods were resistance ignitied and burned in dry oxygen environments. In the zero-gravity drop tower tests, a blue flame surrounded the rod, showing that a gas phase reaction in which carbon monoxide was oxidized to carbon dioxide was taking place. The ratio of flame diameter to rod diameter was obtained as a function of time. It was found that this ratio was inversely proportional to both the oxygen pressure and the rod diameter. In the normal gravity tests, direct mass spectrometric sampling was used to measure gas phase concentrations. The gas sampling probe was positioned near the circumference of a horizontally mounted 0.615 cm diameter carbon rod, either at the top or at angles of 45 deg to 90 deg from the top, and yielded concentration profiles of CO2, CO, and O2 as a function of distance from the surface. The mechanism controlling the combustion process was found to change from chemical process control at the 90 deg and 45 deg probe positions to mass transfer control at the 0 deg probe position at the top of the rod. Under the experimental conditions used, carbon combustion was characterized by two surface reactions, 2C + O2 yields 2CO and CO2 + C yields 2CO, and a gas phase reaction, 2CO + O2 yields 2CO2.

A Mars environmental survey (MESUR) - Feasibility of a low cost global approach

NASA Technical Reports Server (NTRS)

Hubbard, G. S.; Wercinski, Paul F.; Sarver, George L.; Hanel, Robert P.; Ramos, Ruben

1991-01-01

In situ measurements of Mars' surface and atmosphere are the objectives of a novel network mission concept called the Mars Environmental SURvey (MESUR). As envisioned, the MESUR mission will emplace a pole-to-pole global distribution of 16 landers on the Martian surface over three launch opportunites using medium-lift (Delta-class) launch vehicles. The basic concept is to deploy small free-flying probes which would directly enter the Martian atmosphere, measure the upper atmospheric structure, image the local terrain before landing, and survive landing to perform meteorology, seismology, surface imaging, and soil chemistry measurements. Data will be returned via dedicated relay orbiter or direct-to-earth transmission. The mission philosophy is to: (1) 'grow' a network over a period of years using a series of launch opportunities; (2) develop a level-of-effort which is flexible and responsive to a broad set of objectives; (3) focus on Mars science while providing a solid basis for future human presence; and (4) minimize overall project cost and complexity wherever possible.

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

DOEpatents

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

2014-06-03

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

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

DOEpatents

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

2015-09-29

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

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

DOEpatents

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

2013-08-27

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

Molecular environmental geochemistry

NASA Astrophysics Data System (ADS)

O'Day, Peggy A.

1999-05-01

The chemistry, mobility, and bioavailability of contaminant species in the natural environment are controlled by reactions that occur in and among solid, aqueous, and gas phases. These reactions are varied and complex, involving changes in chemical form and mass transfer among inorganic, organic, and biochemical species. The field of molecular environmental geochemistry seeks to apply spectroscopic and microscopic probes to the mechanistic understanding of environmentally relevant chemical processes, particularly those involving contaminants and Earth materials. In general, empirical geochemical models have been shown to lack uniqueness and adequate predictive capability, even in relatively simple systems. Molecular geochemical tools, when coupled with macroscopic measurements, can provide the level of chemical detail required for the credible extrapolation of contaminant reactivity and bioavailability over ranges of temperature, pressure, and composition. This review focuses on recent advances in the understanding of molecular chemistry and reaction mechanisms at mineral surfaces and mineral-fluid interfaces spurred by the application of new spectroscopies and microscopies. These methods, such as synchrotron X-ray absorption and scattering techniques, vibrational and resonance spectroscopies, and scanning probe microscopies, provide direct chemical information that can elucidate molecular mechanisms, including element speciation, ligand coordination and oxidation state, structural arrangement and crystallinity on different scales, and physical morphology and topography of surfaces. Nonvacuum techniques that allow examination of reactions in situ (i.e., with water or fluids present) and in real time provide direct links between molecular structure and reactivity and measurements of kinetic rates or thermodynamic properties. Applications of these diverse probes to laboratory model systems have provided fundamental insight into inorganic and organic reactions at mineral surfaces and mineral-water interfaces. A review of recent studies employing molecular characterizations of soils, sediments, and biological samples from contaminated sites exemplifies the utility and benefits, as well as the challenge, of applying molecular probes to complicated natural materials. New techniques, technological advances, and the crossover of methods from other disciplines such as biochemistry and materials science promise better examination of environmental chemical processes in real time and at higher resolution, and will further the integration of molecular information into field-scale chemical and hydrologic models.

Four-probe measurements with a three-probe scanning tunneling microscope

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

Salomons, Mark; Martins, Bruno V. C.; Zikovsky, Janik

2014-04-15

We present an ultrahigh vacuum (UHV) three-probe scanning tunneling microscope in which each probe is capable of atomic resolution. A UHV JEOL scanning electron microscope aids in the placement of the probes on the sample. The machine also has a field ion microscope to clean, atomically image, and shape the probe tips. The machine uses bare conductive samples and tips with a homebuilt set of pliers for heating and loading. Automated feedback controlled tip-surface contacts allow for electrical stability and reproducibility while also greatly reducing tip and surface damage due to contact formation. The ability to register inter-tip position bymore » imaging of a single surface feature by multiple tips is demonstrated. Four-probe material characterization is achieved by deploying two tips as fixed current probes and the third tip as a movable voltage probe.« less

Real time dynamics of Si magic clusters mediating phase transformation: Si(111)-(1 × 1) to (7 × 7) reconstruction revisited

NASA Astrophysics Data System (ADS)

Ong, Wei Jie; Tok, Eng Soon

2012-07-01

Using Scanning Tunneling Microscope (STM), we show that the surface undergoes phase transformation from disordered "1 × 1" to (7 × 7) reconstruction which is mediated by the formation of Si magic clusters. Mono-disperse Si magic clusters of size ~ 13.5 ± 0.5 Å can be formed by heating the Si(111) surface to 1200 °C and quenching it to room temperature at cooling rates of at least 100 °C/min. The structure consists of 3 tetra-clusters of size ~ 4.5 Ǻ similar to the Si magic clusters that were formed from Si adatoms deposited by Si solid source on Si(111)-(7 × 7) [1]. Using real time STM scanning to probe the surface at ~ 400 °C, we show that Si magic clusters pop up from the (1 × 1) surface and form spontaneously during the phase transformation. This is attributed to the difference in atomic density between "disordered 1 × 1" and (7 × 7) surface structures which lead to the release of excess Si atoms onto the surface as magic clusters.

Speciation of adsorbates on surface of solids by infrared spectroscopy and chemometrics.

PubMed

Vilmin, Franck; Bazin, Philippe; Thibault-Starzyk, Frédéric; Travert, Arnaud

2015-09-03

Speciation, i.e. identification and quantification, of surface species on heterogeneous surfaces by infrared spectroscopy is important in many fields but remains a challenging task when facing strongly overlapped spectra of multiple adspecies. Here, we propose a new methodology, combining state of the art instrumental developments for quantitative infrared spectroscopy of adspecies and chemometrics tools, mainly a novel data processing algorithm, called SORB-MCR (SOft modeling by Recursive Based-Multivariate Curve Resolution) and multivariate calibration. After formal transposition of the general linear mixture model to adsorption spectral data, the main issues, i.e. validity of Beer-Lambert law and rank deficiency problems, are theoretically discussed. Then, the methodology is exposed through application to two case studies, each of them characterized by a specific type of rank deficiency: (i) speciation of physisorbed water species over a hydrated silica surface, and (ii) speciation (chemisorption and physisorption) of a silane probe molecule over a dehydrated silica surface. In both cases, we demonstrate the relevance of this approach which leads to a thorough surface speciation based on comprehensive and fully interpretable multivariate quantitative models. Limitations and drawbacks of the methodology are also underlined. Copyright © 2015 Elsevier B.V. All rights reserved.

Surface plasmon resonance spectroscopy sensor and methods for using same

DOEpatents

Anderson, Brian Benjamin; Nave, Stanley Eugene

2002-01-01

A surface plasmon resonance ("SPR") probe with a detachable sensor head and system and methods for using the same in various applications is described. The SPR probe couples fiber optic cables directly to an SPR substrate that has a generally planar input surface and a generally curved reflecting surface, such as a substrate formed as a hemisphere. Forming the SPR probe in this manner allows the probe to be miniaturized and operate without the need for high precision, expensive and bulky collimating or focusing optics. Additionally, the curved reflecting surface of the substrate can be coated with one or multiple patches of sensing medium to allow the probe to detect for multiple analytes of interest or to provide multiple readings for comparison and higher precision. Specific applications for the probe are disclosed, including extremely high sensitive relative humidity and dewpoint detection for, e.g., moisture-sensitive environment such as volatile chemical reactions. The SPR probe disclosed operates with a large dynamic range and provides extremely high quality spectra despite being robust enough for field deployment and readily manufacturable.

Sampling probe for microarray read out using electrospray mass spectrometry

DOEpatents

Van Berkel, Gary J.

2004-10-12

An automated electrospray based sampling system and method for analysis obtains samples from surface array spots having analytes. The system includes at least one probe, the probe including an inlet for flowing at least one eluting solvent to respective ones of a plurality of spots and an outlet for directing the analyte away from the spots. An automatic positioning system is provided for translating the probe relative to the spots to permit sampling of any spot. An electrospray ion source having an input fluidicly connected to the probe receives the analyte and generates ions from the analyte. The ion source provides the generated ions to a structure for analysis to identify the analyte, preferably being a mass spectrometer. The probe can be a surface contact probe, where the probe forms an enclosing seal along the periphery of the array spot surface.

Overcoming Short-Circuit in Lead-Free CH3NH3SnI3 Perovskite Solar Cells via Kinetically Controlled Gas-Solid Reaction Film Fabrication Process.

PubMed

Yokoyama, Takamichi; Cao, Duyen H; Stoumpos, Constantinos C; Song, Tze-Bin; Sato, Yoshiharu; Aramaki, Shinji; Kanatzidis, Mercouri G

2016-03-03

The development of Sn-based perovskite solar cells has been challenging because devices often show short-circuit behavior due to poor morphologies and undesired electrical properties of the thin films. A low-temperature vapor-assisted solution process (LT-VASP) has been employed as a novel kinetically controlled gas-solid reaction film fabrication method to prepare lead-free CH3NH3SnI3 thin films. We show that the solid SnI2 substrate temperature is the key parameter in achieving perovskite films with high surface coverage and excellent uniformity. The resulting high-quality CH3NH3SnI3 films allow the successful fabrication of solar cells with drastically improved reproducibility, reaching an efficiency of 1.86%. Furthermore, our Kelvin probe studies show the VASP films have a doping level lower than that of films prepared from the conventional one-step method, effectively lowering the film conductivity. Above all, with (LT)-VASP, the short-circuit behavior often obtained from the conventional one-step-fabricated Sn-based perovskite devices has been overcome. This study facilitates the path to more successful Sn-perovskite photovoltaic research.

A Novel Disintegration Tester for Solid Dosage Forms Enabling Adjustable Hydrodynamics.

PubMed

Kindgen, Sarah; Rach, Regine; Nawroth, Thomas; Abrahamsson, Bertil; Langguth, Peter

2016-08-01

A modified in vitro disintegration test device was designed that enables the investigation of the influence of hydrodynamic conditions on disintegration of solid oral dosage forms. The device represents an improved derivative of the compendial PhEur/USP disintegration test device. By the application of a computerized numerical control, a variety of physiologically relevant moving velocities and profiles can be applied. With the help of computational fluid dynamics, the hydrodynamic and mechanical forces present in the probe chamber were characterized for a variety of device moving speeds. Furthermore, a proof of concept study aimed at the investigation of the influence of hydrodynamic conditions on disintegration times of immediate release tablets. The experiments demonstrated the relevance of hydrodynamics for tablet disintegration, especially in media simulating the fasted state. Disintegration times increased with decreasing moving velocity. A correlation between experimentally determined disintegration times and computational fluid dynamics predicted shear stress on tablet surface was established. In conclusion, the modified disintegration test device is a valuable tool for biorelevant in vitro disintegration testing of solid oral dosage forms. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Nanoscale imaging of fundamental li battery chemistry: solid-electrolyte interphase formation and preferential growth of lithium metal nanoclusters.

PubMed

Sacci, Robert L; Black, Jennifer M; Balke, Nina; Dudney, Nancy J; More, Karren L; Unocic, Raymond R

2015-03-11

The performance characteristics of Li-ion batteries are intrinsically linked to evolving nanoscale interfacial electrochemical reactions. To probe the mechanisms of solid electrolyte interphase (SEI) formation and to track Li nucleation and growth mechanisms from a standard organic battery electrolyte (LiPF6 in EC:DMC), we used in situ electrochemical scanning transmission electron microscopy (ec-S/TEM) to perform controlled electrochemical potential sweep measurements while simultaneously imaging site-specific structures resulting from electrochemical reactions. A combined quantitative electrochemical measurement and STEM imaging approach is used to demonstrate that chemically sensitive annular dark field STEM imaging can be used to estimate the density of the evolving SEI and to identify Li-containing phases formed in the liquid cell. We report that the SEI is approximately twice as dense as the electrolyte as determined from imaging and electron scattering theory. We also observe site-specific locations where Li nucleates and grows on the surface and edge of the glassy carbon electrode. Lastly, this report demonstrates the investigative power of quantitative nanoscale imaging combined with electrochemical measurements for studying fluid-solid interfaces and their evolving chemistries.

Solid-state voltammetry-based electrochemical immunosensor for Escherichia coli using graphene oxide-Ag nanoparticle composites as labels.

PubMed

Jiang, Xiaochun; Chen, Kun; Wang, Jing; Shao, Kang; Fu, Tao; Shao, Feng; Lu, Donglian; Liang, Jiangong; Foda, M Frahat; Han, Heyou

2013-06-21

A new electrochemical immunosensor based on solid-state voltammetry was fabricated for the detection of Escherichia coli (E. coli) by using graphene oxide-Ag nanoparticle composites (P-GO-Ag) as labels. To construct the platform, Au nanoparticles (AuNPs) were first self-assembled on an Au electrode surface through cysteamine and served as an effective matrix for antibody (Ab) attachment. Under a sandwich-type immunoassay format, the analyte and the probe (P-GO-Ag-Ab) were successively captured onto the immunosensor. Finally, the bonded AgNPs were detected through a solid-state redox process in 0.2 M of KCl solution. Combining the advantages of the high-loading capability of graphene oxide with promoted electron-transfer rate of AuNPs, this immunosensor produced a 26.92-fold signal enhancement compared with the unamplified protocol. Under the optimal conditions, the immunosensor exhibited a wide linear dependence on the logarithm of the concentration of E. coli ranging from 50 to 1.0 × 10(6) cfu mL(-1) with a detection limit of 10 cfu mL(-1). Moreover, as a practical application, the proposed immunosensor was used to monitor E. coli in lake water with satisfactory results.

Terahertz pulsed imaging as an advanced characterisation tool for film coatings--a review.

PubMed

Haaser, Miriam; Gordon, Keith C; Strachan, Clare J; Rades, Thomas

2013-12-05

Solid dosage forms are the pharmaceutical drug delivery systems of choice for oral drug delivery. These solid dosage forms are often coated to modify the physico-chemical properties of the active pharmaceutical ingredients (APIs), in particular to alter release kinetics. Since the product performance of coated dosage forms is a function of their critical coating attributes, including coating thickness, uniformity, and density, more advanced quality control techniques than weight gain are required. A recently introduced non-destructive method to quantitatively characterise coating quality is terahertz pulsed imaging (TPI). The ability of terahertz radiation to penetrate many pharmaceutical materials enables structural features of coated solid dosage forms to be probed at depth, which is not readily achievable with other established imaging techniques, e.g. near-infrared (NIR) and Raman spectroscopy. In this review TPI is introduced and various applications of the technique in pharmaceutical coating analysis are discussed. These include evaluation of coating thickness, uniformity, surface morphology, density, defects and buried structures as well as correlation between TPI measurements and drug release performance, coating process monitoring and scale up. Furthermore, challenges and limitations of the technique are discussed. Copyright © 2013 Elsevier B.V. All rights reserved.

16 CFR 1505.51 - Hot surfaces.

Code of Federal Regulations, 2011 CFR

2011-01-01

... CHILDREN Policies and Interpretations § 1505.51 Hot surfaces. (a) Test probe. Section 1505.6(g)(2) defines... inches long. To test for accessibility using this test probe, it shall be inserted no more than 3 inches into any opening in the toy. Unless the probe contacts a surface within 3 inches of the plane of the...

16 CFR 1505.51 - Hot surfaces.

Code of Federal Regulations, 2014 CFR

2014-01-01

... CHILDREN Policies and Interpretations § 1505.51 Hot surfaces. (a) Test probe. Section 1505.6(g)(2) defines... inches long. To test for accessibility using this test probe, it shall be inserted no more than 3 inches into any opening in the toy. Unless the probe contacts a surface within 3 inches of the plane of the...

16 CFR 1505.51 - Hot surfaces.

Code of Federal Regulations, 2012 CFR

2012-01-01

... CHILDREN Policies and Interpretations § 1505.51 Hot surfaces. (a) Test probe. Section 1505.6(g)(2) defines... inches long. To test for accessibility using this test probe, it shall be inserted no more than 3 inches into any opening in the toy. Unless the probe contacts a surface within 3 inches of the plane of the...

High repetition ration solid state switched CO2 TEA laser employed in industrial ultrasonic testing of aircraft parts

NASA Astrophysics Data System (ADS)

von Bergmann, Hubertus; Morkel, Francois; Stehmann, Timo

2015-02-01

Laser Ultrasonic Testing (UT) is an important technique for the non-destructive inspection of composite parts in the aerospace industry. In laser UT a high power, short pulse probe laser is scanned across the material surface, generating ultrasound waves which can be detected by a second low power laser system and are used to draw a defect map of the part. We report on the design and testing of a transversely excited atmospheric pressure (TEA) CO2 laser system specifically optimised for laser UT. The laser is excited by a novel solid-state switched pulsing system and utilises either spark or corona preionisation. It provides short output pulses of less than 100 ns at repetition rates of up to 1 kHz, optimised for efficient ultrasonic wave generation. The system has been designed for highly reliable operation under industrial conditions and a long term test with total pulse counts in excess of 5 billion laser pulses is reported.

Humidity Effect on Nanoscale Electrochemistry in Solid Silver Ion Conductors and the Dual Nature of Its Locality

DOE PAGES

Yang, Sangmo; Strelcov, Evgheni; Paranthaman, Mariappan Parans; ...

2015-01-07

Scanning probe microscopy (SPM) is a powerful tool to investigate electrochemistry in nanoscale volumes. While most SPM-based studies have focused on reactions at the tip-surface junction, charge and mass conservation requires coupled and intrinsically non-local cathodic and anodic processes that can be significantly affected by ambient humidity. Here, we explore the role of water in both cathodic and anodic processes, associated charge transport, and topographic volume changes depending on the polarity of tip bias. The first-order reversal curve current-voltage technique combined with simultaneous detection of the sample topography, referred to as FORC-IVz, was applied to a silver solid ion conductor.more » We found that the protons generated from water affect silver ionic conduction, silver particle formation and dissolution, and mechanical integrity of the material. This work highlights the dual nature (simultaneously local and non-local) of electrochemical SPM studies, which should be considered for comprehensive understanding of nanoscale electrochemistry.« less

Humidity effect on nanoscale electrochemistry in solid silver ion conductors and the dual nature of its locality.

PubMed

Yang, Sang Mo; Strelcov, Evgheni; Paranthaman, M Parans; Tselev, Alexander; Noh, Tae Won; Kalinin, Sergei V

2015-02-11

Scanning probe microscopy (SPM) is a powerful tool to investigate electrochemistry in nanoscale volumes. While most SPM-based studies have focused on reactions at the tip-surface junction, charge and mass conservation requires coupled and intrinsically nonlocal cathodic and anodic processes that can be significantly affected by ambient humidity. Here, we explore the role of water in both cathodic and anodic processes, associated charge transport, and topographic volume changes depending on the polarity of tip bias. The first-order reversal curve current-voltage technique combined with simultaneous detection of the sample topography, referred to as FORC-IVz, was applied to a silver solid ion conductor. We found that the protons generated from water affect silver ionic conduction, silver particle formation and dissolution, and mechanical integrity of the material. This work highlights the dual nature (simultaneously local and nonlocal) of electrochemical SPM studies, which should be considered for comprehensive understanding of nanoscale electrochemistry.

Multiplexed interfacial transduction of nucleic acid hybridization using a single color of immobilized quantum dot donor and two acceptors in fluorescence resonance energy transfer.

PubMed

Algar, W Russ; Krull, Ulrich J

2010-01-01

A multiplexed solid-phase assay for the detection of nucleic acid hybridization was developed on the basis of a single color of immobilized CdSe/ZnS quantum dot (QD) as a donor in fluorescence resonance energy transfer (FRET). This work demonstrated that two channels of detection did not necessitate two different QD donors. Two probe oligonucleotides were coimmobilized on optical fibers modified with QDs, and a sandwich assay was used to associate the acceptor dyes with interfacial hybridization events without target labeling. FRET-sensitized acceptor emission provided an analytical signal that was concentration dependent down to 10 nM. Changes in the ratio of coimmobilized probe oligonucleotides were found to yield linear changes in the relative amounts of acceptor emission. These changes were compared to previous studies that used mixed films of two QD donors for two detection channels. The analysis indicated that probe dilution effects were primarily driven by changes in acceptor number density and that QD dilution effects or changes in mean donor-acceptor distance were secondary. Hybridization kinetics were found to be consistent between different ratios of coimmobilized probes, suggesting that hybridization in this type of system occurred via the accepted model for solid-phase hybridization, where adsorption and then diffusion at the solid interface drove hybridization.

Hot tube method for the measuring of thermophysical properties of materials

NASA Astrophysics Data System (ADS)

Dieška, Peter; Boháč, Vlastimil; Vretenár, Viliam

2017-07-01

The measurement of thermal properties of materials that do not keep the form is problematic, because usually, the basic condition of the most models predicts constant dimensions. The plastic materials like clay or loam in natural condition always contain some water and thus are viscous and squeeze out of specimen holder when clamped even at weak force produced by specimen holder. Thus, the specimen dimensions are changing in during the measurement when it is not placed in a solid container. Even at this arrangement the shrinkage of material at the measurements causes the lowering the specimen thickness when using two probe method like pulse transient technique. This effect problem could be lowered or neglected at single probe techniques like the planar hot disk or this newly derived hot tube method. Hot tube method is derived for the probe made as the rectangular plane bended around the solid cylinder or tube made of thermally low conducting material. The probe generates the heat and the rate of temperature rise in it is driven by heat transfer ability of the measured surrounding material. Such a probe should be used in laboratory as well as in the field conditions.

Surface studies of solids using integral x-ray-induced photoemission yield

DOE PAGES

Stoupin, Stanislav; Zhernenkov, Mikhail; Shi, Bing

2016-11-22

X-ray induced photoemission yield contains structural information complementary to that provided by X-ray Fresnel reflectivity, which presents an advantage to a wide variety of surface studies if this information is made easily accessible. Photoemission in materials research is commonly acknowledged as a method with a probing depth limited by the escape depth of the photoelectrons. Here we show that the integral hard-X-ray-induced photoemission yield is modulated by the Fresnel reflectivity of a multilayer structure and carries structural information that extends well beyond the photoelectron escape depth. A simple electric self-detection of the integral photoemission yield and Fourier data analysis permitmore » extraction of thicknesses of individual layers. The approach does not require detection of the reflected radiation and can be considered as a framework for non-invasive evaluation of buried layers with hard X-rays under grazing incidence.« less

Surface studies of solids using integral X-ray-induced photoemission yield

PubMed Central

Stoupin, Stanislav; Zhernenkov, Mikhail; Shi, Bing

2016-01-01

X-ray induced photoemission yield contains structural information complementary to that provided by X-ray Fresnel reflectivity, which presents an advantage to a wide variety of surface studies if this information is made easily accessible. Photoemission in materials research is commonly acknowledged as a method with a probing depth limited by the escape depth of the photoelectrons. Here we show that the integral hard-X-ray-induced photoemission yield is modulated by the Fresnel reflectivity of a multilayer structure and carries structural information that extends well beyond the photoelectron escape depth. A simple electric self-detection of the integral photoemission yield and Fourier data analysis permit extraction of thicknesses of individual layers. The approach does not require detection of the reflected radiation and can be considered as a framework for non-invasive evaluation of buried layers with hard X-rays under grazing incidence. PMID:27874041

InP/ZnS nanocrystals: coupling NMR and XPS for fine surface and interface description.

PubMed

Virieux, Héloïse; Le Troedec, Marianne; Cros-Gagneux, Arnaud; Ojo, Wilfried-Solo; Delpech, Fabien; Nayral, Céline; Martinez, Hervé; Chaudret, Bruno

2012-12-05

Advanced (1)H, (13)C, and (31)P solution- and solid-state NMR studies combined with XPS were used to probe, at the molecular scale, the composition (of the core, the shell, and the interface) and the surface chemistry of InP/ZnS core/shell quantum dots prepared via a non-coordinating solvent strategy. The interface between the mismatched InP and ZnS phases is composed of an amorphous mixed oxide phase incorporating InPO(x) (with x = 3 and predominantly 4), In(2)O(3), and InO(y)(OH)(3-2y) (y = 0, 1). Thanks to the analysis of the underlying reaction mechanisms, we demonstrate that the oxidation of the upper part of the InP core is the consequence of oxidative conditions brought by decarboxylative coupling reactions (ketonization). These reactions occur during both the core preparation and the coating process, but according to different mechanisms.

Tribological properties of surfaces

NASA Technical Reports Server (NTRS)

Buckley, D. H.

1978-01-01

The real area of contact between two solid surfaces is only a small portion of the apparent area. Deformation of these areas can result in solid state contact through surface films. For clean solid to solid contact strong adhesive bonding occurs across the interface. Under these conditions many properties of the solid such as the metallurgical and chemical nature of metals can influence adhesion, friction, and wear behavior. The presence of gases, liquids, and solid films on the surface of solids alter markedly tribological characteristics. These surface films can also considerably change the mechanical effects of solid state contact on bulk material behavior.

Non-thermal processes on ice and liquid micro-jet surfaces

NASA Astrophysics Data System (ADS)

Olanrewaju, Babajide O.

The primary focus of this research is to investigate non-thermal processes occurring on ice surfaces and the photo-ejection of ions from liquid surfaces. Processes at the air-water/ice interface are known to play a very important role in the release of reactive halogen species with atmospheric aerosols serving as catalysts. The ability to make different types of ice with various morphologies, hence, different adsorption and surface properties in vacuum, provide a useful way to probe the catalytic effect of ice in atmospheric reactions. Also, the use of the liquid jet technique provides the rare opportunity to probe liquid samples at the interface; hitherto impossible to investigate with traditional surface science techniques. In Chapter 2, the effect of ice morphology on the release of reactive halogen species from photodissociation of adsorbed organic halides on ice will be presented. Quantum state resolved measurements of neutral atomic iodine from the photon irradiation of submonolayer coverages of methyl iodide adsorbed on low temperature water ice were conducted. Temperature programmed desorption (TPD) studies of methyl iodide adsorbed on ice were performed to provide information on the effect of ice morphology on the adsorption of submonolayer methyl iodide. The interaction and autoionization of HCl on low-temperature (80{140 K) water ice surfaces has been studied using low-energy (5-250 eV) electron-stimulated desorption (ESD) and temperature programmed desorption (TPD). A detailed ESD study of the interactions of low concentrations of HCl with low-temperature porous amorphous solid water (PASW), amorphous solid water (ASW) and crystalline ice (CI) surfaces will be presented in Chapter 3. The ESD cation yields from HCl adsorbed on ice, as well as the coverage dependence, kinetic energy distributions and TPD measurements were all monitored. Probing liquid surface using traditional surface science technique is usually difficult because of the problem of keeping the liquid surface clean and the distortion of information by the interference of equilibrium dense vapor above the liquid. By using the liquid jet technique the ejection of ions from surface of micron sized liquid can be adequately probed with a linear time-of-flight mass spectrometer. The photoionization of pure water and aqueous solutions of NaOH, NaCl and HCl is presented in Chapter 4. The aim of this investigation was to provide a fundamental understanding of the structure of water/vacuum interfaces. In Chapter 5, the ejection of ions from salt solutions containing divalent cations is also presented. The goal of the experiment was to figure out the solvation structure and reaction dynamics of divalent metal ions, M2+ on the surface of aqueous solution. A lot of work has been done in the gas phase either by a pickup-type cluster source or by collision induced dissociation of ejected ions from electrospray. For the first time the direct monitoring of ions ejected from liquid into gas phase is explored. Possible ejection mechanisms for the ejection of cations are discussed extensively in both Chapters 4 and 5. The results presented in this thesis is a combination of experiments performed at the Georgia Institute of Technology and the Pacific Northwest National Laboratory (PNNL) which includes experiments on ice and micro-jet respectively. The results in Chapters 2 and 3 have been submitted to the Journal of Chemical Physics and the Journal of Physical Chemistry respectively. It is important to note that the data presented in Chapter 3 was originally taken by Dr Janine Herring-Captain as part of her thesis work. It is also presented in this thesis due to effort in analyzing the data and preparation of the submitted manuscript. Chapter 4 and 5 represents papers which will also be submitted for publication in the open scientific literature. All the work leading to the results presented in these two chapters were done during my visit to PNNL and I would like to acknowledge that the instrumentation and data acquisition were done in collaboration with Nikolai Petrik and Greg Kimmel.

Molecular level studies on interfacial hydration of zwitterionic and other antifouling polymers in situ.

PubMed

Leng, Chuan; Sun, Shuwen; Zhang, Kexin; Jiang, Shaoyi; Chen, Zhan

2016-08-01

Antifouling polymers have wide applications in biomedical engineering and marine industry. Recently, zwitterionic materials have been reported as promising candidates for antifouling applications, while strong hydration is believed to be the key antifouling mechanism. Zwitterionic materials can be designed with various molecular structures, which affect their hydration and antifouling performance. Although strong hydration has been proposed to occur at the material surfaces, probing the solid material/water interfaces is challenging with traditional analytical techniques. Here in this review, we will review our studies on surface hydration of zwitterionic materials and other antifouling materials by using sum frequency generation (SFG) vibrational spectroscopy, which provides molecular understanding of the water structures at various material surfaces. The materials studied include zwitterionic polymer brushes with different molecular structures, amphiphilic polymers with zwitterionic groups, uncharged hydrophilic polymer brushes, amphiphilic polypeptoids, and widely used antifouling material poly(ethylene glycol). We will compare the differences among zwitterionic materials with various molecular structures as well as the differences between antifouling materials and fouling surfaces of control samples. We will also discuss the effects of pH and biological molecules like proteins on the surface hydration of the zwitterionic materials. Using SFG spectroscopy, we have measured the hydration layers of antifouling materials and found that strong hydrogen bonds are key to the formation of strong hydration layers preventing protein fouling at the polymer interfaces. Antifouling polymers have wide applications in biomedical engineering and marine industry. Recently, zwitterionic materials have been reported as promising candidates for antifouling applications, while strong hydration is believed to be the key antifouling mechanism. However, zwitterionic materials can be designed with various molecular structures, which affect their hydration and antifouling performance. Moreover, although strong hydration has been proposed to occur at the material surfaces, probing the solid material/water interfaces is challenging with traditional analytical techniques. Here in this manuscript, we will review our studies on surface hydration of zwitterionic materials and other antifouling materials by using sum frequency generation (SFG) vibrational spectroscopy, which provides molecular understanding of the water structures at various material surfaces. The materials studied include zwitterionic polymer brushes with different molecular structures, amphiphilic polymers with zwitterionic groups, uncharged hydrophilic polymer brushes, amphiphilic polypeptoids, and widely used antifouling material poly(ethylene glycol). We will compare the differences among zwitterionic materials with various molecular structures as well as the differences between antifouling materials and fouling surfaces of control samples. We will also discuss the effects of pH and biological molecules like proteins on the surface hydration of the zwitterionic materials. All the SFG results indicate that strongly hydrogen-bonded water at the materials' surfaces (strong surface hydration) is closely correlated to the good antifouling properties of the materials. This review will be widely interested by readers of Acta Biomaterialia and will impact many different research fields in chemistry, materials, engineering, and beyond. Copyright © 2016 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Positron Annihilation Induced Auger and Gamma Spectroscopy of Catalytically Important Surfaces

NASA Astrophysics Data System (ADS)

Weiss, A. H.; Nadesalingam, M. P.; Sundaramoorthy, R.; Mukherjee, S.; Fazleev, N. G.

2006-10-01

The annihilation of positrons with core electrons results in unique signatures in the spectra of Auger-electron and annihilation-gamma rays that can be used to make clear chemical identification of atoms at the surface. Because positrons implanted at low energies are trapped with high efficiency in the image-correlation well where they are localized just outside the surface it is possible to use annihilation induced Auger and Gamma signals to probe the surfaces of solids with single atomic layer depth resolution. In this talk we will report recent applications of Positron Annihilation Induced Auger Electron Spectroscopy (PAES) and Auger-Gamma Coincidence Spectroscopy (AGCS) to the study of surface structure and surface chemistry. Our research has demonstrated that PAES spectra can provide new information regarding the composition of the top-most atomic layer. Applications of PAES to the study of catalytically important surfaces of oxides and wide band-gap semiconductors including TiO2, SiO2,Cu2O, and SiC will be presented. We conclude with a discussion of the use of Auger-Gamma and Gamma-Gamma coincidence spectroscopy for the study of surfaces at pressures closer to those found in practical chemical reactors. Research supported by the Welch Foundation Grant Number Y-1100.

Active radiometer for self-calibrated furnace temperature measurements

DOEpatents

Woskov, Paul P.; Cohn, Daniel R.; Titus, Charles H.; Wittle, J. Kenneth; Surma, Jeffrey E.

1996-01-01

Radiometer with a probe beam superimposed on its field-of-view for furnace temperature measurements. The radiometer includes a heterodyne millimeter/submillimeter-wave receiver including a millimeter/submillimeter-wave source for probing. The receiver is adapted to receive radiation from a surface whose temperature is to be measured. The radiation includes a surface emission portion and a surface reflection portion which includes the probe beam energy reflected from the surface. The surface emission portion is related to the surface temperature and the surface reflection portion is related to the emissivity of the surface. The simultaneous measurement of surface emissivity serves as a real time calibration of the temperature measurement.

Determination of interfacial states in solid heterostructures using a variable-energy positron beam

DOEpatents

Asoka kumar, Palakkal P. V.; Lynn, Kelvin G.

1993-01-01

A method and means is provided for characterizing interfacial electron states in solid heterostructures using a variable energy positron beam to probe the solid heterostructure. The method includes the steps of directing a positron beam having a selected energy level at a point on the solid heterostructure so that the positron beam penetrates into the solid heterostructure and causes positrons to collide with the electrons at an interface of the solid heterostructure. The number and energy of gamma rays emitted from the solid heterostructure as a result of the annihilation of positrons with electrons at the interface are detected. The data is quantified as a function of the Doppler broadening of the photopeak about the 511 keV line created by the annihilation of the positrons and electrons at the interface, preferably, as an S-parameter function; and a normalized S-parameter function of the data is obtained. The function of data obtained is compared with a corresponding function of the Doppler broadening of the annihilation photopeak about 511 keV for a positron beam having a second energy level directed at the same material making up a portion of the solid heterostructure. The comparison of these functions facilitates characterization of the interfacial states of electrons in the solid heterostructure at points corresponding to the penetration of positrons having the particular energy levels into the interface of the solid heterostructure. Accordingly, the invention provides a variable-energy non-destructive probe of solid heterostructures, such as SiO.sub.2 /Si, MOS or other semiconductor devices.

Determination of interfacial states in solid heterostructures using a variable-energy positron beam

DOEpatents

Asokakumar, P.P.V.; Lynn, K.G.

1993-04-06

A method and means is provided for characterizing interfacial electron states in solid heterostructures using a variable energy positron beam to probe the solid heterostructure. The method includes the steps of directing a positron beam having a selected energy level at a point on the solid heterostructure so that the positron beam penetrates into the solid heterostructure and causes positrons to collide with the electrons at an interface of the solid heterostructure. The number and energy of gamma rays emitted from the solid heterostructure as a result of the annihilation of positrons with electrons at the interface are detected. The data is quantified as a function of the Doppler broadening of the photopeak about the 511 keV line created by the annihilation of the positrons and electrons at the interface, preferably, as an S-parameter function; and a normalized S-parameter function of the data is obtained. The function of data obtained is compared with a corresponding function of the Doppler broadening of the annihilation photopeak about 511 keV for a positron beam having a second energy level directed at the same material making up a portion of the solid heterostructure. The comparison of these functions facilitates characterization of the interfacial states of electrons in the solid heterostructure at points corresponding to the penetration of positrons having the particular energy levels into the interface of the solid heterostructure. Accordingly, the invention provides a variable-energy non-destructive probe of solid heterostructures, such as SiO[sub 2]/Si, MOS or other semiconductor devices.

Molecular-Level Design of Heterogeneous Chiral Catalysis

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

Francisco Zaera

2012-03-21

The following is a proposal to continue our multi-institutional research on heterogeneous chiral catalysis. Our team combines the use of surface-sensitive analytical techniques for the characterization of model systems with quantum and statistical mechanical calculations to interpret experimental data and guide the design of future research. Our investigation focuses on the interrelation among the three main mechanisms by which enantioselectivity can be bestowed to heterogeneous catalysts, namely: (1) by templating chirality via the adsorption of chiral supramolecular assemblies, (2) by using chiral modifiers capable of forming chiral complexes with the reactant and force enantioselective surface reactions, and (3) by formingmore » naturally chiral surfaces using imprinting chiral agents. Individually, the members of our team are leaders in these various aspects of chiral catalysis, but the present program provides the vehicle to generate and exploit the synergies necessary to address the problem in a comprehensive manner. Our initial work has advanced the methodology needed for these studies, including an enantioselective titration procedure to identify surface chiral sites, infrared spectroscopy in situ at the interface between gases or liquids and solids to mimic realistic catalytic conditions, and DFT and Monte Carlo algorithms to simulate and understand chirality on surfaces. The next step, to be funded by the monies requested in this proposal, is to apply those methods to specific problems in chiral catalysis, including the identification of the requirements for the formation of supramolecular surface structures with enantioselective behavior, the search for better molecules to probe the chiral nature of the modified surfaces, the exploration of the transition from supramolecular to one-to-one chiral modification, the correlation of the adsorption characteristics of one-to-one chiral modifiers with their physical properties, in particular with their configuration, and the development of ways to imprint chiral centers on achiral solid surfaces. Chiral catalysis is not only a problem of great importance in its own right, but also the ultimate test of how to control selectivity in catalysis. The time is ripe for fundamental work in heterogeneous chiral catalysis to provide the U.S. with a leadership role in developing the next generation of catalytic processes for medicinal and agrochemical manufacturing. Our team provides the required expertise for a synergistic and comprehensive integration of physical and chemical experimentation with solid state and molecular reactivity theories to solve this problem.« less

Hollow Au-Ag Nanoparticles Labeled Immunochromatography Strip for Highly Sensitive Detection of Clenbuterol

NASA Astrophysics Data System (ADS)

Wang, Jingyun; Zhang, Lei; Huang, Youju; Dandapat, Anirban; Dai, Liwei; Zhang, Ganggang; Lu, Xuefei; Zhang, Jiawei; Lai, Weihua; Chen, Tao

2017-01-01

The probe materials play a significant role in improving the detection efficiency and sensitivity of lateral-flow immunochromatographic test strip (ICTS). Unlike conventional ICTS assay usually uses single-component, solid gold nanoparticles as labeled probes, in our present study, a bimetallic, hollow Au-Ag nanoparticles (NPs) labeled ICTS was successfully developed for the detection of clenbuterol (CLE). The hollow Au-Ag NPs with different Au/Ag mole ratio and tunable size were synthesized by varying the volume ratio of [HAuCl4]:[Ag NPs] via the galvanic replacement reaction. The surface of hollow Ag-Au NPs was functionalized with 11-mercaptoundecanoic acid (MUA) for further covalently bonded with anti-CLE monoclonal antibody. Overall size of the Au-Ag NPs, size of the holes within individual NPs and also Au/Ag mole ratio have been systematically optimized to amplify both the visual inspection signals and the quantitative data. The sensitivity of optimized hollow Au-Ag NPs probes has been achieved even as low as 2 ppb in a short time (within 15 min), which is superior over the detection performance of conventional test strip using Au NPs. The optimized hollow Au-Ag NPs labeled test strip can be used as an ideal candidate for the rapid screening of CLE in food samples.

Innovative fiber systems for laser medicine and technology

NASA Astrophysics Data System (ADS)

Artiouchenko, Viatcheslav G.; Wojciechowski, Cezar

2003-10-01

Development of Polycrystalline Infrared (PIR-) fibers extruded from solid solutions of AgCl/AgBr has opened a new horizon of molecular spectroscopy applications in 4-18 micron range of spectra. PIR-fiber cables and probes could be coupled with a variety of Fourier Transform Infrared (FTIR) spectrometer and Tunable Diode Lasers (TDL), including pig tailing of Mercury Cadmium Tellurium (MCT) detectors. Using these techniques no sample preparation is necessary for PIR-fiber probes have been used to measure reflection and absorption spectra, in situ, in vivo, in real time and even multiplexed. Such PIR-fiber probes have been used for evanescent absorption spectroscopy of malignant tissue and skin surface diagnostics in-vivo, glucose detection in blood as well as crude oil composition analysis, for organic pollution and nuclear waste monitoring. A review of various PIR-fiber applications in medicine, industry and environment control is presented. The synergy of PIR-fibers flexibility with a super high spectral resolution of TDL spectrometers with Δv=10-4cm-1, provides the unique tool for gas analysis, specifically wiht PIR-fibers are coupled as pigtails with MCT-detectors and Pb-salt lasers. Design of multichannel PIR-fiber tailed TDL spectrometer could be used as a portable device for multispectral gas analysis as 1 ppb level of detectivity for various applications in medicine and biotechnology.

Innovative fiber systems for laser medicine and technology

NASA Astrophysics Data System (ADS)

Artiouchenko, Viatcheslav G.; Wojciechowski, Cezar

2004-09-01

Development of Polycrystalline Infrared (PIR-) fibers extruded from solid solutions of AgCl/AgBr has opened a new horizon of molecular spectroscopy applications in 4 - 18 micron range of spectra. PIR-fiber cables and probes could be coupled with a variety of Fourier Transform Infrared (FTIR) spectrometer and Tunable Diode Lasers (TDL), including pig tailing of Mercury Cadmium Tellurium (MCT) detectors. Using these techniques no sample preparation is necessary for PIR-fiber probes to measure reflection and absorption spectra, in situ, in vivo, in real time and even multiplexed. Such PIR-fiber probes have been used for evanescent absorption spectroscopy of malignant tissue and skin surface diagnostics in-vivo, glucose detection in blood as well as crude oil composition analysis, for organic pollution and nuclear waste monitoring. A review of various PIR-fiber applications in medicine, industry and environment control is presented. The synergy of PIR-fibers flexibility with a super high spectral resolution of TDL spectrometers with Δν=10-4cm-1, provides the unique tool for gas analysis, specifically when PIR-fibers are coupled as pigtails with MCT-detectors and Pb-salt lasers. Design of multichannel PIR-fiber tailed TDL spectrometer could be used as a portable device for multispectral gas analysis at 1 ppb level of detectivity for various applications in medicine and biotechnology.

Intracellular Biosynthesis of Fluorescent CdSe Quantum Dots in Bacillus subtilis: A Strategy to Construct Signaling Bacterial Probes for Visually Detecting Interaction Between Bacillus subtilis and Staphylococcus aureus.

PubMed

Yan, Zheng-Yu; Ai, Xiao-Xia; Su, Yi-Long; Liu, Xin-Ying; Shan, Xiao-Hui; Wu, Sheng-Mei

2016-02-01

In this work, fluorescent Bacillus subtilis (B. subtilis) cells were developed as probes for imaging applications and to explore behaviorial interaction between B. subtilis and Staphylococcus aureus (S. aureus). A novel biological strategy of coupling intracellular biochemical reactions for controllable biosynthesis of CdSe quantum dots by living B. subtilis cells was demonstrated, through which highly luminant and photostable fluorescent B. subtilis cells were achieved with good uniformity. With the help of the obtained fluorescent B. subtilis cells probes, S. aureus cells responded to co-cultured B. subtilis and to aggregate. The degree of aggregation was calculated and nonlinearly fitted to a polynomial model. Systematic investigations of their interactions implied that B. subtilis cells inhibit the growth of neighboring S. aureus cells, and this inhibition was affected by both the growth stage and the amount of surrounding B. subtilis cells. Compared to traditional methods of studying bacterial interaction between two species, such as solid culture medium colony observation and imaging mass spectrometry detection, the procedures were more simple, vivid, and photostable due to the efficient fluorescence intralabeling with less influence on the cells' surface, which might provide a new paradigm for future visualization of microbial behavior.

16 CFR § 1505.51 - Hot surfaces.

Code of Federal Regulations, 2013 CFR

2013-01-01

... CHILDREN Policies and Interpretations § 1505.51 Hot surfaces. (a) Test probe. Section 1505.6(g)(2) defines... inches long. To test for accessibility using this test probe, it shall be inserted no more than 3 inches into any opening in the toy. Unless the probe contacts a surface within 3 inches of the plane of the...

Formative Assessment Probes: Is It a Solid? Claim Cards and Argumentation

ERIC Educational Resources Information Center

Keeley, Page

2013-01-01

A "Framework for K-12 Science Education"'s disciplinary core idea PS1.A states that students should know by the end of grade 2 that different kinds of matter exist and many of them can be solid or liquid, depending on temperature (NRC 2012). By the end of grade 8, they describe solids, liquids, and gases by the arrangement and…

Optic probe for semiconductor characterization

DOEpatents

Sopori, Bhushan L [Denver, CO; Hambarian, Artak [Yerevan, AM

2008-09-02

Described herein is an optical probe (120) for use in characterizing surface defects in wafers, such as semiconductor wafers. The optical probe (120) detects laser light reflected from the surface (124) of the wafer (106) within various ranges of angles. Characteristics of defects in the surface (124) of the wafer (106) are determined based on the amount of reflected laser light detected in each of the ranges of angles. Additionally, a wafer characterization system (100) is described that includes the described optical probe (120).

A compact, high temperature nuclear magnetic resonance probe for use in a narrow-bore superconducting magnet

NASA Astrophysics Data System (ADS)

Adler, Stuart B.; Michaels, James N.; Reimer, Jeffrey A.

1990-11-01

The design of a nuclear magnetic resonance (NMR) probe is reported, that can be used in narrow-bore superconducting solenoids for the observation of nuclear induction at high temperatures. The probe is compact, highly sensitive, and stable in continuous operation at temperatures up to 1050 C. The essential feature of the probe is a water-cooled NMR coil that contains the sample-furnace; this design maximizes sensitivity and circuit stability by maintaining the probe electronics at ambient temperature. The design is demonstrated by showing high temperature O-17 NMR spectra and relaxation measurements in solid barium bismuth oxide and yttria-stabilized zirconia.

A peptide that inhibits hydroxyapatite growth is in an extended conformation on the crystal surface

PubMed Central

Long, Joanna R.; Dindot, John L.; Zebroski, Henry; Kiihne, Suzanne; Clark, Rutilio H.; Campbell, Allison A.; Stayton, Patrick S.; Drobny, Gary P.

1998-01-01

Proteins play an important role in the biological mechanisms controlling hard tissue development, but the details of molecular recognition at inorganic crystal interfaces remain poorly characterized. We have applied a recently developed homonuclear dipolar recoupling solid-state NMR technique, dipolar recoupling with a windowless sequence (DRAWS), to directly probe the conformation of an acidic peptide adsorbed to hydroxyapatite (HAP) crystals. The phosphorylated hexapeptide, DpSpSEEK (N6, where pS denotes phosphorylated serine), was derived from the N terminus of the salivary protein statherin. Constant-composition kinetic characterization demonstrated that, like the native statherin, this peptide inhibits the growth of HAP seed crystals when preadsorbed to the crystal surface. The DRAWS technique was used to measure the internuclear distance between two 13C labels at the carbonyl positions of the adjacent phosphoserine residues. Dipolar dephasing measured at short mixing times yielded a mean separation distance of 3.2 ± 0.1 Å. Data obtained by using longer mixing times suggest a broad distribution of conformations about this average distance. Using a more complex model with discrete α-helical and extended conformations did not yield a better fit to the data and was not consistent with chemical shift analysis. These results suggest that the peptide is predominantly in an extended conformation rather than an α-helical state on the HAP surface. Solid-state NMR approaches can thus be used to determine directly the conformation of biologically relevant peptides on HAP surfaces. A better understanding of peptide and protein conformation on biomineral surfaces may provide design principles useful for the modification of orthopedic and dental implants with coatings and biological growth factors that are designed to enhance biocompatibility with surrounding tissue. PMID:9770443

Selective Individual Primary Cell Capture Using Locally Bio-Functionalized Micropores

PubMed Central

Liu, Jie; Bombera, Radoslaw; Leroy, Loïc; Roupioz, Yoann; Baganizi, Dieudonné R.; Marche, Patrice N.; Haguet, Vincent; Mailley, Pascal; Livache, Thierry

2013-01-01

Background Solid-state micropores have been widely employed for 6 decades to recognize and size flowing unlabeled cells. However, the resistive-pulse technique presents limitations when the cells to be differentiated have overlapping dimension ranges such as B and T lymphocytes. An alternative approach would be to specifically capture cells by solid-state micropores. Here, the inner wall of 15-µm pores made in 10 µm-thick silicon membranes was covered with antibodies specific to cell surface proteins of B or T lymphocytes. The selective trapping of individual unlabeled cells in a bio-functionalized micropore makes them recognizable just using optical microscopy. Methodology/Principal Findings We locally deposited oligodeoxynucleotide (ODN) and ODN-conjugated antibody probes on the inner wall of the micropores by forming thin films of polypyrrole-ODN copolymers using contactless electro-functionalization. The trapping capabilities of the bio-functionalized micropores were validated using optical microscopy and the resistive-pulse technique by selectively capturing polystyrene microbeads coated with complementary ODN. B or T lymphocytes from a mouse splenocyte suspension were specifically immobilized on micropore walls functionalized with complementary ODN-conjugated antibodies targeting cell surface proteins. Conclusions/Significance The results showed that locally bio-functionalized micropores can isolate target cells from a suspension during their translocation throughout the pore, including among cells of similar dimensions in complex mixtures. PMID:23469221

Electrochemical detection of Francisella tularensis genomic DNA using solid-phase recombinase polymerase amplification.

PubMed

del Río, Jonathan Sabaté; Yehia Adly, Nouran; Acero-Sánchez, Josep Lluis; Henry, Olivier Y F; O'Sullivan, Ciara K

2014-04-15

Solid-phase isothermal DNA amplification was performed exploiting the homology protein recombinase A (recA). The system was primarily tested on maleimide activated microtitre plates as a proof-of-concept and later translated to an electrochemical platform. In both cases, forward primer for Francisella tularensis holarctica genomic DNA was surface immobilised via a thiol or an amino moiety and then elongated during the recA mediated amplification, carried out in the presence of specific target sequence and reverse primers. The formation of the subsequent surface tethered amplicons was either colorimetrically or electrochemically monitored using a horseradish peroxidase (HRP)-labelled DNA secondary probe complementary to the elongated strand. The amplification time was optimised to amplify even low amounts of DNA copies in less than an hour at a constant temperature of 37°C, achieving a limit of detection of 1.3×10(-13) M (4×10(6) copies in 50 μL) for the colorimetric assay and 3.3×10(-14) M (2×10(5) copies in 10 μL) for the chronoamperometric assay. The system was demonstrated to be highly specific with negligible cross-reactivity with non-complementary targets or primers. © 2013 Elsevier B.V. All rights reserved.

Dynamic Nuclear Polarization enhanced NMR at 187 GHz/284 MHz using an Extended Interaction Klystron amplifier.

PubMed

Kemp, Thomas F; Dannatt, Hugh R W; Barrow, Nathan S; Watts, Anthony; Brown, Steven P; Newton, Mark E; Dupree, Ray

2016-04-01

A Dynamic Nuclear Polarisation (DNP) enhanced solid-state Magic Angle Spinning (MAS) NMR spectrometer which uses a 187 GHz (corresponding to (1)H NMR frequency of 284 MHz) Extended Interaction Klystron (EIK) amplifier as the microwave source is briefly described. Its performance is demonstrated for a biomolecule (bacteriorhodopsin), a pharmaceutical, and surface functionalised silica. The EIK is very compact and easily incorporated into an existing spectrometer. The bandwidth of the amplifier is sufficient that it obviates the need for a sweepable magnetic field, once set, for all commonly used radicals. The variable power (CW or pulsed) output from the EIK is transmitted to the DNP-NMR probe using a quasi-optic system with a high power isolator and a corrugated waveguide which feeds the microwaves into the DNP-NMR probe. Curved mirrors inside the probe project the microwaves down the axis of the MAS rotor, giving a very efficient system such that maximum DNP enhancement is achieved with less than 3 W output from the microwave source. The DNP-NMR probe operates with a sample temperature down to 90K whilst spinning at 8 kHz. Significant enhancements, in excess of 100 for bacteriorhodopsin in purple membrane (bR in PM), are shown along with spectra which are enhanced by ≈25 with respect to room temperature, for both the pharmaceutical furosemide and surface functionalised silica. These enhancements allow hitherto prohibitively time consuming experiments to be undertaken. The power at which the DNP enhancement in bR in PM saturates does not change significantly between 90K and 170 K even though the enhancement drops by a factor of ≈11. As the DNP build up time decreases by a factor 3 over this temperature range, the reduction in T1n is presumably a significant contribution to the drop in enhancement. Copyright © 2016 The Authors. Published by Elsevier Inc. All rights reserved.

Optimization of ultrasound-assisted extraction of phenolic compounds from grapefruit (Citrus paradisi Macf.) leaves via D-optimal design and artificial neural network design with categorical and quantitative variables.

PubMed

Ciğeroğlu, Zeynep; Aras, Ömür; Pinto, Carlos A; Bayramoglu, Mahmut; Kırbaşlar, Ş İsmail; Lorenzo, José M; Barba, Francisco J; Saraiva, Jorge A; Şahin, Selin

2018-03-06

The extraction of phenolic compounds from grapefruit leaves assisted by ultrasound-assisted extraction (UAE) was optimized using response surface methodology (RSM) by means of D-optimal experimental design and artificial neural network (ANN). For this purpose, five numerical factors were selected: ethanol concentration (0-50%), extraction time (15-60 min), extraction temperature (25-50 °C), solid:liquid ratio (50-100 g L -1 ) and calorimetric energy density of ultrasound (0.25-0.50 kW L -1 ), whereas ultrasound probe horn diameter (13 or 19 mm) was chosen as categorical factor. The optimized experimental conditions yielded by RSM were: 10.80% for ethanol concentration; 58.52 min for extraction time; 30.37 °C for extraction temperature; 52.33 g L -1 for solid:liquid ratio; 0.457 kW L -1 for ultrasonic power density, with thick probe type. Under these conditions total phenolics content was found to be 19.04 mg gallic acid equivalents g -1 dried leaf. The same dataset was used to train multilayer feed-forward networks using different approaches via MATLAB, with ANN exhibiting superior performance to RSM (differences included categorical factor in one model and higher regression coefficients), while close values were obtained for the extraction variables under study, except for ethanol concentration and extraction time. © 2018 Society of Chemical Industry. © 2018 Society of Chemical Industry.

A scanning probe mounted on a field-effect transistor: Characterization of ion damage in Si.

PubMed

Shin, Kumjae; Lee, Hoontaek; Sung, Min; Lee, Sang Hoon; Shin, Hyunjung; Moon, Wonkyu

2017-10-01

We have examined the capabilities of a Tip-On-Gate of Field-Effect Transistor (ToGoFET) probe for characterization of FIB-induced damage in Si surface. A ToGoFET probe is the SPM probe which the Field Effect Transistor(FET) is embedded at the end of a cantilever and a Pt tip was mounted at the gate of FET. The ToGoFET probe can detect the surface electrical properties by measuring source-drain current directly modulated by the charge on the tip. In this study, a Si specimen whose surface was processed with Ga+ ion beam was prepared. Irradiation and implantation with Ga+ ions induce highly localized modifications to the contact potential. The FET embedded on ToGoFET probe detected the surface electric field profile generated by schottky contact between the Pt tip and the sample surface. Experimentally, it was shown that significant differences of electric field due to the contact potential barrier in differently processed specimens were observed using ToGOFET probe. This result shows the potential that the local contact potential difference can be measured by simple working principle with high sensitivity. Copyright © 2017 Elsevier Ltd. All rights reserved.

Liquid Microjunction Surface Sampling Probe Fluid Dynamics: Computational and Experimental Analysis of Coaxial Intercapillary Positioning Effects on Sample Manipulation

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

ElNaggar, Mariam S; Barbier, Charlotte N; Van Berkel, Gary J

A coaxial geometry liquid microjunction surface sampling probe (LMJ-SSP) enables direct extraction of analytes from surfaces for subsequent analysis by techniques like mass spectrometry. Solution dynamics at the probe-to-sample surface interface in the LMJ-SSP has been suspected to influence sampling efficiency and dispersion but has not been rigorously investigated. The effect on flow dynamics and analyte transport to the mass spectrometer caused by coaxial retraction of the inner and outer capillaries from each other and the surface during sampling with a LMJ-SSP was investigated using computational fluid dynamics and experimentation. A transparent LMJ-SSP was constructed to provide the means formore » visual observation of the dynamics of the surface sampling process. Visual observation, computational fluid dynamics (CFD) analysis, and experimental results revealed that inner capillary axial retraction from the flush position relative to the outer capillary transitioned the probe from a continuous sampling and injection mode through an intermediate regime to sample plug formationmode caused by eddy currents at the sampling end of the probe. The potential for analytical implementation of these newly discovered probe operational modes is discussed.« less

Active radiometer for self-calibrated furnace temperature measurements

DOEpatents

Woskov, P.P.; Cohn, D.R.; Titus, C.H.; Wittle, J.K.; Surma, J.E.

1996-11-12

A radiometer is described with a probe beam superimposed on its field-of-view for furnace temperature measurements. The radiometer includes a heterodyne millimeter/submillimeter-wave receiver including a millimeter/submillimeter-wave source for probing. The receiver is adapted to receive radiation from a surface whose temperature is to be measured. The radiation includes a surface emission portion and a surface reflection portion which includes the probe beam energy reflected from the surface. The surface emission portion is related to the surface temperature and the surface reflection portion is related to the emissivity of the surface. The simultaneous measurement of surface emissivity serves as a real time calibration of the temperature measurement. 5 figs.

Surface Morphology of Liquid and Solid Thin Films via X-Ray Reflectivity.

NASA Astrophysics Data System (ADS)

Shindler, Joseph Daniel

X-ray reflectivity can be used to measure the spatial variations in the electron density on length scales from Angstroms to microns. It is sensitive to atomic scale roughness, interdiffusion in buried layers, the thickness of multilayer stacks, and in-plane correlations in each of these cases. We have pioneered the use of a high intensity, moderate resolution configuration for x-ray reflectivity which utilizes a bent crystal graphite monochromator. With this technique we can obtain a beam intensity one hundred times greater than is possible using the high resolution rotating anode configuration, while we have shown that the resulting instrumental resolution is appropriate for the vast majority of thin film work. For all of the systems studied, we were able to measure the weak diffuse scattering signal to probe the in-plane length scales of interfacial roughness, a measurement which had previously only been attempted at synchrotron sources. Studied systems include thin films and surfaces with a wide range of structural order and surface morphologies. Interest in liquid films has been of a fundamental nature. Theories on the expected film evolution with changing thickness and temperature are currently being tested with scattering experiments. We have pursued the issues of film/substrate wetting and conformality, focussing on the temperature dependence of these phenomena near the triple point. Despite the heterogeneity of the substrate potential, we see a very sharp wetting transition at or near the triple point, although below the triple point the film is still smooth, consistent with a uniform layer. We also see a loss of conformality as the fluid films thicken; this is consistent with theory and with other recent experiments. The properties of a multilayer solid film depend not only on the magnitude of the roughness of each interface, but also on the conformality between interfaces and the length scales of the roughness--i.e., whether the roughness is on the atomic lengths of interdiffusion, crystalline order lengths of faceting, or even longer lengths due to other processes. In a joint project with Alcoa, we combined the methods of x-ray Bragg diffraction and small angle reflectivity to probe aluminum thin films as precursors to true multilayer films, correlating grain size and orientation with the magnitude and length-scales of surface roughness. We also correlated all film properties with such parameters as the deposition method, substrate roughness, and film thickness.

Influence of the side chain and substrate on polythiophene thin film surface, bulk, and buried interfacial structures.

PubMed

Xiao, Minyu; Jasensky, Joshua; Zhang, Xiaoxian; Li, Yaoxin; Pichan, Cayla; Lu, Xiaolin; Chen, Zhan

2016-08-10

The molecular structures of organic semiconducting thin films mediate the performance of various devices composed of such materials. To fully understand how the structures of organic semiconductors alter on substrates due to different polymer side chains and different interfacial interactions, thin films of two kinds of polythiophene derivatives with different side-chains, poly(3-hexylthiophene) (P3HT) and poly(3-potassium-6-hexanoate thiophene) (P3KHT), were deposited and compared on various surfaces. A combination of analytical tools was applied in this research: contact angle goniometry and X-ray photoelectron spectroscopy (XPS) were used to characterize substrate dielectric surfaces with varied hydrophobicity for polymer film deposition; X-ray diffraction and UV-vis spectroscopy were used to examine the polythiophene film bulk structure; sum frequency generation (SFG) vibrational spectroscopy was utilized to probe the molecular structures of polymer film surfaces in air and buried solid/solid interfaces. Both side-chain hydrophobicity and substrate hydrophobicity were found to mediate the crystallinity of the polythiophene film, as well as the orientation of the thiophene ring within the polymer backbone at the buried polymer/substrate interface and the polymer thin film surface in air. For the same type of polythiophene film deposited on different substrates, a more hydrophobic substrate surface induced thiophene ring alignment with the surface normal at both the buried interface and on the surface in air. For different films (P3HT vs. P3KHT) deposited on the same dielectric substrate, a more hydrophobic polythiophene side chain caused the thiophene ring to align more towards the surface at the buried polymer/substrate interface and on the surface in air. We believe that the polythiophene surface, bulk, and buried interfacial molecular structures all influence the hole mobility within the polythiophene film. Successful characterization of an organic conducting thin film surface, buried interfacial, and bulk structures is a first crucial step in understanding the structure-function relationship of such films in order to optimize device performance. An in-depth understanding on how the side-chain influences the interfacial and surface polymer orientation will guide the future molecular structure design of organic semiconductors.

Near-field vector intensity measurements of a small solid rocket motor.

PubMed

Gee, Kent L; Giraud, Jarom H; Blotter, Jonathan D; Sommerfeldt, Scott D

2010-08-01

Near-field vector intensity measurements have been made of a 12.7-cm diameter nozzle solid rocket motor. The measurements utilized a test rig comprised of four probes each with four low-sensitivity 6.35-mm pressure microphones in a tetrahedral arrangement. Measurements were made with the rig at nine positions (36 probe locations) within six nozzle diameters of the plume shear layer. Overall levels at these locations range from 135 to 157 dB re 20 microPa. Vector intensity maps reveal that, as frequency increases, the dominant source region contracts and moves upstream with peak directivity at greater angles from the plume axis.

Iron in solution with aluminum matrix after non-equilibrium processing: an atom probe tomography study

NASA Astrophysics Data System (ADS)

Saller, Brandon D.; Sha, Gang; Yang, Li Mei; Liu, Fan; Ringer, Simon P.; Schoenung, Julie M.

2017-03-01

In this paper, we report on the influence of rapid solidification and severe plastic deformation on the solid solubility of Fe in Al. Atom probe tomography, for the first time, was performed on fine (3-4 μm diameter) and coarse ( 100 μm) as-atomised Al-5 at.% Fe powder and cryomilled Al-5 at.% Fe powder. The atomised powders exhibited negligible Fe in solution with Al, whereas the cryomilled powder contained 2 at.% Fe in solution. Moreover, our results suggest that severe plastic deformation is preferable to atomisation/rapid solidification for increasing the non-equilibrium solid solubility of Fe in Al.

Studying Electrical Conductivity Using a 3D Printed Four-Point Probe Station

ERIC Educational Resources Information Center

Lu, Yang; Santino, Luciano M.; Acharya, Shinjita; Anandarajah, Hari; D'Arcy, Julio M.

2017-01-01

The design and fabrication of functional scientific instrumentation allows students to forge a link between commonly reported numbers and physical material properties. Here, a two-point and four-point probe station for measuring electrical properties of solid materials is fabricated via 3D printing utilizing an inexpensive benchtop…

Development and utilization of new diagnostics for dense-phase pneumatic transport. Quarterly technical progress report, October 1-December 31, 1989

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

Louge, M. Y.; Jenkins, J. T.

The main objective of this work is to develop probes for local measurements of solid velocity and holdup in dense gas-solid flows. In particular, capacitance probes are designed to measure local, time-dependent particle concentrations. In addition, a new optical fiber probe based on laser-induced-phosphorescence is developed to measure particle velocities. The principles for the capacitance and optical diagnostics were given in our first and second quarterly reports. In this reporting period, we have demonstrated with success the feasibility of the optical fiber probe. Another objective of this work is to develop a model of dense-phase conveying and to test thismore » model in a setup that incorporates our diagnostics. In this period, as a prelude to these modeling efforts scheduled for the third year of the contract, we have carried out additional computer simulations of rapid granular flows to verify the theories of Jenkins and Richman (1988) on the anisotropy of the second moment in simple shear. 2 refs., 5 figs.« less

Gas composition of fluid inclusions using solid probe mass spectrometry and its application to study of mineralizing processes

NASA Astrophysics Data System (ADS)

Guha, Jayanta; Lu, Huan-Zhang; Gagnon, Michel

1990-03-01

A quadrupole mass spectrometer and a solid probe which can be inserted directly into the ionization chamber have been used to analyze gas compositions of fluid inclusions. The probe holds a solid sample which can be heated continuously or stepwise from 30 to 750°C using variable heating rates. The decrepitated gas is released directly into the spectrometer source, thus reducing contamination. A Single Ion Monitoring mode program is used for the analysis, which is capable of detecting 26 preselected gases separately, and gases at picogram levels have been analyzed with this method. Each single burst of inclusions is detected and analyzed separately using a surface area integrator, and the computer program automatically traces the baseline above the background. Gas ratios are calculated for single bursts, or bursts over different ranges of temperature, as well as the sum of the total range. Routine petrographic and microthermometric analyses are used to determine the different generations of inclusions and their decrepitation temperatures. Then tiny pieces of the doubly polished section containing representative fluid inclusions or inclusions targeted for analysis are cut and introduced into the solid probe and heated accordingly. The principal gas species which have been analyzed are CO 2, CON 2 (not discriminated), H 2O, H 2S, and nearly all light hydrocarbons. Fluid inclusions from different host minerals such as quartz, fluorite, barite, and sulfides have also been analyzed. The most important advantage of this method is that analytical results can be correlated with specific inclusion types since a small amount of sample material is required which makes it easier to choose specific areas from doubly polished sections. Another advantage is its capability to match the presence of gases in inclusions in quartz with those in associated sulfides, thereby confirming or denying that similar fluids were trapped by both the minerals. More tests are underway to examine the use of fluid inclusion data from sulfides. Preliminary tests on samples from an Archean gold deposit indicate the potential of this method, not only to detect the presence of different gases in the fluid, but also to determine gas ratios of fluid inclusions rapidly and fairly accurately. It has previously been established through alteration assemblage studies that CO 2H 2O ratios of the fluid decreased outwards from the gold-bearing zones and the new fluid inclusion data confirm this. This method also detected the presence of other gases such as CO/N 2, CH 4, C 2H 6, and H 2S, indicating a multi-component C-O-N-H-S system. This method can be useful for both reconnaissance and detailed investigations where gas compositions of fluid inclusions are important for the understanding of fluid evolution processes.

CRYOCHEM, Thermodynamic Model for Cryogenic Chemical Systems: Solid-Vapor and Solid-Liquid-Vapor Phase Equilibria Toward Applications on Titan and Pluto

NASA Astrophysics Data System (ADS)

Tan, S. P.; Kargel, J. S.; Adidharma, H.; Marion, G. M.

2014-12-01

Until in-situ measurements can be made regularly on extraterrestrial bodies, thermodynamic models are the only tools to investigate the properties and behavior of chemical systems on those bodies. The resulting findings are often critical in describing physicochemical processes in the atmosphere, surface, and subsurface in planetary geochemistry and climate studies. The extremely cold conditions on Triton, Pluto and other Kuiper Belt Objects, and Titan introduce huge non-ideality that prevents conventional models from performing adequately. At such conditions, atmospheres as a whole—not components individually—are subject to phase equilibria with their equilibrium solid phases or liquid phases or both. A molecular-based thermodynamic model for cryogenic chemical systems, referred to as CRYOCHEM, the development of which is still in progress, was shown to reproduce the vertical composition profile of Titan's atmospheric methane measured by the Huygens probe (Tan et al., Icarus 2013, 222, 53). Recently, the model was also used to describe Titan's global circulation where the calculated composition of liquid in Ligeia Mare is consistent with the bathymetry and microwave absorption analysis of T91 Cassini fly-by data (Tan et al., 2014, submitted). Its capability to deal with equilibria involving solid phases has also been demonstrated (Tan et al., Fluid Phase Equilib. 2013, 360, 320). With all those previous works done, our attention is now shifting to the lower temperatures in Titan's tropopause and on Pluto's surface, where much technical development remains for CRYOCHEM to assure adequate performance at low temperatures. In these conditions, solid-vapor equilibrium (SVE) is the dominant phase behavior that determines the composition of the atmosphere and the existing ices. Another potential application is for the subsurface phase equilibrium, which also involves liquid, thus three-phase equilibrium: solid-liquid-vapor (SLV). This presentation will discuss the current state of CRYOCHEM in representing the SVE and SLV of chemical systems at temperatures and pressures relevant to Titan's tropopause and Pluto and the upper crusts of these objects.

Imaging the molecular dimensions and oligomerization of protein molecules at the solid-liquid interface by surface oriented molecular sizing (SOMS) microscopy

NASA Astrophysics Data System (ADS)

Waner, Mark Joseph

The structure and behavior of proteins at the solid/liquid interface is of great scientific interest. It has application both to fundamental biochemical understanding, as well as to biotechnological purposes. Interfaces play a critical role in many physiological processes. The mechanism of protein adsorption to surfaces is not very well understood. The current model put forth in much of the literature assumes a two step model. In the first step of this model the protein collides with the surface and adsorbs if its energy is sufficient to overcome the free energy of desorption of surface adsorbed solvent. The second step is often assumed to involve significant conformational change of the secondary and tertiary structure of the protein or enzyme, akin to denaturation. This unfolding of the protein would tend to indicate that loss of function would occur concomitantly, but studies have found very little loss in activity upon adsorption for a number of different protein systems. The recent development of the atomic force microscope (AFM) offers another tool for the examination of protein structure at liquid/solid interfaces. For atomically flat crystals the AFM has been used to determine atomic positions to <1 A resolution. In the case of samples with topographic features larger than atoms, the probe tip of the AFM 'convolutes' with the size and shape of surface features. This has hindered the use of AFM for molecular level structural determination of proteins at the liquid/solid interface. The work presented in this dissertation covers the development of the surface oriented molecular sizing (SOMS) technique which makes use of the angstrom height resolution of the AFM and a physically based mathematical framework for the analysis of the height distribution of adsorbed protein molecules. The surface adsorption and orientation (SAO) model is developed using statistical thermodynamics to model the expected height distributions for molecules adsorbed on a surface. The SOMS technique will be shown to be viable through studies of ferritin and concanavalin A (Con A) at the water/mica interface. Using this technique we are able to determine both the three-dimensional size and the oligomerization state of the adsorbed molecules. This technique will then be utilized for the examination of denaturation of Con A at the interface, by a number of mechanisms. Further, the structural and orientational changes in Con A as a function of pH will also be presented. The final chapter of this dissertation will present an extension of these studies to the deposition and structure of Con A thin films on mica.

Stretchable ultrasonic transducer arrays for three-dimensional imaging on complex surfaces

PubMed Central

Zhu, Xuan; Li, Xiaoshi; Chen, Zeyu; Chen, Yimu; Lei, Yusheng; Li, Yang; Nomoto, Akihiro; Zhou, Qifa; di Scalea, Francesco Lanza

2018-01-01

Ultrasonic imaging has been implemented as a powerful tool for noninvasive subsurface inspections of both structural and biological media. Current ultrasound probes are rigid and bulky and cannot readily image through nonplanar three-dimensional (3D) surfaces. However, imaging through these complicated surfaces is vital because stress concentrations at geometrical discontinuities render these surfaces highly prone to defects. This study reports a stretchable ultrasound probe that can conform to and detect nonplanar complex surfaces. The probe consists of a 10 × 10 array of piezoelectric transducers that exploit an “island-bridge” layout with multilayer electrodes, encapsulated by thin and compliant silicone elastomers. The stretchable probe shows excellent electromechanical coupling, minimal cross-talk, and more than 50% stretchability. Its performance is demonstrated by reconstructing defects in 3D space with high spatial resolution through flat, concave, and convex surfaces. The results hold great implications for applications of ultrasound that require imaging through complex surfaces. PMID:29740603

Laser-based ultrasonics by dual-probe interferometer detection and narrow-band ultrasound generation

NASA Astrophysics Data System (ADS)

Huang, Jin

1993-01-01

Despite the advantages of laser-based ultrasonic (LBU) systems, the overall sensitivity of LBU systems needs to be improved for practical applications. Progress is reported to achieve better LBU detection accuracy and sensitivity for applications with surface waves and Lamb waves. A novel dual-probe laser interferometer has been developed to measure the same signal at two points. The dual-probe interferometer is a modification of a conventional single-probe interferometer in that the reference beam is guided to a second detecting point on the specimen surface to form a differential measurement mode, which measure the difference of the displacements at the two points. This dual-probe interferometer is particularly useful for accurate measurements of the speed and attenuation of surface waves and Lamb waves. The dual-probe interferometer has been applied to obtain accurate measurements of the surface wave speed and attenuation on surfaces of increasing surface roughness. It has also been demonstrated that with an appropriate signal processing method, namely, the power cepstrum method, the dual-probe interferometer is applicable to measure the local surface wave speed even when the probe separation is so small that the two waveforms in the interferometer output signal overlap in the time domain. Narrow-band signal generation and detection improve the sensitivity of LBU systems. It is proposed to use a diffraction grating to form an array of illuminating strips which form a source of narrowband surface and Lamb waves. The line-array of thermoelastic sources generates narrow-band signals whose frequency and bandwidth can be easily controlled. The optimum line-array parameters, such as width, spacing and the number of lines in the array have been derived theoretically and verified experimentally. Narrow-band signal generation with optimum parameters has been demonstrated. The enhanced LBU system with dual-probe detection and narrowband signal generation has been successfully applied to the detection of cracks emanating from rivet holes in aircraft fuselage panel samples. A compact fiber-optic dual-probe interferometer has also been developed and applied to the above mentioned problem of crack detection. Results agree well with those obtained with a bulk LBU system.

Single-Molecule Interfacial Electron Transfer

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

Ho, Wilson

Interfacial electron transfer (ET) plays an important role in many chemical and biological processes. Specifically, interfacial ET in TiO 2-based systems is important to solar energy technology, catalysis, and environmental remediation technology. However, the microscopic mechanism of interfacial ET is not well understood with regard to atomic surface structure, molecular structure, bonding, orientation, and motion. In this project, we used two complementary methodologies; single-molecule fluorescence spectroscopy, and scanning-tunneling microscopy and spectroscopy (STM and STS) to address this scientific need. The goal of this project was to integrate these techniques and measure the molecular dependence of ET between adsorbed molecules andmore » TiO 2 semiconductor surfaces and the ET induced reactions such as the splitting of water. The scanning probe techniques, STM and STS, are capable of providing the highest spatial resolution but not easily time-resolved data. Single-molecule fluorescence spectroscopy is capable of good time resolution but requires further development to match the spatial resolution of the STM. The integrated approach involving Peter Lu at Bowling Green State University (BGSU) and Wilson Ho at the University of California, Irvine (UC Irvine) produced methods for time and spatially resolved chemical imaging of interfacial electron transfer dynamics and photocatalytic reactions. An integral aspect of the joint research was a significant exchange of graduate students to work at the two institutions. This project bridged complementary approaches to investigate a set of common problems by working with the same molecules on a variety of solid surfaces, but using appropriate techniques to probe under ambient (BGSU) and ultrahigh vacuum (UCI) conditions. The molecular level understanding of the fundamental interfacial electron transfer processes obtained in this joint project will be important for developing efficient light harvesting, solar energy conversion, and broadly applicable to problems in interface chemistry and surface physics.« less

The Harp probe - An in situ Bragg scattering sensor

NASA Technical Reports Server (NTRS)

Mollo-Christensen, E.; Huang, N. E.; Long, S. R.; Bliven, L. F.

1984-01-01

A wave sensor, consisting of parallel, evenly spaced capacitance wires, whose output is the sum of the water surface deflections at the wires, has been built and tested in a wave tank. The probe output simulates Bragg scattering of electromagnetic waves from a water surface with waves; it can be used to simulate electromagnetic probing of the sea surface by radar. The study establishes that the wave probe, called the 'Harp' for short, will simulate Bragg scattering and that it can also be used to study nonlinear wave processes.

Design and Optimization of Nanomaterials for Sensing Applications

NASA Astrophysics Data System (ADS)

Sanderson, Robert Noboru

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

Molecular dynamics analysis of a equilibrium nanoscale droplet on a solid surface with periodic roughness

NASA Astrophysics Data System (ADS)

Furuta, Yuma; Surblys, Donatas; Yamaguchi, Yastaka

2016-11-01

Molecular dynamics simulations of the equilibrium wetting behavior of hemi-cylindrical argon droplets on solid surfaces with a periodic roughness were carried out. The rough solid surface is located at the bottom of the calculation cell with periodic boundary conditions in surface lateral directions and mirror boundary condition at the top boundary. Similar to on a smooth surface, the change of the cosine of the droplet contact angle was linearly correlated to the potential well depth of the inter-atomic interaction between liquid and solid on a surface with a short roughness period while the correlation was deviated on one with a long roughness period. To further investigate this feature, solid-liquid, solid-vapor interfacial free energies per unit projected area of solid surface were evaluated by using the thermodynamic integration method in independent quasi-one-dimensional simulation systems with a liquid-solid interface or vapor-solid interface on various rough solid surfaces at a constant pressure. The cosine of the apparent contact angles estimated from the density profile of the droplet systems corresponded well with ones calculated from Young's equation using the interfacial energies evaluated in the quasi-one dimensional systems.

Parametric computational study of sheaths in multicomponent Ar/O2 plasma

NASA Astrophysics Data System (ADS)

Hromadka, J.; Ibehej, T.; Hrach, R.

2018-02-01

Our study is devoted to sheath structures emerging in Ar/O2 plasma. By means of two dimensional PIC/MCC computer model two configurations were investigated - sheath structure in the vicinity of a cylindrical Langmuir probe for two different biases and changes of the sheath structure when a cylindrical probe passes into a semi-planar probe. It was shown that O+ ions play important role in shielding out negative bias of a solid immersed in Ar/O2 plasma and edge effects of a semi-planar probe on its sheath structure were evaluated.

Mediated Electron Transfer at Vertically Aligned Single-Walled Carbon Nanotube Electrodes During Detection of DNA Hybridization.

PubMed

Wallen, Rachel; Gokarn, Nirmal; Bercea, Priscila; Grzincic, Elissa; Bandyopadhyay, Krisanu

2015-12-01

Vertically aligned single-walled carbon nanotube (VASWCNT) assemblies are generated on cysteamine and 2-mercaptoethanol (2-ME)-functionalized gold surfaces through amide bond formation between carboxylic groups generated at the end of acid-shortened single-walled carbon nanotubes (SWCNTs) and amine groups present on the gold surfaces. Atomic force microscopy (AFM) imaging confirms the vertical alignment mode of SWCNT attachment through significant changes in surface roughness compared to bare gold surfaces and the lack of any horizontally aligned SWCNTs present. These SWCNT assemblies are further modified with an amine-terminated single-stranded probe-DNA. Subsequent hybridization of the surface-bound probe-DNA in the presence of complementary strands in solution is followed using impedance measurements in the presence of Fe(CN)6 (3-/4-) as the redox probe in solution, which show changes in the interfacial electrochemical properties, specifically the charge-transfer resistance, due to hybridization. In addition, hybridization of the probe-DNA is also compared when it is attached directly to the gold surfaces without any intermediary SWCNTs. Contrary to our expectations, impedance measurements show a decrease in charge-transfer resistance with time due to hybridization with 300 nM complementary DNA in solution with the probe-DNA attached to SWCNTs. In contrast, an increase in charge-transfer resistance is observed with time during hybridization when the probe-DNA is attached directly to the gold surfaces. The decrease in charge-transfer resistance during hybridization in the presence of VASWCNTs indicates an enhancement in the electron transfer process of the redox probe at the VASWCNT-modified electrode. The results suggest that VASWCNTs are acting as mediators of electron transfer, which facilitate the charge transfer of the redox probe at the electrode-solution interface.

Mediated Electron Transfer at Vertically Aligned Single-Walled Carbon Nanotube Electrodes During Detection of DNA Hybridization

NASA Astrophysics Data System (ADS)

Wallen, Rachel; Gokarn, Nirmal; Bercea, Priscila; Grzincic, Elissa; Bandyopadhyay, Krisanu

2015-06-01

Vertically aligned single-walled carbon nanotube (VASWCNT) assemblies are generated on cysteamine and 2-mercaptoethanol (2-ME)-functionalized gold surfaces through amide bond formation between carboxylic groups generated at the end of acid-shortened single-walled carbon nanotubes (SWCNTs) and amine groups present on the gold surfaces. Atomic force microscopy (AFM) imaging confirms the vertical alignment mode of SWCNT attachment through significant changes in surface roughness compared to bare gold surfaces and the lack of any horizontally aligned SWCNTs present. These SWCNT assemblies are further modified with an amine-terminated single-stranded probe-DNA. Subsequent hybridization of the surface-bound probe-DNA in the presence of complementary strands in solution is followed using impedance measurements in the presence of Fe(CN)6 3-/4- as the redox probe in solution, which show changes in the interfacial electrochemical properties, specifically the charge-transfer resistance, due to hybridization. In addition, hybridization of the probe-DNA is also compared when it is attached directly to the gold surfaces without any intermediary SWCNTs. Contrary to our expectations, impedance measurements show a decrease in charge-transfer resistance with time due to hybridization with 300 nM complementary DNA in solution with the probe-DNA attached to SWCNTs. In contrast, an increase in charge-transfer resistance is observed with time during hybridization when the probe-DNA is attached directly to the gold surfaces. The decrease in charge-transfer resistance during hybridization in the presence of VASWCNTs indicates an enhancement in the electron transfer process of the redox probe at the VASWCNT-modified electrode. The results suggest that VASWCNTs are acting as mediators of electron transfer, which facilitate the charge transfer of the redox probe at the electrode-solution interface.

Li Distribution Heterogeneity in Solid Electrolyte Li10GeP2S12 upon Electrochemical Cycling Probed by 7Li MRI.

PubMed

Chien, Po-Hsiu; Feng, Xuyong; Tang, Mingxue; Rosenberg, Jens T; O'Neill, Sean; Zheng, Jin; Grant, Samuel C; Hu, Yan-Yan

2018-04-19

All-solid-state rechargeable batteries embody the promise for high energy density, increased stability, and improved safety. However, their success is impeded by high resistance for mass and charge transfer at electrode-electrolyte interfaces. Li deficiency has been proposed as a major culprit for interfacial resistance, yet experimental evidence is elusive due to the challenges associated with noninvasively probing the Li distribution in solid electrolytes. In this Letter, three-dimensional 7 Li magnetic resonance imaging (MRI) is employed to examine Li distribution homogeneity in solid electrolyte Li 10 GeP 2 S 12 within symmetric Li/Li 10 GeP 2 S 12 /Li batteries. 7 Li MRI and the derived histograms reveal Li depletion from the electrode-electrolyte interfaces and increased heterogeneity of Li distribution upon electrochemical cycling. Significant Li loss at interfaces is mitigated via facile modification with a poly(ethylene oxide)/bis(trifluoromethane)sulfonimide Li salt thin film. This study demonstrates a powerful tool for noninvasively monitoring the Li distribution at the interfaces and in the bulk of all-solid-state batteries as well as a convenient strategy for improving interfacial stability.

Two-dimensional ice mapping of molecular cores

NASA Astrophysics Data System (ADS)

Noble, J. A.; Fraser, H. J.; Pontoppidan, K. M.; Craigon, A. M.

2017-06-01

We present maps of the column densities of H2O, CO2 and CO ices towards the molecular cores B 35A, DC 274.2-00.4, BHR 59 and DC 300.7-01.0. These ice maps, probing spatial distances in molecular cores as low as 2200 au, challenge the traditional hypothesis that the denser the region observed, the more ice is present, providing evidence that the relationships between solid molecular species are more varied than the generic picture we often adopt to model gas-grain chemical processes and explain feedback between solid phase processes and gas phase abundances. We present the first combined solid-gas maps of a single molecular species, based upon observations of both CO ice and gas phase C18O towards B 35A, a star-forming dense core in Orion. We conclude that molecular species in the solid phase are powerful tracers of 'small-scale' chemical diversity, prior to the onset of star formation. With a component analysis approach, we can probe the solid phase chemistry of a region at a level of detail greater than that provided by statistical analyses or generic conclusions drawn from single pointing line-of-sight observations alone.

Array of nucleic acid probes on biological chips for diagnosis of HIV and methods of using the same

DOEpatents

Chee, Mark; Gingeras, Thomas R.; Fodor, Stephen P. A.; Hubble, Earl A.; Morris, MacDonald S.

1999-01-19

The invention provides an array of oligonucleotide probes immobilized on a solid support for analysis of a target sequence from a human immunodeficiency virus. The array comprises at least four sets of oligonucleotide probes 9 to 21 nucleotides in length. A first probe set has a probe corresponding to each nucleotide in a reference sequence from a human immunodeficiency virus. A probe is related to its corresponding nucleotide by being exactly complementary to a subsequence of the reference sequence that includes the corresponding nucleotide. Thus, each probe has a position, designated an interrogation position, that is occupied by a complementary nucleotide to the corresponding nucleotide. The three additional probe sets each have a corresponding probe for each probe in the first probe set. Thus, for each nucleotide in the reference sequence, there are four corresponding probes, one from each of the probe sets. The three corresponding probes in the three additional probe sets are identical to the corresponding probe from the first probe or a subsequence thereof that includes the interrogation position, except that the interrogation position is occupied by a different nucleotide in each of the four corresponding probes.

Formation and properties of surface-anchored polymer assemblies with tunable physico-chemical characteristics

NASA Astrophysics Data System (ADS)

Wu, Tao

We describe two new methodologies leading to the formation of novel surface-anchored polymer assemblies on solid substrates. While the main goal is to understand the fundamentals pertaining to the preparation and properties of the surface-bound polymer assemblies (including neutral and chargeable polymers), several examples also are mentioned throughout the Thesis that point out to practical applications of such structures. The first method is based on generating assemblies comprising anchored polymers with a gradual variation of grafting densities on solid substrates. These structures are prepared by first covering the substrate with a molecular gradient of the polymerization initiator, followed by polymerization from these substrate-bound initiator centers ("grafting from"). We apply this technique to prepare grafting density gradients of poly(acryl amide) (PAAm) and poly(acrylic acid) (PAA) on silica-covered substrates. We show that using the grafting density gradient geometry, the characteristics of surface-anchored polymers in both the low grafting density ("mushroom") regime as well as the high grafting density ("brush") regime can be accessed conveniently on a single sample. We use a battery of experimental methods, including Fourier transform infrared spectroscopy (FTIR), Near-edge absorption fine structure spectroscopy (NEXAFS), contact angle, ellipsometry, to study the characteristics of the surface-bound polymer layers. We also probe the scaling laws of neutral polymer as a function of grafting density, and for weak polyelectrolyte, in addition to the grafting density, we study the affect of solution ionic strength and pH values. In the second novel method, which we coined as "mechanically assisted polymer assembly" (MAPA), we form surface anchored polymers by "grafting from" polymerization initiators deposited on elastic surfaces that have been previously extended uniaxially by a certain length increment, Deltax. Upon releasing the strain in the substrate after completion of polymerization, we show the grafting density of the polymers grafted to flexible substrates can be tuned as a function of Deltax.

Fe-Impregnated Mineral Colloids for Peroxide Activation: Effects of Mineral Substrate and Fe Precursor.

PubMed

Li, Yue; Machala, Libor; Yan, Weile

2016-02-02

Heterogeneous iron species at the mineral/water interface are important catalysts for the generation of reactive oxygen species at circumneutral pH. One significant pathway leading to the formation of such species arises from deposition of dissolved iron onto mineral colloids due to changes in redox conditions. This study investigates the catalytic properties of Fe impregnated on silica, alumina, and titania nanoparticles (as prototypical mineral colloids). Fe impregnation was carried out by immersing the mineral nanoparticles in dilute Fe(II) or Fe(III) solutions at pH 6 and 3, respectively, in an aerobic environment. The uptake of iron per unit surface area follows the order of nTiO2 > nAl2O3 > nSiO2 for both types of Fe precursors. Impregnation of mineral particles in Fe(II) solutions results in predominantly Fe(III) species due to efficient surface-mediated oxidation. The catalytic activity of the impregnated solids to produce hydroxyl radical (·OH) from H2O2 decomposition was evaluated using benzoic acid as a probe compound under dark conditions. Invariably, the rates of benzoic acid oxidation with different Fe-laden particles increase with the surface density of Fe until a critical density above which the catalytic activity approaches a plateau, suggesting active Fe species are formed predominantly at low surface loadings. The critical surface density of Fe varies with the mineral substrate as well as the aqueous Fe precursor. Fe impregnated on TiO2 exhibits markedly higher activity than its Al2O3 and SiO2 counterparts. The speciation of interfacial Fe is analyzed with diffuse reflectance UV-vis analysis and interpretation of the data in the context of benzoic oxidation rates suggests that the surface activity of the solids for ·OH generation correlates strongly with the isolated (i.e., mononuclear) Fe species. Therefore, iron dispersed on mineral colloids is a significant form of reactive iron surfaces in the aquatic environment.

Conductive-probe atomic force microscopy characterization of silicon nanowire

PubMed Central

2011-01-01

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

Using tobacco mosaic virus to probe enhanced surface diffusion of molecular glasses.

PubMed

Zhang, Yue; Potter, Richard; Zhang, William; Fakhraai, Zahra

2016-11-09

Recent studies have shown that diffusion on the surface of organic glasses can be many orders of magnitude faster than bulk diffusion. Developing new probes that can readily measure surface diffusion can help study the effect of parameters such as chemical structure, intermolecular interaction, molecules' shape and size on the enhanced surface diffusion. In this study, we develop a novel probe that significantly simplifies these types of studies. Tobacco mosaic virus (TMV) is used as probe particle to measure surface diffusion coefficient of molecular glass N,N'-bis(3-methylphenyl)-N,N'-diphenylbenzidine (TPD). The evolution of the meniscus formed around TMV is probed as a function of time at various temperatures. TMV has a well-defined, mono-dispersed, cylindrical shape, with a large aspect-ratio (average diameter of 16.6 nm, length of 300 nm). As such, the shape of the meniscus around the center of TMV is semi-two dimensional, which compared to using a nanosphere as probe, increases the driving force for meniscus formation and simplifies the analysis of surface diffusion. We show that under these conditions, after a short transient time the shape of the meniscus is self-similar, allowing accurate determination of the surface diffusion coefficient. Measurements at various temperatures are then performed to investigate the temperature dependence of the surface diffusion coefficient. It is found that surface diffusion is greatly enhanced in TPD and has a lower activation barrier compared to the bulk counterpart. These observations are consistent with previous studies of surface diffusion on molecular glasses, demonstrating the accuracy of this method.

Pump-probe Kelvin-probe force microscopy: Principle of operation and resolution limits

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

Murawski, J.; Graupner, T.; Milde, P., E-mail: peter.milde@tu-dresden.de

Knowledge on surface potential dynamics is crucial for understanding the performance of modern-type nanoscale devices. We describe an electrical pump-probe approach in Kelvin-probe force microscopy that enables a quantitative measurement of dynamic surface potentials at nanosecond-time and nanometer-length scales. Also, we investigate the performance of pump-probe Kelvin-probe force microscopy with respect to the relevant experimental parameters. We exemplify a measurement on an organic field effect transistor that verifies the undisturbed functionality of our pump-probe approach in terms of simultaneous and quantitative mapping of topographic and electronic information at a high lateral and temporal resolution.

Advancements in non-contact metrology of asphere and diffractive optics

NASA Astrophysics Data System (ADS)

DeFisher, Scott

2017-11-01

Advancements in optical manufacturing technology allow optical designers to implement steep aspheric or high departure surfaces into their systems. Measuring these surfaces with profilometers or CMMs can be difficult due to large surface slopes or sharp steps in the surface. OptiPro has developed UltraSurf to qualify the form and figure of steep aspheric and diffractive optics. UltraSurf is a computer controlled, non-contact coordinate measuring machine. It incorporates five air-bearing axes, linear motors, high-resolution feedback, and a non-contact probe. The measuring probe is scanned over the optical surface while maintaining perpendicularity and a constant focal offset. Multiple probe technologies are available on UltraSurf. Each probe has strengths and weaknesses relative to the material properties, surface finish, and figure error of an optical component. The measuring probes utilize absolute distance to resolve step heights and diffractive surface patterns. The non-contact scanning method avoids common pitfalls with stylus contact instruments. Advancements in measuring speed and precision has enabled fast and accurate non-contact metrology of diffractive and steep aspheric surfaces. The benefits of data sampling with twodimensional profiles and three-dimensional topography maps will be presented. In addition, accuracy, repeatability, and machine qualification will be discussed with regards to aspheres and diffractive surfaces.

In Situ Real-Time Mechanical and Morphological Characterization of Electrodes for Electrochemical Energy Storage and Conversion by Electrochemical Quartz Crystal Microbalance with Dissipation Monitoring.

PubMed

Shpigel, Netanel; Levi, Mikhael D; Sigalov, Sergey; Daikhin, Leonid; Aurbach, Doron

2018-01-16

Quartz crystal microbalance with dissipation monitoring (QCM-D) generates surface-acoustic waves in quartz crystal plates that can effectively probe the structure of films, particulate composite electrodes of complex geometry rigidly attached to quartz crystal surface on one side and contacting a gas or liquid phase on the other side. The output QCM-D characteristics consist of the resonance frequency (MHz frequency range) and resonance bandwidth measured with extra-ordinary precision of a few tenths of Hz. Depending on the electrodes stiffness/softness, QCM-D operates either as a gravimetric or complex mechanical probe of their intrinsic structure. For at least 20 years, QCM-D has been successfully used in biochemical and environmental science and technology for its ability to probe the structure of soft solvated interfaces. Practical battery and supercapacitor electrodes appear frequently as porous solids with their stiffness changing due to interactions with electrolyte solutions or as a result of ion intercalation/adsorption and long-term electrode cycling. Unfortunately, most QCM measurements with electrochemical systems are carried out based on a single (fundamental) frequency and, as such, provided that the resonance bandwidth remains constant, are suitable for only gravimetric sensing. The multiharmonic measurements have been carried out mainly on conducting/redox polymer films rather than on typical composite battery/supercapacitor electrodes. Here, we summarize the most recent publications devoted to the development of electrochemical QCM-D (EQCM-D)-based methodology for systematic characterization of mechanical properties of operating battery/supercapacitor electrodes. By varying the electrodes' composition and structure (thin/thick layers, small/large particles, binders with different mechanical properties, etc.), nature of the electrolyte solutions and charging/cycling conditions, the method is shown to be operated in different application modes. A variety of useful electrode-material properties are assessed noninvasively, in situ, and in real time frames of ion intercalation into the electrodes of interest. A detailed algorithm for the mechanical characterization of battery electrodes kept in the gas phase and immersed into the electrolyte solutions has been developed for fast recognition of stiff and viscoelastic materials in terms of EQCM-D signatures treated by the hydrodynamic and viscoelastic models. Working examples of the use of in situ hydrodynamic spectroscopy to characterize stiff rough/porous solids of complex geometry and viscoelastic characterization of soft electrodes are presented. The most demonstrative example relates to the formation of solid electrolyte interphase on Li 4 Ti 5 O 12 electrodes in the presence of different electrolyte solutions and additives: only a few cycles (an experiment during ∼30 min) were required for screening the electrolyte systems for their ability to form high-quality surface films in experimental EQCM-D cells as compared to 100 cycles (200 h cycling) in conventional coin cells. Thin/small-mass electrodes required for the EQCM-D analysis enable accelerated cycling tests for ultrafast mechanical characterization of these electrodes in different electrolyte solutions. Hence, this methodology can be easily implemented as a highly effective in situ analytical tool in the field of energy storage and conversion.

Eddy current probe with foil sensor mounted on flexible probe tip and method of use

DOEpatents

Viertl, John R. M.; Lee, Martin K.

2001-01-01

A pair of copper coils are embedded in the foil strip. A first coil of the pair generates an electromagnetic field that induces eddy currents on the surface, and the second coil carries a current influenced by the eddy currents on the surface. The currents in the second coil are analyzed to obtain information on the surface eddy currents. An eddy current probe has a metal housing having a tip that is covered by a flexible conductive foil strip. The foil strip is mounted on a deformable nose at the probe tip so that the strip and coils will conform to the surface to which they are applied.

Laminar Boundary Layer Stability Measurements at Mach 7 Including Wall Temperature Effects

DTIC Science & Technology

1977-11-01

Diagnostics were done by a four-probe rake bearing a pitot tube, a To probe and two hot films - a boundary layer hot film probe (BLHF) and a freestream hot...tunnel. Inset shows hot film probe close to the surface with second probe positioned higher to sample simultaneously the frcestream turbulence ( pitot ... rake away from the surface by small increments and taking readings at each stop. The readings were simultaneously recorded and reduced by the Tunnel B

Test probe for surface mounted leadless chip carrier

DOEpatents

Meyer, Kerry L.; Topolewski, John

1989-05-23

A test probe for a surface mounted leadless chip carrier is disclosed. The probed includes specially designed connector pins which allow size reductions in the probe. A thermoplastic housing provides spring action to ensure good mechanical and electrical contact between the pins and the contact strips of a leadless chip carrier. Other features include flexible wires molded into the housing and two different types of pins alternately placed in the housing. These features allow fabrication of a smaller and simpler test probe.

Test probe for surface mounted leadless chip carrier

DOEpatents

Meyer, K.L.; Topolewski, J.

1987-10-02

A test probe for a surface mounted leadless chip carrier is disclosed. The probe includes specially designed connector pins which allow size reductions in the probe. A thermoplastic housing provides spring action to ensure good mechanical and electrical contact between the pins and the contact strips of a leadless chip carrier. Other features include flexible wires molded into the housing and two different types of pins alternately placed in the housing. These features allow fabrication of a smaller and simpler test probe. 1 fig.

Modeling and visualization of carrier motion in organic films by optical second harmonic generation and Maxwell-displacement current

NASA Astrophysics Data System (ADS)

Iwamoto, Mitsumasa; Manaka, Takaaki; Taguchi, Dai

2015-09-01

The probing and modeling of carrier motions in materials as well as in electronic devices is a fundamental research subject in science and electronics. According to the Maxwell electromagnetic field theory, carriers are a source of electric field. Therefore, by probing the dielectric polarization caused by the electric field arising from moving carriers and dipoles, we can find a way to visualize the carrier motions in materials and in devices. The techniques used here are an electrical Maxwell-displacement current (MDC) measurement and a novel optical method based on the electric field induced optical second harmonic generation (EFISHG) measurement. The MDC measurement probes changes of induced charge on electrodes, while the EFISHG probes nonlinear polarization induced in organic active layers due to the coupling of electron clouds of molecules and electro-magnetic waves of an incident laser beam in the presence of a DC field caused by electrons and holes. Both measurements allow us to probe dynamical carrier motions in solids through the detection of dielectric polarization phenomena originated from dipolar motions and electron transport. In this topical review, on the basis of Maxwell’s electro-magnetism theory of 1873, which stems from Faraday’s idea, the concept for probing electron and hole transport in solids by using the EFISHG is discussed in comparison with the conventional time of flight (TOF) measurement. We then visualize carrier transit in organic devices, i.e. organic field effect transistors, organic light emitting diodes, organic solar cells, and others. We also show that visualizing an EFISHG microscopic image is a novel way for characterizing anisotropic carrier transport in organic thin films. We also discuss the concept of the detection of rotational dipolar motions in monolayers by means of the MDC measurement, which is capable of probing the change of dielectric spontaneous polarization formed by dipoles in organic monolayers. Finally we conclude that the ideas and experiments on EFISHG and MDC lead to a novel way of analyzing dynamical motions of electrons, holes, and dipoles in solids, and thus are available in organic electronic device application.

Melting probes revisited - Ice penetration experiments under Mars surface pressure conditions

NASA Astrophysics Data System (ADS)

Kömle, Norbert I.; Tiefenbacher, Patrick; Weiss, Peter; Bendiukova, Anastasiia

2018-07-01

Melting probes as vehicles to explore terrestrial ice sheets have been designed and applied successfully since the early 1960's. Later on, in the 1990's, various proposals were made to apply such probes also as a means to explore ice sheets on other bodies of the solar system, e.g. Jupiter's icy satellite Europa or the ice caps of Mars. For this type of subsurface probes the name cryobot has become common. We review both early developments and more recent efforts to develop probes for application in planetary environments, i.e. under low pressures and low temperatures. The current state of art as well as the pros and cons of the different concepts hitherto considered are described. While many tests with various probes have been done in terrestrial environments, experiments under low surface pressure conditions are rare. Therefore, we report here on lab tests with a simple melting probe under the range of pressure and temperature conditions that would be encountered on the surface of Mars and compare them with corresponding tests under a much lower gas pressure, possibly representative for icy satellites. The contribution of evaporation during the melting and its variation with surface pressure is also considered. All surface pressure measurements that have been performed on Mars up to now indicate a surface pressure above the water triple point pressure (612 Pa). This means that water ice always transforms into the liquid phase when warmed up to 0°C, before it evaporates into the ambient atmosphere. The temporary existence of the liquid phase around the heated tip of the cryobot allows good thermal conductance between probe and surrounding ice, which is an important pre-requisite for efficient melt penetration. Our experiments indicate that under all possible Mars surface pressures the liquid phase is present when the probe is heated up. This finding confirms experimentally that a probe as it was proposed by Paige (1992) for in situ exploration of the Mars north polar layers would work in the expected way, although the penetration velocity must be expected be lower than under Earth pressure conditions. A test with the same probe, but under an almost two orders of magnitude lower gas pressure than on Mars, still indicates the temporary existence of the liquid phase in the contact region between the probe and the surrounding ice.

The study of surface wetting, nanobubbles and boundary slip with an applied voltage: A review.

PubMed

Pan, Yunlu; Bhushan, Bharat; Zhao, Xuezeng

2014-01-01

The drag of fluid flow at the solid-liquid interface in the micro/nanoscale is an important issue in micro/nanofluidic systems. Drag depends on the surface wetting, nanobubbles, surface charge and boundary slip. Some researchers have focused on the relationship between these interface properties. In this review, the influence of an applied voltage on the surface wettability, nanobubbles, surface charge density and slip length are discussed. The contact angle (CA) and contact angle hysteresis (CAH) of a droplet of deionized (DI) water on a hydrophobic polystyrene (PS) surface were measured with applied direct current (DC) and alternating current (AC) voltages. The nanobubbles in DI water and three kinds of saline solution on a PS surface were imaged when a voltage was applied. The influence of the surface charge density on the nanobubbles was analyzed. Then the slip length and the electrostatic force on the probe were measured on an octadecyltrichlorosilane (OTS) surface with applied voltage. The influence of the surface charge on the boundary slip and drag of fluid flow has been discussed. Finally, the influence of the applied voltage on the surface wetting, nanobubbles, surface charge, boundary slip and the drag of liquid flow are summarized. With a smaller surface charge density which could be achieved by applying a voltage on the surface, larger and fewer nanobubbles, a larger slip length and a smaller drag of liquid flow could be found.

Particle trapping in 3-D using a single fiber probe with an annular light distribution.

PubMed

Taylor, R; Hnatovsky, C

2003-10-20

A single optical fiber probe has been used to trap a solid 2 ìm diameter glass bead in 3-D in water. Optical confinement in 2-D was produced by the annular light distribution emerging from a selectively chemically etched, tapered, hollow tipped metalized fiber probe. Confinement of the bead in 3-D was achieved by balancing an electrostatic force of attraction towards the tip and the optical scattering force pushing the particle away from the tip.

Fast probe of local electronic states in nanostructures utilizing a single-lead quantum dot

PubMed Central

Otsuka, Tomohiro; Amaha, Shinichi; Nakajima, Takashi; Delbecq, Matthieu R.; Yoneda, Jun; Takeda, Kenta; Sugawara, Retsu; Allison, Giles; Ludwig, Arne; Wieck, Andreas D.; Tarucha, Seigo

2015-01-01

Transport measurements are powerful tools to probe electronic properties of solid-state materials. To access properties of local electronic states in nanostructures, such as local density of states, electronic distribution and so on, micro-probes utilizing artificial nanostructures have been invented to perform measurements in addition to those with conventional macroscopic electronic reservoirs. Here we demonstrate a new kind of micro-probe: a fast single-lead quantum dot probe, which utilizes a quantum dot coupled only to the target structure through a tunneling barrier and fast charge readout by RF reflectometry. The probe can directly access the local electronic states with wide bandwidth. The probe can also access more electronic states, not just those around the Fermi level, and the operations are robust against bias voltages and temperatures. PMID:26416582

Tribological behavior of micro/nano-patterned surfaces in contact with AFM colloidal probe

NASA Astrophysics Data System (ADS)

Zhang, Xiaoliang; Wang, Xiu; Kong, Wen; Yi, Gewen; Jia, Junhong

2011-10-01

In effort to investigate the influence of the micro/nano-patterning or surface texturing on the nanotribological properties of patterned surfaces, the patterned polydimethylsiloxane (PDMS) surfaces with pillars were fabricated by replica molding technique. The surface morphologies of patterned PDMS surfaces with varying pillar sizes and spacing between pillars were characterized by atomic force microscope (AFM) and scanning electron microscope (SEM). The AFM/FFM was used to acquire the friction force images of micro/nano-patterned surfaces using a colloidal probe. A difference in friction force produced a contrast on the friction force images when the colloidal probe slid over different regions of the patterned polymer surfaces. The average friction force of patterned surface was related to the spacing between the pillars and their size. It decreased with the decreasing of spacing between the pillars and the increasing of pillar size. A reduction in friction force was attributed to the reduced area of contact between patterned surface and colloidal probe. Additionally, the average friction force increased with increasing applied load and sliding velocity.

Hybrid catadioptric system for advanced optical cavity velocimetry

DOEpatents

Frayer, Daniel K.

2018-02-06

A probe including reflector is disclosed to measure the velocity distribution of a moving surface along many lines of sight. Laser light, directed to the surface by the probe and then reflected back from the surface, is Doppler shifted by the moving surface, collected into probe, and then directed to detection equipment through optic fibers. The received light is mixed with reference laser light and using photonic Doppler velocimetry, a continuous time record of the surface movement is obtained. An array of single-mode optical fibers provides an optic signal to one or more lens groups and a reflector, such as a parabolic reflector having a mirrored interior surface.

Reversible electrochemical modification of the surface of a semiconductor by an atomic-force microscope probe

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

Kozhukhov, A. S., E-mail: antonkozhukhov@yandex.ru; Sheglov, D. V.; Latyshev, A. V.

A technique for reversible surface modification with an atomic-force-microscope (AFM) probe is suggested. In this method, no significant mechanical or topographic changes occur upon a local variation in the surface potential of a sample under the AFM probe. The method allows a controlled relative change in the ohmic resistance of a channel in a Hall bridge within the range 20–25%.

Solid Lubrication Fundamentals and Applications. Properties of Clean Surfaces: Adhesion, Friction, and Wear

NASA Technical Reports Server (NTRS)

Miyoshi, Kazuhisa

1998-01-01

This chapter presents the adhesion, friction, and wear behaviors of smooth, atomically clean surfaces of solid-solid couples, such as metal-ceramic couples, in a clean environment. Surface and bulk properties, which determine the adhesion, friction, and wear behaviors of solid-solid couples, are described. The primary emphasis is on the nature and character of the metal, especially its surface energy and ductility. Also, the mechanisms of friction and wear for clean, smooth surfaces are stated.

Eliminating Size-Associated Diffusion Constraints for Rapid On-Surface Bioassays with Nanoparticle Probes.

PubMed

Li, Junwei; Zrazhevskiy, Pavel; Gao, Xiaohu

2016-02-24

Nanoparticle probes enable implementation of advanced on-surface assay formats, but impose often underappreciated size-associated constraints, in particular on assay kinetics and sensitivity. The present study highlights substantially slower diffusion-limited assay kinetics due to the rapid development of a nanoprobe depletion layer next to the surface, which static incubation and mixing of bulk solution employed in conventional assay setups often fail to disrupt. In contrast, cyclic solution draining and replenishing yields reaction-limited assay kinetics irrespective of the probe size. Using common surface bioassays, enzyme-linked immunosorbent assays and immunofluorescence, this study shows that this conceptually distinct approach effectively "erases" size-dependent diffusion constraints, providing a straightforward route to rapid on-surface bioassays employing bulky probes and procedures involving multiple labeling cycles, such as multicycle single-cell molecular profiling. For proof-of-concept, the study demonstrates that the assay time can be shortened from hours to minutes with the same probe concentration and, at a typical incubation time, comparable target labeling can be achieved with up to eight times lower nanoprobe concentration. The findings are expected to enable realization of novel assay formats and stimulate development of rapid on-surface bioassays with nanoparticle probes. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Quantum Dot Surface Engineering: Toward Inert Fluorophores with Compact Size and Bright, Stable Emission

PubMed Central

Lim, Sung Jun; Ma, Liang; Schleife, André; Smith, Andrew M.

2016-01-01

The surfaces of colloidal nanocrystals are complex interfaces between solid crystals, coordinating ligands, and liquid solutions. For fluorescent quantum dots, the properties of the surface vastly influence the efficiency of light emission, stability, and physical interactions, and thus determine their sensitivity and specificity when they are used to detect and image biological molecules. But after more than 30 years of study, the surfaces of quantum dots remain poorly understood and continue to be an important subject of both experimental and theoretical research. In this article, we review the physics and chemistry of quantum dot surfaces and describe approaches to engineer optimal fluorescent probes for applications in biomolecular imaging and sensing. We describe the structure and electronic properties of crystalline facets, the chemistry of ligand coordination, and the impact of ligands on optical properties. We further describe recent advances in compact coatings that have significantly improved their properties by providing small hydrodynamic size, high stability and fluorescence efficiency, and minimal nonspecific interactions with cells and biological molecules. While major progress has been made in both basic and applied research, many questions remain in the chemistry and physics of quantum dot surfaces that have hindered key breakthroughs to fully optimize their properties. PMID:28344357

Local structures of mesoporous bioactive glasses and their surface alterations in vitro: inferences from solid-state nuclear magnetic resonance

PubMed Central

Gunawidjaja, Philips N.; Mathew, Renny; Lo, Andy Y. H.; Izquierdo-Barba, Isabel; García, Ana; Arcos, Daniel; Mattias Edén, María Vallet-Regí

2012-01-01

We review the benefits of using 29Si and 1H magic angle spinning (MAS) nuclear magnetic resonance (NMR) spectroscopy for probing the local structures of both bulk and surface portions of mesoporous bioactive glasses (MBGs) of the CaO–SiO2−(P2O5) system. These mesoporous materials exhibit an ordered pore arrangement, and are promising candidates for improved bone and tooth implants. We discuss experimental MAS NMR results from three MBGs displaying different Ca, Si and P contents: the 29Si NMR spectra were recorded either directly by employing radio-frequency pulses to 29Si, or by magnetization transfers from neighbouring protons using cross polarization, thereby providing quantitative information about the silicate speciation present in the pore wall and at the MBG surface, respectively. The surface modifications were monitored for the three MBGs during their immersion in a simulated body fluid (SBF) for intervals between 30 min and one week. The results were formulated as a reaction sequence describing the interconversions between the distinct silicate species. We generally observed a depletion of Ca2+ ions at the MBG surface, and a minor condensation of the silicate-surface network over one week of SBF soaking. PMID:22349247

Surface enhanced Raman gene probe and methods thereof

DOEpatents

Vo-Dinh, T.

1998-09-29

The subject invention disclosed herein is a new gene probe biosensor and methods based on surface enhanced Raman scattering (SERS) label detection. The SER gene probe biosensor comprises a support means, a SER gene probe having at least one oligonucleotide strand labeled with at least one SERS label, and a SERS active substrate disposed on the support means and having at least one of the SER gene probes adsorbed thereon. Biotargets such as bacterial and viral DNA, RNA and PNA are detected using a SER gene probe via hybridization to oligonucleotide strands complementary to the SER gene probe. The support means supporting the SERS active substrate includes a fiberoptic probe, an array of fiberoptic probes for performance of multiple assays and a waveguide microsensor array with charge-coupled devices or photodiode arrays. 18 figs.

Surface enhanced Raman gene probe and methods thereof

DOEpatents

Vo-Dinh, Tuan

1998-01-01

The subject invention disclosed herein is a new gene probe biosensor and methods thereof based on surface enhanced Raman scattering (SERS) label detection. The SER gene probe biosensor comprises a support means, a SER gene probe having at least one oligonucleotide strand labeled with at least one SERS label, and a SERS active substrate disposed on the support means and having at least one of the SER gene probes adsorbed thereon. Biotargets such as bacterial and viral DNA, RNA and PNA are detected using a SER gene probe via hybridization to oligonucleotide strands complementary to the SER gene probe. The support means supporting the SERS active substrate includes a fiberoptic probe, an array of fiberoptic probes for performance of multiple assays and a waveguide microsensor array with charge-coupled devices or photodiode arrays.

Surface enhanced Raman gene probe and methods thereof

DOEpatents

Vo-Dinh, T.

1998-02-24

The subject invention disclosed is a new gene probe biosensor and methods based on surface enhanced Raman scattering (SERS) label detection. The SER gene probe biosensor comprises a support means, a SER gene probe having at least one oligonucleotide strand labeled with at least one SERS label, and a SERS active substrate disposed on the support means and having at least one of the SER gene probes adsorbed thereon. Biotargets such as bacterial and viral DNA, RNA and PNA are detected using a SER gene probe via hybridization to oligonucleotide strands complementary to the SER gene probe. The support means includes a fiberoptic probe, an array of fiberoptic probes for performance of multiple assays and a waveguide microsensor array with charge-coupled devices or photodiode arrays. 18 figs.

Surface enhanced Raman gene probe and methods thereof

DOEpatents

Vo-Dinh, T.

1998-07-21

The subject invention disclosed is a new gene probe biosensor and methods based on surface enhanced Raman scattering (SERS) label detection. The SER gene probe biosensor comprises a support means, a SER gene probe having at least one oligonucleotide strand labeled with at least one SERS label, and a SERS active substrate disposed on the support means and having at least one of the SER gene probes adsorbed. Biotargets such as bacterial and viral DNA, RNA and PNA are detected using a SER gene probe via hybridization to oligonucleotide strands complementary to the SER gene probe. The support means supporting the SERS active substrate includes a fiberoptic probe, an array of fiberoptic probes for performance of multiple assays and a waveguide microsensor array with charge-coupled devices or photodiode arrays. 18 figs.

Solid-state NMR imaging system

DOEpatents

Gopalsami, Nachappa; Dieckman, Stephen L.; Ellingson, William A.

1992-01-01

An apparatus for use with a solid-state NMR spectrometer includes a special imaging probe with linear, high-field strength gradient fields and high-power broadband RF coils using a back projection method for data acquisition and image reconstruction, and a real-time pulse programmer adaptable for use by a conventional computer for complex high speed pulse sequences.

Femtosecond fluorescence dynamics of porphyrin in solution and solid films: the effects of aggregation and interfacial electron transfer between porphyrin and TiO2.

PubMed

Luo, Liyang; Lo, Chen-Fu; Lin, Ching-Yao; Chang, I-Jy; Diau, Eric Wei-Guang

2006-01-12

The excited-state relaxation dynamics of a synthetic porphyrin, ZnCAPEBPP, in solution, coated on a glass substrate as solid films, mixed with PMMA and coated on a glass substrate as solid films, and sensitized on nanocrystalline TiO2 films were investigated by using femtosecond fluorescence up-conversion spectroscopy with excitation in the Soret band, S2. We found that the S2--> S1 electronic relaxation of ZnCAPEBPP in solution and on PMMA films occurs in 910 and 690 fs, respectively, but it becomes extremely rapid, <100 fs, in solid films and TiO2 films due to formation of porphyrin aggregates. When probed in the S1 state of porphyrin, the fluorescence transients of the solid films show a biphasic kinetic feature with the rapid and slow components decaying in 1.9-2.4 and 19-26 ps, respectively. The transients in ZnCAPEBPP/TiO2 films also feature two relaxation processes but they occur on different time scales, 100-300 fs and 0.8-4.1 ps, and contain a small offset. According to the variation of relaxation period as a function of molecular density on a TiO2 surface, we assigned the femtosecond component of the TiO2 films as due to indirect interfacial electron transfer through a phenylethynyl bridge attached to one of four meso positions of the porphyrin ring, and the picosecond component arising from intermolecular energy transfer among porphyrins. The observed variation of aggregate-induced relaxation periods between solid and TiO2 films is due mainly to aggregation of two types: J-type aggregation is dominant in the former case whereas H-type aggregation prevails in the latter case.

Methods of and apparatus for levitating an eddy current probe

DOEpatents

Stone, William J.

1988-05-03

An eddy current probe is supported against the force of gravity with an air earing while being urged horizontally toward the specimen being examined by a spring and displaced horizontally against the force of the spring pneumatically. The pneumatic displacement is accomplished by flowing air between a plenum chamber fixed with respect to the probe and the surface of the specimen. In this way, the surface of the specimen can be examined without making mechanical contact therewith while precisely controlling the distance at which the probe stands-off from the surface of the specimen.

Surface topography acquisition method for double-sided near-right-angle structured surfaces based on dual-probe wavelength scanning interferometry.

PubMed

Zhang, Tao; Gao, Feng; Jiang, Xiangqian

2017-10-02

This paper proposes an approach to measure double-sided near-right-angle structured surfaces based on dual-probe wavelength scanning interferometry (DPWSI). The principle and mathematical model is discussed and the measurement system is calibrated with a combination of standard step-height samples for both probes vertical calibrations and a specially designed calibration artefact for building up the space coordinate relationship of the dual-probe measurement system. The topography of the specially designed artefact is acquired by combining the measurement results with white light scanning interferometer (WLSI) and scanning electron microscope (SEM) for reference. The relative location of the two probes is then determined with 3D registration algorithm. Experimental validation of the approach is provided and the results show that the method is able to measure double-sided near-right-angle structured surfaces with nanometer vertical resolution and micrometer lateral resolution.

Heated Surface Temperatures Measured by Infrared Detector in a Cascade Environment

NASA Technical Reports Server (NTRS)

Boyle, Robert J.

2002-01-01

Investigators have used infrared devices to accurately measure heated surface temperatures. Several of these applications have been for turbine heat transfer studies involving film cooling and surface roughness, typically, these measurements use an infrared camera positioned externally to the test section. In cascade studies, where several blades are used to ensure periodic flow, adjacent blades block the externally positioned camera's views of the test blade. To obtain a more complete mapping of the surface temperatures, researchers at the NASA Glenn Research Center fabricated a probe with an infrared detector to sense the blade temperatures. The probe size was kept small to minimize the flow disturbance. By traversing and rotating the probe, using the same approach as for total pressure surveys, one can find the blade surface temperatures. Probe mounted infrared detectors are appropriate for measuring surface temperatures where an externally positioned infrared camera is unable to completely view the test object. This probe consists of a 8-mm gallium arsenide (GaAs) lens mounted in front of a mercury-cadmium-zinc-tellurium (HgCdZnTe) detector. This type of photovoltaic detector was chosen because of its high sensitivity to temperature when the detector is uncooled. The particular application is for relatively low surface temperatures, typically ambient to 100 C. This requires a detector sensitive at long wavelengths. The detector is a commercial product enclosed in a 9-mm-diameter package. The GaAs lens material was chosen because of its glass-like hardness and its good long-wavelength transmission characteristics. When assembled, the 6.4-mm probe stem is held in the traversing actuator. Since the entire probe is above the measurement plane, the flow field disturbance in the measurement plane is minimized. This particular probe body is somewhat wider than necessary, because it was designed to have replaceable detectors and lenses. The signal for the detector is fed through the hollow probe body. The detector's signal goes to an externally mounted preamplifier. The detector assembly, along with a preamplifier, is calibrated as a function of the surface temperature for various detector temperatures. The output voltage is a function of both the detector and object temperatures.

Stable glow discharge detector

DOEpatents

Koo, Jackson C.; Yu, Conrad M.

2004-05-18

A highly sensitive electronic ion cell for the measurement of trace elements in He carrier gas which involves glow discharge. A constant wave (CW) stable glow discharge detector which is controlled through a biased resistor, can detect the change of electron density caused by impurities in the He carrier gas by many orders of magnitude larger than that caused by direct ionization or electron capture. The stable glow discharge detector utilizes a floating pseudo-electrode to form a probe in or near the plasma and a solid rod electrode. By using this probe, the large variation of electron density due to trace amounts of impurities can be directly measured. The solid rod electrode provides greater stability and thus easier alignment.

Heat transfer fouling characteristics of microfiltered thin stillage from the dry grind process.

PubMed

Arora, Amit; Dien, Bruce S; Belyea, Ronald L; Singh, Vijay; Tumbleson, M E; Rausch, Kent D

2010-08-01

We investigated effects of microfiltration (MF) on heat transfer fouling tendencies of thin stillage. A stainless steel MF membrane (0.1 micron pore size) was used to remove solids from thin stillage. At filtration conditions of 690kPa, the MF process effectively recovered total solids from thin stillage. Thin stillage was concentrated from 7.0% to 22.4% solids with average permeate flux rates of 180+/-30 L/m(2)/h at 75 degrees C. In retentate streams, protein and fat contents were increased from 23.5 and 16.7% db to 27.6 and 31.1% db, respectively, and ash content was reduced from 10.5% to 3.8% db. Removal of solids, protein and fat generated a microfiltration permeate (MFP) that was used as an input stream to the fouling probe system; MFP fouling tendencies were measured. An annular fouling probe was used to measure fouling tendencies of thin stillage from a commercial dry grind facility. When comparing diluted thin stillage (DTS) stream and MFP, a reduction in solids concentration was not the only reason of fouling decrement. Selective removal of protein and fat played an important role in mitigating the fouling. At t=10h, mean fouling rates of MFP were an order of magnitude lower when compared to thin stillage and diluted streams. When maximum probe temperature (200 degrees C) was reached, mean fouling rates for thin stillage, DTS and MFP were 7.1x10(-4), 4.2x10(-4) and 2.6x10(-4) m(2) degrees C/kW/min, respectively. In DTS and MFP, the induction period was prolonged by factors of 4.3 and 9.5, respectively, compared to the induction period for thin stillage fouling. Mean fouling rates were decreased by factors of 2.3 and 23.4 for DTS and MFP, respectively. Fouling of MFP took twice the time to reach a probe temperature of 200 degrees C than did thin stillage (22 h vs 10 h, respectively). A reduction in heat transfer fouling could be achieved by altering process stream composition using microfiltration. Copyright 2010 Elsevier Ltd. All rights reserved.

Darkfield microspectroscopy of nanostructures on silver tip-enhanced Raman scattering probes

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

Itoh, Tamitake, E-mail: tamitake-itou@aist.go.jp; Yamamoto, Yuko S., E-mail: yamayulab@gmail.com; Department of Chemistry, School of Science and Technology, Kagawa University, Takamatsu, Kagawa 761-0396

2016-01-11

We report an evaluation method employing darkfield microspectroscopy for silver probes used in tip-enhanced Raman scattering (TERS). By adjusting the darkfield illumination, the diffracted light from the probe outlines disappears and the diffracted light from the surface nanostructures and tips of the probes appears as colorful spots. Scanning electron microscopy reveals that the spectral variations in these spots reflect the shapes of the surface nanostructures. The tip curvatures correlate to the spectral maxima of their spots. Temporal color changes in the spots indicate the deterioration due to the oxidation of the silver surfaces. These results show that the proposed methodmore » is useful for in situ evaluation of plasmonic properties of TERS probes.« less

Overcoming Short-Circuit in Lead-Free CH 3 NH 3 SnI 3 Perovskite Solar Cells via Kinetically Controlled Gas–Solid Reaction Film Fabrication Process

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

Yokoyama, Takamichi; Cao, Duyen H.; Stoumpos, Constantinos C.

2016-02-17

The development of Sn-based perovskite solar cells has been challenging because devices often show short-circuit behavior due to poor morphologies and undesired electrical properties of the thin films. A low-temperature vapor-assisted solution process (LT-VASP) has been employed as a novel kinetically controlled gas–solid reaction film fabrication method to prepare lead-free CH3NH3SnI3 thin films. We show that the solid SnI2 substrate temperature is the key parameter in achieving perovskite films with high surface coverage and excellent uniformity. The resulting high-quality CH3NH3SnI3 films allow the successful fabrication of solar cells with drastically improved reproducibility, reaching an efficiency of 1.86%. Furthermore, our Kelvinmore » probe studies show the VASP films have a doping level lower than that of films prepared from the conventional one-step method, effectively lowering the film conductivity. Above all, with (LT)-VASP, the short-circuit behavior often obtained from the conventional one-step-fabricated Sn-based perovskite devices has been overcome. This study facilitates the path to more successful Sn-perovskite photovoltaic research.« less

Nano-Architecture of nitrogen-doped graphene films synthesized from a solid CN source.

PubMed

Maddi, Chiranjeevi; Bourquard, Florent; Barnier, Vincent; Avila, José; Asensio, Maria-Carmen; Tite, Teddy; Donnet, Christophe; Garrelie, Florence

2018-02-19

New synthesis routes to tailor graphene properties by controlling the concentration and chemical configuration of dopants show great promise. Herein we report the direct reproducible synthesis of 2-3% nitrogen-doped 'few-layer' graphene from a solid state nitrogen carbide a-C:N source synthesized by femtosecond pulsed laser ablation. Analytical investigations, including synchrotron facilities, made it possible to identify the configuration and chemistry of the nitrogen-doped graphene films. Auger mapping successfully quantified the 2D distribution of the number of graphene layers over the surface, and hence offers a new original way to probe the architecture of graphene sheets. The films mainly consist in a Bernal ABA stacking three-layer architecture, with a layer number distribution ranging from 2 to 6. Nitrogen doping affects the charge carrier distribution but has no significant effects on the number of lattice defects or disorders, compared to undoped graphene synthetized in similar conditions. Pyridinic, quaternary and pyrrolic nitrogen are the dominant chemical configurations, pyridinic N being preponderant at the scale of the film architecture. This work opens highly promising perspectives for the development of self-organized nitrogen-doped graphene materials, as synthetized from solid carbon nitride, with various functionalities, and for the characterization of 2D materials using a significant new methodology.

The structure and binding mode of citrate in the stabilization of gold nanoparticles

NASA Astrophysics Data System (ADS)

Al-Johani, Hind; Abou-Hamad, Edy; Jedidi, Abdesslem; Widdifield, Cory M.; Viger-Gravel, Jasmine; Sangaru, Shiv Shankar; Gajan, David; Anjum, Dalaver H.; Ould-Chikh, Samy; Hedhili, Mohamed Nejib; Gurinov, Andrei; Kelly, Michael J.; El Eter, Mohamad; Cavallo, Luigi; Emsley, Lyndon; Basset, Jean-Marie

2017-09-01

Elucidating the binding mode of carboxylate-containing ligands to gold nanoparticles (AuNPs) is crucial to understand their stabilizing role. A detailed picture of the three-dimensional structure and coordination modes of citrate, acetate, succinate and glutarate to AuNPs is obtained by 13C and 23Na solid-state NMR in combination with computational modelling and electron microscopy. The binding between the carboxylates and the AuNP surface is found to occur in three different modes. These three modes are simultaneously present at low citrate to gold ratios, while a monocarboxylate monodentate (1κO1) mode is favoured at high citrate:gold ratios. The surface AuNP atoms are found to be predominantly in the zero oxidation state after citrate coordination, although trace amounts of Auδ+ are observed. 23Na NMR experiments show that Na+ ions are present near the gold surface, indicating that carboxylate binding occurs as a 2e- L-type interaction for each oxygen atom involved. This approach has broad potential to probe the binding of a variety of ligands to metal nanoparticles.

Synthesis and improved SERS performance of silver nanoparticles-decorated surface mesoporous silica microspheres

NASA Astrophysics Data System (ADS)

Jiang, Tao; Wang, Xiaolong; Zhang, Li; Zhou, Jun; Zhao, Ziqi

2016-08-01

This study reported the improved Raman enhancement ability of silver nanoparticles (Ag NPs) decorated on surface mesoporous silica microspheres (MSiO2@Ag) than that of Ag NPs on solid silica microspheres (SSiO2@Ag). These two kinds of hybrid structures were prepared by a facile single-step hydrothermal reaction with polyvinylpyrrolidone (PVP) serves as both a reductant and stabilizer. The as-synthesized MSiO2@Ag microspheres show more significant surface-enhanced Raman scattering (SERS) activity for 4-mercaptobenzoic acid (4MBA) than SSiO2@Ag microspheres with enhancement factors as 9.20 × 106 and 4.39 × 106, respectively. The proposed reason for the higher SERS activity is estimated to be the contribution of more Raman probe molecules at the mesoporous channels where an enhanced electromagnetic field exists. Such a field was identified by theoretical calculation result. The MSiO2@Ag microspheres were eventually demonstrated for the SERS detection of a typical chemical toxin namely methyl parathion with a detection limit as low as 1 × 10-3 ppm, showing its promising potential in biosensor application.

Crude Oil Remote Sensing, Characterization and Cleaning with CW and Pulsed Lasers

NASA Technical Reports Server (NTRS)

Kukhtareva, Tatiana; Chirita, Arc; Gallegos, Sonia C.

2014-01-01

For detection, identification and characterization of crude oil we combine several optical methods of remote sensing of crude oil films and emulsions (coherent fringe projection illumination (CFP), holographic in-line interferometry (HILI), and laser induced fluorescence). These methods allow the three-dimensional characterization of oil spills, important for practical applications. Combined methods of CFP and HILI are described in the frame of coherent superposition of partial interference patterns. It is shown, that in addition to detection/identification laser illumination in the green-blue region can also degrade oil slicks. Different types of surfaces contaminated by oil spills are tested: oil on the water, oil on the flat solid surfaces and oil on the curved surfaces of pipes. For the detection and monitoring of the laser-induced oil degradation in pipes, coherent fiber bundles were used. Both continuous-wave (CW) and pulsed lasers are tested using pump-probe schemes. This finding suggests that properly structured laser clean-up can be an alternative environmentally-friendly method of decontamination, as compared to the currently used chemical methods that are dangerous to environment.

Fabrication and surface enhanced Raman scattering effect of centimeter level AgCuAu composite nanowires

NASA Astrophysics Data System (ADS)

Xu, Dapeng; Zhang, Song; Yang, Wei; Chen, Jian

2017-10-01

Centimeter level AgCuAu composite nanowires were prepared by a solid-state ionics method under a direct current electric field (DCEF) using fast ionic conductor RbAg4I5 films and vacuum thermal evaporation method. The surface morphology and chemical composition of the AuAgCu composite nanowires were characterized by scanning electron microscopy (SEM) and energy dispersive spectrometer (EDS), respectively. Raman enhancement performance of the AgCuAu composite nanowires substrates was detected by Rhodamine 6G (R6G) aqueous solutions as probe molecules. Long-range order and short-range order AgCuAu composite nanowires with the length of 1 cm were prepared. The nanowires were bamboo-shaped with high surface roughness and the diameters of nanowires ranged from 60 to 100 nm. The molar ratio of Ag:Cu:Au in composite nanowires is 15:2:1. The intrinsic Raman peaks of 10-16 mol/L R6G at 612, 773, 1125, 1182, 1307, 1361, 1418, 1506, 1545, 1575, 1597, 1650 cm-1 are all present when AgCuAu composite nanowires were used as the SERS substrates.

The reactivity of Fe(II) associated with goethite formed during short redox cycles toward Cr(VI) reduction under oxic conditions

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

Tomaszewski, Elizabeth J.; Lee, Seungyeol; Rudolph, Jared

Chromium (Cr) is a toxic metal that causes a myriad of health problems and enters the environment as a result of anthropogenic activities and/or natural processes. The toxicity and solubility of chromium is linked to its oxidation state; Cr(III) is poorly soluble and relatively nontoxic, while Cr(VI) is soluble and a known carcinogen. Solid Fe(II) in iron-bearing minerals, such as pyrite, magnetite, and green rusts, reduce the oxidation state of chromium, reducing its toxicity and mobility. However, these minerals are not the only potential sources of solid-associated Fe(II) available for Cr(VI) reduction. For example, ferric (Fe(III)) (hydr)oxides, such as goethitemore » or hematite, can have Fe(II) in the solid without phase transformation; however, the reactivity of Fe(II) within Fe(III) (hydr)oxides with contaminants, has not been previously investigated. Here, we cyclically react goethite with dissolved Fe(II) followed by dissolved O2, leading to the formation of reactive Fe(II) associated with goethite. In separate reactors, the reactivity of this Fe(II) is probed under oxic conditions, by exposure to chromate (CrO42 -) after either one, two, three or four redox cycles. Cr is not present during redox cycling; rather, it is introduced to a subset of the solid after each oxidation half-cycle. Analysis of X-ray absorption near edge structure (XANES) spectra reveals that the extent of Cr(VI) reduction to Cr(III) depends not only on solid Fe(II) content but also surface area and mean size of ordered crystalline domains, determined by BET surface area analysis and X-ray diffraction (XRD), respectively. Shell-by-shell fitting of the extended X-ray absorption fine structure (EXAFS) spectra demonstrates chromium forms both single and double corner sharing complexes on the surface of goethite, in addition to sorbed Cr(III) species. Finally, transmission electron microscope (TEM) imaging and X-ray energy-dispersive spectroscopy (EDS) illustrate that Cr preferentially localizes on the (100) face of goethite, independent of the number of redox cycles goethite undergoes. This work demonstrates that under oxic conditions, solid Fe(II) associated with goethite resulting from rapid redox cycling is reactive and available for electron transfer to Cr(VI), suggesting Fe(III) (hydr)oxides may act as reservoirs of reactive electron density, even in oxygen saturated environments.« less

Directional self-cleaning superoleophobic surface.

PubMed

Zhao, Hong; Law, Kock-Yee

2012-08-14

In this work, we report the creation of a grooved surface comprising 3 μm grooves (height ~4 μm) separated by 3 μm from each other on a silicon wafer by photolithography. The grooved surface was then modified chemically with a fluorosilane layer (FOTS). The surface property was studied by both static and dynamic contact angle measurements using water, hexadecane, and a polyethylene wax ink as the probing liquids. Results show that the grooved surface is both superhydrophobic and superoleophobic. Its observed contact angles agree well with the calculated Cassie-Baxter angles. More importantly, we are able to make a replica of the composite wax ink-air interface and study it by SEM. Microscopy results not only show that the droplet of the wax ink "sits" on air in the composite interface but also further reveal that the ink drop actually pins underneath the re-entrant structure in the side wall of the grooved structure. Contact angle measurement results indicate that wetting on the grooved surface is anisotropic. Although liquid drops are found to have lower static and advancing contact angles in the parallel direction, the drops are found to be more mobile, showing smaller hysteresis and lower sliding angles (as compared to the FOTS wafer surface and a comparable 3-μm-diameter pillar array FOTS surface). The enhanced mobility is attributable to the lowering of the resistance against an advancing liquid because 50% of the advancing area is made of a solid strip where the liquid likes to wet. This also implies that the contact line for advancing is no longer smooth but rather is ragged, having the solid strip area leading the wetting and the air strip area trailing behind. This interpretation is supported by imaging the geometry of the contact lines using molten ink drops recovered from the sliding angle experiments in both the parallel and orthogonal directions. Because the grooved surface is mechanically stronger against mechanical abrasion, the self-cleaning effect exhibited in the parallel direction suggests that groove texturing is a viable approach to create mechanically robust, self-cleaning, superoleophobic surfaces.

Robotic end effector

DOEpatents

Minichan, Richard L.

1993-01-01

An end effector for use in probing a surface with a robotic arm. The end effector has a first portion that carries a gimbal with a probe, the gimbal holding the probe normal to the surface, and a second portion with a set of three shafts within a housing for urging the gimbal and probe against the surface. The second portion contains a potentiometer connected by another shaft to the first portion to measure the position of the first portion with respect to the second so that the second portion can be moved to place and maintain the shafts at the midpoint of their travel. Then, as irregularities in the surface are encountered, the first portion can respond by moving closer to or farther from the second portion.

Robotic end effector

DOEpatents

Minichan, R.L.

1993-10-05

An end effector is described for use in probing a surface with a robotic arm. The end effector has a first portion that carries a gimbal with a probe, the gimbal holding the probe normal to the surface, and a second portion with a set of three shafts within a housing for urging the gimbal and probe against the surface. The second portion contains a potentiometer connected by another shaft to the first portion to measure the position of the first portion with respect to the second so that the second portion can be moved to place and maintain the shafts at the midpoint of their travel. Then, as irregularities in the surface are encountered, the first portion can respond by moving closer to or farther from the second portion. 7 figures.

Calcium-43 chemical shift tensors as probes of calcium binding environments. Insight into the structure of the vaterite CaCO3 polymorph by 43Ca solid-state NMR spectroscopy.

PubMed

Bryce, David L; Bultz, Elijah B; Aebi, Dominic

2008-07-23

Natural-abundance (43)Ca solid-state NMR spectroscopy at 21.1 T and gauge-including projector-augmented-wave (GIPAW) DFT calculations are developed as tools to provide insight into calcium binding environments, with special emphasis on the calcium chemical shift (CS) tensor. The first complete analysis of a (43)Ca solid-state NMR spectrum, including the relative orientation of the CS and electric field gradient (EFG) tensors, is reported for calcite. GIPAW calculations of the (43)Ca CS and EFG tensors for a series of small molecules are shown to reproduce experimental trends; for example, the trend in available solid-state chemical shifts is reproduced with a correlation coefficient of 0.983. The results strongly suggest the utility of the calcium CS tensor as a novel probe of calcium binding environments in a range of calcium-containing materials. For example, for three polymorphs of CaCO3 the CS tensor span ranges from 8 to 70 ppm and the symmetry around calcium is manifested differently in the CS tensor as compared with the EFG tensor. The advantages of characterizing the CS tensor are particularly evident in very high magnetic fields where the effect of calcium CS anisotropy is augmented in hertz while the effect of second-order quadrupolar broadening is often obscured for (43)Ca because of its small quadrupole moment. Finally, as an application of the combined experimental-theoretical approach, the solid-state structure of the vaterite polymorph of calcium carbonate is probed and we conclude that the hexagonal P6(3)/mmc space group provides a better representation of the structure than does the orthorhombic Pbnm space group, thereby demonstrating the utility of (43)Ca solid-state NMR as a complementary tool to X-ray crystallographic methods.

Recent advances in the mechanical durability of superhydrophobic materials.

PubMed

Milionis, Athanasios; Loth, Eric; Bayer, Ilker S

2016-03-01

Large majority of superhydrophobic surfaces have very limited mechanical wear robustness and long-term durability. This problem has restricted their utilization in commercial or industrial applications and resulted in extensive research efforts on improving resistance against various types of wear damage. In this review, advances and developments since 2011 in this field will be covered. As such, we summarize progress on fabrication, design and understanding of mechanically durable superhydrophobic surfaces. This includes an overview of recently published diagnostic techniques for probing and demonstrating tribo-mechanical durability against wear and abrasion as well as other effects such as solid/liquid spray or jet impact and underwater resistance. The review is organized in terms of various types of mechanical wear ranging from substrate adhesion, tangential surface abrasion, and dynamic impact to ultrasonic processing underwater. In each of these categories, we highlight the most successful approaches to produce robust surfaces that can maintain their non-wetting state after the wear or abrasive action. Finally, various recommendations for improvement of mechanical wear durability and its quantitative evaluation are discussed along with potential future directions towards more systematic testing methods which will also be acceptable for industry. Copyright © 2015 Elsevier B.V. All rights reserved.

Examining Model Atmospheric Particles Inside and Out

NASA Astrophysics Data System (ADS)

Wingen, L. M.; Zhao, Y.; Fairhurst, M. C.; Perraud, V. M.; Ezell, M. J.; Finlayson-Pitts, B. J.

2017-12-01

Atmospheric particles scatter incoming solar radiation and act as cloud condensation nuclei (CCN), thereby directly and indirectly affecting the earth's radiative balance and reducing visibility. These atmospheric particles may not be uniform in composition. Differences in the composition of a particle's outer surface from its core can arise during particle growth, (photo)chemical aging, and exchange of species with the gas phase. The nature of the surface on a molecular level is expected to impact growth mechanisms as well as their ability to act as CCN. Model laboratory particle systems are explored using direct analysis in real time-mass spectrometry (DART-MS), which is sensitive to surface composition, and contrasted with average composition measurements using high resolution, time-of-flight aerosol mass spectrometry (HR-ToF-AMS). Results include studies of the heterogeneous reactions of amines with solid dicarboxylic acid particles, which are shown to generate aminium dicarboxylate salts at the particle surface, leaving an unreacted core. Combination of both mass spectrometric techniques reveals a trend in reactivity of C3-C7 dicarboxylic acids with amines and allows calculation of the DART probe depth into the particles. The results of studies on additional model systems that are currently being explored will also be reported.

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

NASA Astrophysics Data System (ADS)

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

2005-03-01

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

Nanoscale On-Silico Electron Transport via Ferritins.

PubMed

Bera, Sudipta; Kolay, Jayeeta; Banerjee, Siddhartha; Mukhopadhyay, Rupa

2017-02-28

Silicon is a solid-state semiconducting material that has long been recognized as a technologically useful one, especially in electronics industry. However, its application in the next-generation metalloprotein-based electronics approaches has been limited. In this work, the applicability of silicon as a solid support for anchoring the iron-storage protein ferritin, which has a semiconducting iron nanocore, and probing electron transport via the ferritin molecules trapped between silicon substrate and a conductive scanning probe has been investigated. Ferritin protein is an attractive bioelectronic material because its size (X-ray crystallographic diameter ∼12 nm) should allow it to fit well in the larger tunnel gaps (>5 nm), fabrication of which is relatively more established, than the smaller ones. The electron transport events occurring through the ferritin molecules that are covalently anchored onto the MPTMS-modified silicon surface could be detected at the molecular level by current-sensing atomic force spectroscopy (CSAFS). Importantly, the distinct electronic signatures of the metal types (i.e., Fe, Mn, Ni, and Au) within the ferritin nanocore could be distinguished from each other using the transport band gap analyses. The CSAFS measurements on holoferritin, apoferritin, and the metal core reconstituted ferritins reveal that some of these ferritins behave like n-type semiconductors, while the others behave as p-type semiconductors. The band gaps for the different ferritins are found to be within 0.8 to 2.6 eV, a range that is valid for the standard semiconductor technology (e.g., diodes based on p-n junction). The present work indicates effective on-silico integration of the ferritin protein, as it remains functionally viable after silicon binding and its electron transport activities can be detected. Potential use of the ferritin-silicon nanohybrids may therefore be envisaged in applications other than bioelectronics, too, as ferritin is a versatile nanocore-containing biomaterial (for storage/transport of metals and drugs) and silicon can be a versatile nanoscale solid support (for its biocompatible nature).

In vitro performance of DIAGNOdent laser fluorescence device for dental calculus detection on human tooth root surfaces.

PubMed

Rams, Thomas E; Alwaqyan, Abdulaziz Y

2017-10-01

This study assessed the reproducibility of a red diode laser device, and its capability to detect dental calculus in vitro on human tooth root surfaces. On each of 50 extracted teeth, a calculus-positive and calculus-free root surface was evaluated by two independent examiners with a low-power indium gallium arsenide phosphide diode laser (DIAGNOdent) fitted with a periodontal probe-like sapphire tip and emitting visible red light at 655 nm wavelength. Laser autofluorescence intensity readings of examined root surfaces were scored on a 0-99 scale, with duplicate assessments performed using the laser probe tip directed both perpendicular and parallel to evaluated tooth root surfaces. Pearson correlation coefficients of untransformed measurements, and kappa analysis of data dichotomized with a >40 autofluorescence intensity threshold, were calculated to assess intra- and inter-examiner reproducibility of the laser device. Mean autofluorescence intensity scores of calculus-positive and calculus-free root surfaces were evaluated with the Student's t -test. Excellent intra- and inter-examiner reproducibility was found for DIAGNOdent laser autofluorescence intensity measurements, with Pearson correlation coefficients above 94%, and kappa values ranging between 0.96 and 1.0, for duplicate readings taken with both laser probe tip orientations. Significantly higher autofluorescence intensity values were measured when the laser probe tip was directed perpendicular, rather than parallel, to tooth root surfaces. However, calculus-positive roots, particularly with calculus in markedly-raised ledges, yielded significantly greater mean DIAGNOdent laser autofluorescence intensity scores than calculus-free surfaces, regardless of probe tip orientation. DIAGNOdent autofluorescence intensity values >40 exhibited a stronger association with calculus (36.6 odds ratio) then measurements of ≥5 (20.1 odds ratio) when the laser probe tip was advanced parallel to root surfaces. Excellent intra- and inter-examiner reproducibility of autofluorescence intensity measurements was obtained with the DIAGNOdent laser fluorescence device on human tooth roots. Calculus-positive root surfaces exhibited significantly greater DIAGNOdent laser autofluorescence than calculus-free tooth roots, even with the laser probe tip directed parallel to root surfaces. These findings provide further in vitro validation of the potential utility of a DIAGNOdent laser fluorescence device for identifying dental calculus on human tooth root surfaces.

Transfer of Materials from Water to Solid Surfaces Using Liquid Marbles.

PubMed

Kawashima, Hisato; Paven, Maxime; Mayama, Hiroyuki; Butt, Hans-Jürgen; Nakamura, Yoshinobu; Fujii, Syuji

2017-09-27

Remotely controlling the movement of small objects is desirable, especially for the transportation and selection of materials. Transfer of objects between liquid and solid surfaces and triggering their release would allow for development of novel material transportation technology. Here, we describe the remote transport of a material from a water film surface to a solid surface using quasispherical liquid marbles (LMs). A light-induced Marangoni flow or an air stream is used to propel the LMs on water. As the LMs approach the rim of the water film, gravity forces them to slide down the water rim and roll onto the solid surface. Through this method, LMs can be efficiently moved on water and placed on a solid surface. The materials encapsulated within LMs can be released at a specific time by an external stimulus. We analyzed the velocity, acceleration, and force of the LMs on the liquid and solid surfaces. On water, the sliding friction due to the drag force resists the movement of the LMs. On a solid surface, the rolling distance is affected by the surface roughness of the LMs.

Two-probe STM experiments at the atomic level.

PubMed

Kolmer, Marek; Olszowski, Piotr; Zuzak, Rafal; Godlewski, Szymon; Joachim, Christian; Szymonski, Marek

2017-11-08

Direct characterization of planar atomic or molecular scale devices and circuits on a supporting surface by multi-probe measurements requires unprecedented stability of single atom contacts and manipulation of scanning probes over large, nanometer scale area with atomic precision. In this work, we describe the full methodology behind atomically defined two-probe scanning tunneling microscopy (STM) experiments performed on a model system: dangling bond dimer wire supported on a hydrogenated germanium (0 0 1) surface. We show that 70 nm long atomic wire can be simultaneously approached by two independent STM scanners with exact probe to probe distance reaching down to 30 nm. This allows direct wire characterization by two-probe I-V characteristics at distances below 50 nm. Our technical results presented in this work open a new area for multi-probe research, which can be now performed with precision so far accessible only by single-probe scanning probe microscopy (SPM) experiments.

Some studies on a solid-state sulfur probe for coal gasification systems

NASA Technical Reports Server (NTRS)

Jacob, K. T.; Rao, D. B.; Nelson, H. G.

1978-01-01

As a part of a program for the development of a sulfur probe for monitoring the sulfur potential in coal gasification reactors, an investigation was conducted regarding the efficiency of the solid electrolyte cell Ar+H2+H2S/CaS+CaF2+(Pt)//CaF2//Pt)+CaF2+CaS/H2S+H2+Ar. A demonstration is provided of the theory, design, and operation of a solid-state sulfur probe based on CaF2 electrolyte. It was found that the cell responds to changes in sulfur potential in a manner predicted by the Nernst equation. The response time of the cell at 1225 K, after a small change in temperature or gas composition, was 2.5 Hr, while at a lower temperature of 990 K the response time was approximately 9 hr. The cell emf was insensitive to a moderate increase in the flow rate of the test gas and/or the reference gas. The exact factors affecting the slow response time of galvanic cells based on a CaF2 electrolyte have not yet been determined. The rate-limiting steps may be either the kinetics of electrode reactions or the rate of transport through the electrolyte.

Introducing cymantrene labels into scattering scanning near-field infrared microscopy.

PubMed

Kopf, Ilona; N'Dongo, Harmel W Peindy; Ballout, Fouad; Schatzschneider, Ulrich; Bründermann, Erik; Havenith, Martina

2012-11-07

In this paper we investigate metal-organic compounds as infrared (IR) active labels by scattering scanning near-field infrared microscopy (IR s-SNOM, often also abbreviated as s-SNIM) with a lateral resolution of 90 × 90 nm(2). Tailor-made IR spectroscopic probes based on cymantrene (CpMn(CO)(3) with Cp = η(5)-C(5)H(5)) conjugated to a cysteine-modified pseudoneurotensin (pNT-Cys-OH) peptide were prepared by automated microwave-assisted solid phase peptide synthesis (SPPS) and characterized by HPLC, ESI-MS and IR. Well-defined patterned self-assembled monolayers on a gold surface were prepared by microcontact printing of 1-octadecanethiol (ODT) followed by additional incubation in ethanolic solution of the cymantrene-peptide derivative. The self-assembled monolayers have been evidenced by infrared reflection absorption spectroscopy (IRRAS) and AFM. CO laser source radiation was tuned (1944, 1900, 1798 and 1658 cm(-1)) for imaging contrast with good matching correlation between spectroscopic and topographic patterns at specific characteristic metal carbonyl and amide bands (1944 cm(-1) (λ = 5.14 μm) and 1658 cm(-1) (λ = 6.03 μm)). Cymantrene probes provide an attractive method to tag a unique spectroscopic feature on any bio(macro)molecule. Introducing such probes into super-resolution IR s-SNOM will enable molecular tracking and distribution studies even in complex biological systems.

PIR-fiber spectroscopy with FTIR and TDL spectrometers in the middle infared range of spectra

NASA Astrophysics Data System (ADS)

Artjushenko, Vjacheslav G.; Afanasyeva, Natalia I.; Bruch, Reinhard F.; Daniellian, G.; Stepanov, Eugene V.

2000-07-01

Development of Polycrystalline Infrared (PIR-) fibers extruded from solid solutions of AgCl/AgBr has opened a new horizon of molecular spectroscopy applications in 4 - 18 micron range of spectra. PIR-fiber cables and probes could be coupled with a variety of Fourier Transform Infrared spectrometer and Tunable Diode Lasers (TDL), including pig tailing of Mercury Cadmium Tellurium (MCT) detectors. Using these techniques no sample preparation is necessary for PIR- fiber probes to measure reflection and absorption spectra, in situ, in vivo, in real time and even multiplexed. Such PIR-fiber probes have been used for evanescent absorption spectroscopy of malignant tissue and skin surface diagnostics in-vivo, glucose detection in blood as well as crude oil composition analysis, for organic pollution and nuclear waste monitoring. A review of various PIR-fiber applications in medicine, industry and environment control is presented. The synergy of PIR-fibers flexibility with a super high resolution of TDL spectrometers with (Delta) v equals 10-4 cm-1, provides the unique tool for gas analysis, specifically when PIR-fibers are coupled as pigtails with MCT-detectors, and Pb-salt lasers. Design of multichannel PIR-fiber tailed TDL spectrometer could be used as a portable device for multispectral gas analysis at 1 ppb level of detectivity for various applications in medicine and biotechnology.

Profiling the decomposition odour at the grave surface before and after probing.

PubMed

Forbes, S L; Troobnikoff, A N; Ueland, M; Nizio, K D; Perrault, K A

2016-02-01

Human remains detection (HRD) dogs are recognised as a valuable and non-invasive search method for remains concealed in many different environments, including clandestine graves. However, the search for buried remains can be a challenging task as minimal odour may be available at the grave surface for detection by the dogs. Handlers often use a soil probe during these searches in an attempt to increase the amount of odour available for detection, but soil probing is considered an invasive search technique. The aim of this study was to determine whether the soil probe assists with increasing the abundance of volatile organic compounds (VOCs) available at the grave surface. A proof-of-concept method was developed using porcine remains to collect VOCs within the grave without disturbing the burial environment, and to compare their abundance at the grave surface before and after probing. Detection and identification of the VOC profiles required the use of comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC×GC-TOFMS) due to its superior sensitivity and selectivity for decomposition odour profiling. The abundance of decomposition VOCs was consistently higher within the grave environment compared to the grave surface, except when the grave surface had been disturbed, confirming the reduced availability of odour at the grave surface. Although probing appeared to increase the abundance of VOCs at the grave surface on many of the sampling days, there were no clear trends identified across the study and no direct relationships with the environmental variables measured. Typically, the decomposition VOCs that were most prevalent in the grave soil were the same VOCs detected at the grave surface, whereas the trace VOCs detected in these environments varied throughout the post-burial period. This study highlighted that probing the soil can assist with releasing decomposition VOCs but is likely correlated to environmental and burial variables which require further study. The use of a soil probe to assist HRD dogs should not be disregarded but should only follow the use of non-invasive methods if deemed appropriate. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

The effects of solid rocket motor effluents on selected surfaces and solid particle size, distribution, and composition for simulated shuttle booster separation motors

NASA Technical Reports Server (NTRS)

Jex, D. W.; Linton, R. C.; Russell, W. M.; Trenkle, J. J.; Wilkes, D. R.

1976-01-01

A series of three tests was conducted using solid rocket propellants to determine the effects a solid rocket plume would have on thermal protective surfaces (TPS). The surfaces tested were those which are baselined for the shuttle vehicle. The propellants used were to simulate the separation solid rocket motors (SSRM) that separate the solid rocket boosters (SRB) from the shuttle launch vehicle. Data cover: (1) the optical effects of the plume environment on spacecraft related surfaces, and (2) the solid particle size, distribution, and composition at TPS sample locations.

Atmospheric Probe Model: Construction and Wind Tunnel Tests

NASA Technical Reports Server (NTRS)

Vogel, Jerald M.

1998-01-01

The material contained in this document represents a summary of the results of a low speed wind tunnel test program to determine the performance of an atmospheric probe at low speed. The probe configuration tested consists of a 2/3 scale model constructed from a combination of hard maple wood and aluminum stock. The model design includes approximately 130 surface static pressure taps. Additional hardware incorporated in the baseline model provides a mechanism for simulating external and internal trailing edge split flaps for probe flow control. Test matrix parameters include probe side slip angle, external/internal split flap deflection angle, and trip strip applications. Test output database includes surface pressure distributions on both inner and outer annular wings and probe center line velocity distributions from forward probe to aft probe locations.

DESIGN NOTE: The measurement of thermal conductivities of solid fruits and vegetables

NASA Astrophysics Data System (ADS)

Liang, Xin-Gang; Zhang, Yinping; Ge, Xinshi

1999-07-01

A thermal conductivity probe consisting of a heating cell, a thermocouple and a guard tube over the heating cell was developed and is described here. Analyses demonstrate that the guard tube acts as a thermal contact resistance. This resistance does not influence measurements of thermal conductivity significantly, but it must be considered in an accurate measurement of thermal diffusivity, especially when there is a gap between the heater and the guard tube. Calibration of the probe with glycerine in this work exhibits an accuracy of 1.4% for thermal conductivity measurements. The probe was used to measure the thermal conductivities of some solid fruits and vegetables. The sizes of both specimen and probe were analysed and their influences controlled to be under 1.0%. Each measurement was completed within two minutes and the temperature rise was less than under 6 °C. The water content of fruits and vegetables was found to be the dominant factor in determining their thermal conductivities. An empirical relationship between thermal conductivity and mass density is proposed based on the measurements. It is shown that this relation gives a deviation from experimental data of only 11%.

Reactive solid surface morphology variation via ionic diffusion.

PubMed

Sun, Zhenchao; Zhou, Qiang; Fan, Liang-Shih

2012-08-14

In gas-solid reactions, one of the most important factors that determine the overall reaction rate is the solid morphology, which can be characterized by a combination of smooth, convex and concave structures. Generally, the solid surface structure varies in the course of reactions, which is classically noted as being attributed to one or more of the following three mechanisms: mechanical interaction, molar volume change, and sintering. Here we show that if a gas-solid reaction involves the outward ionic diffusion of a solid-phase reactant then this outward ionic diffusion could eventually smooth the surface with an initial concave and/or convex structure. Specifically, the concave surface is filled via a larger outward diffusing surface pointing to the concave valley, whereas the height of the convex surface decreases via a lower outward diffusion flux in the vertical direction. A quantitative 2-D continuum diffusion model is established to analyze these two morphological variation processes, which shows consistent results with the experiments. This surface morphology variation by solid-phase ionic diffusion serves to provide a fourth mechanism that supplements the traditionally acknowledged solid morphology variation or, in general, porosity variation mechanisms in gas-solid reactions.

Improvement of arthroscopic cartilage stiffness probe using amorphous diamond coating.

PubMed

Töyräs, Juha; Korhonen, Rami K; Voutilainen, Tanja; Jurvelin, Jukka S; Lappalainen, Reijo

2005-04-01

During arthroscopic evaluation of articular cartilage unstable contact and even slipping of the measurement instrument on the tissue surface may degrade the reproducibility of the measurement. The main aim of the present study was to achieve more stable contact by controlling the friction between articular cartilage surface and the arthroscopic cartilage stiffness probe (Artscan 200, Artscan Oy, Helsinki, Finland) using amorphous diamond (AD) coating. In order to obtain surfaces with different average roughnesses (R(a)), polished stainless steel disks were coated with AD by using the filtered pulsed arc-discharge (FPAD) method. Dynamic coefficient of friction (mu) between the articular cartilage (n = 8) and the coated plates along one non-coated plate was then determined. The friction between AD and cartilage could be controlled over a wide range (mu = 0.027-0.728, p < 0.05, Wilcoxon test) by altering the roughness. Possible deterioration of cartilage was investigated by measuring surface roughness after friction tests and comparing it with the roughness of the adjacent, untested samples (n = 8). Importantly, even testing with the roughest AD (R(a) = 1250 nm) did not damage articular surface. On the basis of the friction measurements, a proper AD coating was selected for the stiffness probe. The performance of coated and non-coated probe was compared by measuring bovine osteochondral samples (n = 22) with both instruments. The reproducibility of the stiffness measurements was significantly better with the AD-coated probe (CV% = 4.7) than with the uncoated probe (CV% = 8.2). To conclude, AD coating can be used to safely control dynamic friction with articular surface. Sufficient friction between articular surface and reference plate of the arthroscopic probe improves significantly reproducibility of the stiffness measurements. (c) 2005 Wiley Periodicals, Inc.

Preassembled Fluorescent Multivalent Probes for the Imaging of Anionic Membranes.

PubMed

Roland, Felicia M; Peck, Evan M; Rice, Douglas R; Smith, Bradley D

2017-04-19

A new self-assembly process known as Synthavidin (synthetic avidin) technology was used to prepare targeted probes for near-infrared fluorescence imaging of anionic membranes and cell surfaces, a hallmark of many different types of disease. The probes were preassembled by threading a tetralactam macrocycle with six appended zinc-dipicolylamine (ZnDPA) targeting units onto a linear scaffold with one or two squaraine docking stations to produce hexavalent or dodecavalent fluorescent probes. A series of liposome titration experiments showed that multivalency promoted stronger membrane binding by the dodecavalent probe. In addition, the dodecavalent probe exhibited turn-on fluorescence due to probe unfolding during fluorescence microscopy at the membrane surface. However, the dodecavalent probe also had a higher tendency to self-aggregate after membrane binding, leading to probe self-quenching under certain conditions. This self-quenching effect was apparent during fluorescence microscopy experiments that recorded low fluorescence intensity from anionic dead and dying mammalian cells that were saturated with the dodecavalent probe. Conversely, probe self-quenching was not a factor with anionic microbial surfaces, where there was intense fluorescence staining by the dodecavalent probe. A successful set of rat tumor imaging experiments confirmed that the preassembled probes have sufficient mechanical stability for effective in vivo imaging. The results demonstrate the feasibility of this general class of preassembled fluorescent probes for multivalent targeting, but fluorescence imaging performance depends on the specific physical attributes of the biomarker target, such as the spatial distance between different copies of the biomarker and the propensity of the probe-biomarker complex to self-aggregate.

In Situ Characterization of the Initial Effect of Water on Molecular Interactions at the Interface of Organic/Inorganic Hybrid Systems

PubMed Central

Pletincx, Sven; Trotochaud, Lena; Fockaert, Laura-Lynn; Mol, Johannes M. C.; Head, Ashley R.; Karslıoğlu, Osman; Bluhm, Hendrik; Terryn, Herman; Hauffman, Tom

2017-01-01

Probing initial interactions at the interface of hybrid systems under humid conditions has the potential to reveal the local chemical environment at solid/solid interfaces under real-world, technologically relevant conditions. Here, we show that ambient pressure X-ray photoelectron spectroscopy (APXPS) with a conventional X-ray source can be used to study the effects of water exposure on the interaction of a nanometer-thin polyacrylic acid (PAA) layer with a native aluminum oxide surface. The formation of a carboxylate ionic bond at the interface is characterized both with APXPS and in situ attenuated total reflectance Fourier transform infrared spectroscopy in the Kretschmann geometry (ATR-FTIR Kretschmann). When water is dosed in the APXPS chamber up to 5 Torr (~28% relative humidity), an increase in the amount of ionic bonds at the interface is observed. To confirm our APXPS interpretation, complementary ATR-FTIR Kretschmann experiments on a similar model system, which is exposed to an aqueous electrolyte, are conducted. These spectra demonstrate that water leads to an increased wet adhesion through increased ionic bond formation. PMID:28327587

Probing the interatomic potential of solids with strong-field nonlinear phononics

NASA Astrophysics Data System (ADS)

von Hoegen, A.; Mankowsky, R.; Fechner, M.; Först, M.; Cavalleri, A.

2018-03-01

Nonlinear optical techniques at visible frequencies have long been applied to condensed matter spectroscopy. However, because many important excitations of solids are found at low energies, much can be gained from the extension of nonlinear optics to mid-infrared and terahertz frequencies. For example, the nonlinear excitation of lattice vibrations has enabled the dynamic control of material functions. So far it has only been possible to exploit second-order phonon nonlinearities at terahertz field strengths near one million volts per centimetre. Here we achieve an order-of-magnitude increase in field strength and explore higher-order phonon nonlinearities. We excite up to five harmonics of the A1 (transverse optical) phonon mode in the ferroelectric material lithium niobate. By using ultrashort mid-infrared laser pulses to drive the atoms far from their equilibrium positions, and measuring the large-amplitude atomic trajectories, we can sample the interatomic potential of lithium niobate, providing a benchmark for ab initio calculations for the material. Tomography of the energy surface by high-order nonlinear phononics could benefit many aspects of materials research, including the study of classical and quantum phase transitions.

Weak interactions between water and clathrate-forming gases at low pressures

DOE PAGES

Thürmer, Konrad; Yuan, Chunqing; Kimmel, Greg A.; ...

2015-07-17

Using scanning probe microscopy and temperature programed desorption we examined the interaction between water and two common clathrate-forming gases, methane and isobutane, at low temperature and low pressure. Water co-deposited with up to 10 –1 mbar methane or 10 –5 mbar isobutane at 140 K onto a Pt(111) substrate yielded pure crystalline ice, i.e., the exposure to up to ~ 10 7 gas molecules for each deposited water molecule did not have any detectable effect on the growing films. Exposing metastable, less than 2 molecular layers thick, water films to 10 –5 mbar methane does not alter their morphology, suggestingmore » that the presence of the Pt(111) surface is not a strong driver for hydrate formation. This weak water–gas interaction at low pressures is supported by our thermal desorption measurements from amorphous solid water and crystalline ice where 1 ML of methane desorbs near ~ 43 K and isobutane desorbs near ~ 100 K. As a result, similar desorption temperatures were observed for desorption from amorphous solid water.« less

Titan probe technology assessment and technology development plan study

NASA Technical Reports Server (NTRS)

Castro, A. J.

1980-01-01

The need for technology advances to accomplish the Titan probe mission was determined by defining mission conditions and requirements and evaluating the technology impact on the baseline probe configuration. Mission characteristics found to be technology drivers include (1) ten years dormant life in space vacuum; (2) unknown surface conditions, various sample materials, and a surface temperature; and (3) mission constraints of the Saturn Orbiter Dual Probe mission regarding weight allocation. The following areas were identified for further development: surface sample acquisition system; battery powered system; nonmetallic materials; magnetic bubble memory devices, and the landing system. Preentry science, reliability, and weight reduction and redundancy must also be considered.

Development progress of the Materials Analysis and Particle Probe

NASA Astrophysics Data System (ADS)

Lucia, M.; Kaita, R.; Majeski, R.; Bedoya, F.; Allain, J. P.; Boyle, D. P.; Schmitt, J. C.; Onge, D. A. St.

2014-11-01

The Materials Analysis and Particle Probe (MAPP) is a compact in vacuo surface science diagnostic, designed to provide in situ surface characterization of plasma facing components in a tokamak environment. MAPP has been implemented for operation on the Lithium Tokamak Experiment at Princeton Plasma Physics Laboratory (PPPL), where all control and analysis systems are currently under development for full remote operation. Control systems include vacuum management, instrument power, and translational/rotational probe drive. Analysis systems include onboard Langmuir probes and all components required for x-ray photoelectron spectroscopy, low-energy ion scattering spectroscopy, direct recoil spectroscopy, and thermal desorption spectroscopy surface analysis techniques.

Development progress of the Materials Analysis and Particle Probe.

PubMed

Lucia, M; Kaita, R; Majeski, R; Bedoya, F; Allain, J P; Boyle, D P; Schmitt, J C; Onge, D A St

2014-11-01

The Materials Analysis and Particle Probe (MAPP) is a compact in vacuo surface science diagnostic, designed to provide in situ surface characterization of plasma facing components in a tokamak environment. MAPP has been implemented for operation on the Lithium Tokamak Experiment at Princeton Plasma Physics Laboratory (PPPL), where all control and analysis systems are currently under development for full remote operation. Control systems include vacuum management, instrument power, and translational/rotational probe drive. Analysis systems include onboard Langmuir probes and all components required for x-ray photoelectron spectroscopy, low-energy ion scattering spectroscopy, direct recoil spectroscopy, and thermal desorption spectroscopy surface analysis techniques.

Ground Simulations of Near-Surface Plasma Field and Charging at the Lunar Terminator

NASA Astrophysics Data System (ADS)

Polansky, J.; Ding, N.; Wang, J.; Craven, P.; Schneider, T.; Vaughn, J.

2012-12-01

Charging in the lunar terminator region is the most complex and is still not well understood. In this region, the surface potential is sensitively influenced by both solar illumination and plasma flow. The combined effects from localized shadow generated by low sun elevation angles and localized wake generated by plasma flow over the rugged terrain can generate strongly differentially charged surfaces. Few models currently exist that can accurately resolve the combined effects of plasma flow and solar illumination over realistic lunar terminator topographies. This paper presents an experimental investigation of lunar surface charging at the terminator region in simulated plasma environments in a vacuum chamber. The solar wind plasma flow is simulated using an electron bombardment gridded Argon ion source. An electrostatic Langmuir probe, nude Faraday probes, a floating emissive probe, and retarding potential analyzer are used to quantify the plasma flow field. Surface potentials of both conducting and dielectric materials immersed in the plasma flow are measured with a Trek surface potential probe. The conducting material surface potential will simultaneously be measured with a high impedance voltmeter to calibrate the Trek probe. Measurement results will be presented for flat surfaces and objects-on-surface for various angles of attack of the plasma flow. The implications on the generation of localized plasma wake and surface charging at the lunar terminator will be discussed. (This research is supported by the NASA Lunar Advanced Science and Exploration Research program.)

Current Developments in Future Planetary Probe Sensors for TPS

NASA Technical Reports Server (NTRS)

Martinez, Ed; Venkatapathy, Ethiraj; Oishu, Tomo

2003-01-01

In-situ Thermal Protection System (TPS) sensors are required to provide traceability of TPS performance and sizing tools. Traceability will lead to higher fidelity design tools, which in turn will lead to lower design safety margins, and decreased heatshield mass. Decreasing TPS mass will enable certain missions that are not otherwise feasible, and directly increase science payload. NASA Ames is currently developing two flight measurements as essential to advancing the state of TPS traceability for material modeling and aerothermal simulation: heat flux and surface recession (for ablators). The heat flux gage is applicable to both ablators and non-ablators and is therefore the more generalized sensor concept of the two with wider applicability to mission scenarios. This paper describes the development of a microsensor capable of surface and in-depth temperature and heat flux measurements for TPS materials appropriate to Titan, Neptune, and Mars aerocapture, and direct entry. The thermal sensor will be monolithic solid state devices composed of thick film platinum RTD on an alumina substrate. Choice of materials and critical dimensions are used to tailor gage response, determined during calibration activities, to specific (forebody vs. aftbody) heating environments. Current design has maximum operating temperature of 1500 K, and allowable constant heat flux of q=28.7 watts per square centimeter, and time constants between 0.05 and 0.2 seconds. The catalytic and radiative response of these heat flux gages can also be changed through the use of appropriate coatings. By using several co-located gages with various surface coatings, data can be obtained to isolate surface heat flux components due to radiation, catalycity and convection. Selectivity to radiative heat flux is a useful feature even for an in-depth gage, as radiative transport may be a significant heat transport mechanism for porous TPS materials in Titan aerocapture. This paper also reports on progress to adapt a previously flown surface recession sensor, based on the Jupiter probe Galileo Analog Resistance Ablation Detector (ARAD), to appropriate aerocapture conditions.

X-ray chemical analyzer for field applications

DOEpatents

Gamba, Otto O. M.

1977-01-01

A self-supporting portable field multichannel X-ray chemical analyzer system comprising a lightweight, flexibly connected, remotely locatable, radioisotope-excited sensing probe utilizing a cryogenically-cooled solid state semi-conductor crystal detector for fast in situ non-destructive, qualitative and quantitative analysis of elements in solid, powder, liquid or slurried form, utilizing an X-ray energy dispersive spectrometry technique.

YSZ thin films with minimized grain boundary resistivity

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

Mills, Edmund M.; Kleine-Boymann, Matthias; Janek, Juergen

2016-03-31

In recent years, interface engineering of solid electrolytes has been explored to increase their ionic conductivity and improve the performance of solid oxide fuel cells and other electrochemical power sources. It has been observed that the ionic conductivity of epitaxially grown thin films of some electrolytes is dramatically enhanced, which is often attributed to effects (e. g. strain-induced mobility changes) at the heterophase boundary with the substrate. Still largely unexplored is the possibility of manipulation of grain boundary resistivity in polycrystalline solid electrolyte films, clearly a limiting factor in their ionic conductivity. Here we report that the ionic conductivity ofmore » yttria stabilized zirconia thin films with nano-­ columnar grains grown on a MgO substrate nearly reaches that of the corresponding single crystal when the thickness of the films becomes less than roughly 8 nm (smaller by a factor of three at 500°C). Using impedance spectroscopy, the grain boundary resistivity was probed as a function of film thickness. The resistivity of the grain boundaries near the film- substrate interface and film surface (within 4 nm of each) was almost entirely eliminated. This minimization of grain boundary resistivity is attributed to Mg2+ diffusion from the MgO substrate into the YSZ grain boundaries, which is supported by time of flight secondary ion mass spectroscopy measurements. We suggest grain boundary “design” as an attractive method to obtain highly conductive solid electrolyte thin films.« less

YSZ thin films with minimized grain boundary resistivity

DOE PAGES

Mills, Edmund M.; Kleine-Boymann, Matthias; Janek, Juergen; ...

2016-03-31

In recent years, interface engineering of solid electrolytes has been explored to increase their ionic conductivity and improve the performance of solid oxide fuel cells and other electrochemical power sources. It has been observed that the ionic conductivity of epitaxially grown thin films of some electrolytes is dramatically enhanced, which is often attributed to effects (e.g. strain-induced mobility changes) at the heterophase boundary with the substrate. Still largely unexplored is the possibility of manipulation of grain boundary resistivity in polycrystalline solid electrolyte films, clearly a limiting factor in their ionic conductivity. Here in this paper, we report that the ionicmore » conductivity of yttria stabilized zirconia thin films with nano-columnar grains grown on a MgO substrate nearly reaches that of the corresponding single crystal when the thickness of the films becomes less than roughly 8 nm (smaller by a factor of three at 500 °C). Using impedance spectroscopy, the grain boundary resistivity was probed as a function of film thickness. The resistivity of the grain boundaries near the film–substrate interface and film surface (within 4 nm of each) was almost entirely eliminated. This minimization of grain boundary resistivity is attributed to Mg 2+ diffusion from the MgO substrate into the YSZ grain boundaries, which is supported by time of flight secondary ion mass spectroscopy measurements. We suggest grain boundary “design” as an attractive method to obtain highly conductive solid electrolyte thin films.« less

How interfaces affect hydrophobically driven polymer folding.

PubMed

Jamadagni, Sumanth N; Godawat, Rahul; Dordick, Jonathan S; Garde, Shekhar

2009-04-02

Studies of folding-unfolding of hydrophobic polymers in water provide an excellent starting point to probe manybody hydrophobic interactions in the context of realistic self-assembly processes. Such studies in bulk water have highlighted the similarities between thermodynamics of polymer collapse and of protein folding, and emphasized the role of hydration-water structure, density, and fluctuations-in the folding kinetics. Hydrophobic polymers are interfacially active-that is, they prefer locations at aqueous interfaces relative to bulk water-consistent with their low solubility. How does the presence of a hydrophobic solid surface or an essentially hydrophobic vapor-water interface affect the structural, thermodynamic, and kinetic aspects of polymer folding? Using extensive molecular dynamics simulations, we show that the large hydrophobic driving force for polymer collapse in bulk water is reduced at a solid alkane-water interface and further reduced at a vapor-water interface. As a result, at the solid-water interface, folded structures are marginally stable, whereas the vapor-liquid interface unfolds polymers completely. Structural sampling is also significantly affected by the interface. For example, at the solid-water interface, polymer conformations are quasi-2- dimensional, with folded states being pancake-like structures. At the vapor-water interface, the hydrophobic polymer is significantly excluded from the water phase and freely samples a broad range of compact to extended structures. Interestingly, although the driving force for folding is considerably lower, kinetics of folding are faster at both interfaces, highlighting the role of enhanced water fluctuations and dynamics at a hydrophobic interface.

Contoured Surface Eddy Current Inspection System

DOEpatents

Batzinger, Thomas James; Fulton, James Paul; Rose, Curtis Wayne; Perocchi, Lee Cranford

2003-04-08

Eddy current inspection of a contoured surface of a workpiece is performed by forming a backing piece of flexible, resiliently yieldable material with a contoured exterior surface conforming in shape to the workpiece contoured surface. The backing piece is preferably cast in place so as to conform to the workpiece contoured surface. A flexible eddy current array probe is attached to the contoured exterior surface of the backing piece such that the probe faces the contoured surface of the workpiece to be inspected when the backing piece is disposed adjacent to the workpiece. The backing piece is then expanded volumetrically by inserting at least one shim into a slot in the backing piece to provide sufficient contact pressure between the probe and the workpiece contoured surface to enable the inspection of the workpiece contoured surface to be performed.

Probing Silica-Biomolecule Interactions by Solid-State NMR and Molecular Dynamics Simulations.

PubMed

Brückner, Stephan Ingmar; Donets, Sergii; Dianat, Arezoo; Bobeth, Manfred; Gutiérrez, Rafael; Cuniberti, Gianaurelio; Brunner, Eike

2016-11-08

Understanding the molecular interactions between inorganic phases such as silica and organic material is fundamental for chromatographic applications, for tailoring silica-enzyme interactions, and for elucidating the mechanisms of biomineralization. The formation, structure, and properties of the organic/inorganic interface is crucial in this context. Here, we investigate the interaction of selectively 13 C-labeled choline with 29 Si-labeled monosilicic acid/silica at the molecular level. Silica/choline nanocomposites were analyzed by solid-state NMR spectroscopy in combination with extended molecular dynamics (MD) simulations to understand the silica/organic interface. Cross-polarization magic angle spinning (CP MAS)-based NMR experiments like 1 H- 13 C CP-REDOR (rotational-echo double resonance), 1 H- 13 C HETCOR (heteronuclear correlation), and 1 H- 29 Si- 1 H double CP are employed to determine spatial parameters. The measurement of 29 Si- 13 C internuclear distances for selectively 13 C-labeled choline provides an experimental parameter that allows the direct verification of MD simulations. Atomistic modeling using classical MD methodologies is performed using the INTERFACE force field. The modeling results are in excellent agreement with the experimental data and reveal the relevant molecular conformations as well as the nature and interplay of the interactions between the choline cation and the silica surface. Electrostatic interactions and hydrogen bonding are both important and depend strongly on the hydration level as well as the charge state of the silica surface.

Anti-Adhesive Behaviors between Solid Hydrate and Liquid Aqueous Phase Induced by Hydrophobic Silica Nanoparticles.

PubMed

Min, Juwon; Baek, Seungjun; Somasundaran, P; Lee, Jae W

2016-09-20

This study introduces an "anti-adhesive force" at the interface of solid hydrate and liquid solution phases. The force was induced by the presence of hydrophobic silica nanoparticles or one of the common anti-agglomerants (AAs), sorbitan monolaurate (Span 20), at the interface. The anti-adhesive force, which is defined as the maximum pushing force that does not induce the formation of a capillary bridge between the cyclopentane (CP) hydrate particle and the aqueous solution, was measured using a microbalance. Both hydrophobic silica nanoparticles and Span 20 can inhibit adhesion between the CP hydrate probe and the aqueous phase because silica nanoparticles have an aggregative property at the interface, and Span 20 enables the hydrate surface to be wetted with oil. Adding water-soluble sodium dodecyl sulfate (SDS) to the nanoparticle system cannot affect the aggregative property or the distribution of silica nanoparticles at the interface and, thus, cannot change the anti-adhesive effect. However, the combined system of Span 20 and SDS dramatically reduces the interfacial tension: emulsion drops were formed at the interface without any energy input and were adsorbed on the CP hydrate surface, which can cause the growth of hydrate particles. Silica nanoparticles have a good anti-adhesive performance with a relatively smaller dosage and are less influenced by the presence of molecular surfactants; consequently, these nanoparticles may have a good potential for hydrate inhibition as AAs.

Recent experimental advances on hydrophobic interactions at solid/water and fluid/water interfaces.

PubMed

Zeng, Hongbo; Shi, Chen; Huang, Jun; Li, Lin; Liu, Guangyi; Zhong, Hong

2015-03-15

Hydrophobic effects play important roles in a wide range of natural phenomena and engineering processes such as coalescence of oil droplets in water, air flotation of mineral particles, and folding and assembly of proteins and biomembranes. In this work, the authors highlight recent experimental attempts to reveal the physical origin of hydrophobic effects by directly quantifying the hydrophobic interaction on both solid/water and fluid/water interfaces using state-of-art nanomechanical techniques such as surface forces apparatus and atomic force microscopy (AFM). For solid hydrophobic surfaces of different hydrophobicity, the range of hydrophobic interaction was reported to vary from ∼10 to >100 nm. With various characterization techniques, the very long-ranged attraction (>100 nm) has been demonstrated to be mainly attributed to nonhydrophobic interaction mechanisms such as pre-existing nanobubbles and molecular rearrangement. By ruling out these factors, intrinsic hydrophobic interaction was measured to follow an exponential law with decay length of 1-2 nm with effective range less than 20 nm. On the other hand, hydrophobic interaction measured at fluid interfaces using AFM droplet/bubble probe technique was found to decay with a much shorter length of ∼0.3 nm. This discrepancy of measured decay lengths is proposed to be attributed to inherent physical distinction between solid and fluid interfaces, which impacts the structure of interface-adjacent water molecules. Direct measurement of hydrophobic interaction on a broader range of interfaces and characterization of interfacial water molecular structure using spectroscopic techniques are anticipated to help unravel the origin of this rigidity-related mismatch of hydrophobic interaction and hold promise to uncover the physical nature of hydrophobic effects. With improved understanding of hydrophobic interaction, intrinsic interaction mechanisms of many biological and chemical pathways can be better elucidated, and novel devices/processes can be developed with capacity to modulate and control the hydrophobic effects from the molecular to the macroscopic scale.

Solid state division progress report, period ending February 29, 1980

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

Not Available

1980-09-01

Research is reported concerning theoretical solid state physics; surface and near-surface properties of solids; defects in solids; transport properties of solids; neutron scattering; crystal growth and characterization; and isotope research materials.

Critical Dipole Length for the Wetting Transition Due to Collective Water-dipoles Interactions

PubMed Central

Wang, Chunlei; Zhou, Bo; Tu, Yusong; Duan, Manyi; Xiu, Peng; Li, Jingye; Fang, Haiping

2012-01-01

The wetting behavior of water on the solid surfaces is fundamental to various physical, chemical and biological processes. Conventionally, the surface with charges or charge dipoles is hydrophilic, whereas the non-polar surface is hydrophobic though some exceptions were recently reported. Using molecular dynamics simulations, we show that there is a critical length of the charge dipoles on the solid surface. The solid surface still exhibited hydrophobic behavior when the dipole length was less than the critical value, indicating that the water molecules on the solid surface seemed not “feel” attractive interactions from the charge dipoles on the solid surface. Those unexpected observations result from the collective interactions between the water molecules and charge dipoles on the solid surface, where the steric exclusion effect between water molecules greatly reduces the water-dipole interactions. Remarkably, the steric exclusion effect is also important for surfaces with charge dipole lengths greater than this critical length. PMID:22496954

Eddy Current Probe for Surface and Sub-Surface Inspection

NASA Technical Reports Server (NTRS)

Wincheski, Russell A. (Inventor); Simpson, John W. (Inventor)

2014-01-01

An eddy current probe includes an excitation coil for coupling to a low-frequency alternating current (AC) source. A magneto-resistive sensor is centrally disposed within and at one end of the excitation coil to thereby define a sensing end of the probe. A tubular flux-focusing lens is disposed between the excitation coil and the magneto-resistive sensor. An excitation wire is spaced apart from the magneto-resistive sensor in a plane that is perpendicular to the sensor's axis of sensitivity and such that, when the sensing end of the eddy current probe is positioned adjacent to the surface of a structure, the excitation wire is disposed between the magneto-resistive sensor and the surface of the structure. The excitation wire is coupled to a high-frequency AC source. The excitation coil and flux-focusing lens can be omitted when only surface inspection is required.

Solid-State Division progress report for period ending March 31, 1983

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

Green, P.H.; Watson, D.M.

1983-09-01

Progress and activities are reported on: theoretical solid-state physics (surfaces; electronic, vibrational, and magnetic properties; particle-solid interactions; laser annealing), surface and near-surface properties of solids (surface, plasma-material interactions, ion implantation and ion-beam mixing, pulsed-laser and thermal processing), defects in solids (radiation effects, fracture, impurities and defects, semiconductor physics and photovoltaic conversion), transport properties of solids (fast-ion conductors, superconductivity, mass and charge transport in materials), neutron scattering (small-angle scattering, lattice dynamics, magnetic properties, structure and instrumentation), and preparation and characterization of research materials (growth and preparative methods, nuclear waste forms, special materials). (DLC)

DNA microdevice for electrochemical detection of Escherichia coli 0157:H7 molecular markers.

PubMed

Berganza, J; Olabarria, G; García, R; Verdoy, D; Rebollo, A; Arana, S

2007-04-15

An electrochemical DNA sensor based on the hybridization recognition of a single-stranded DNA (ssDNA) probe immobilized onto a gold electrode to its complementary ssDNA is presented. The DNA probe is bound on gold surface electrode by using self-assembled monolayer (SAM) technology. An optimized mixed SAM with a blocking molecule preventing the nonspecific adsorption on the electrode surface has been prepared. In this paper, a DNA biosensor is designed by means of the immobilization of a single stranded DNA probe on an electrochemical transducer surface to recognize specifically Escherichia coli (E. coli) 0157:H7 complementary target DNA sequence via cyclic voltammetry experiments. The 21 mer DNA probe including a C6 alkanethiol group at the 5' phosphate end has been synthesized to form the SAM onto the gold surface through the gold sulfur bond. The goal of this paper has been to design, characterise and optimise an electrochemical DNA sensor. In order to investigate the oligonucleotide probe immobilization and the hybridization detection, experiments with different concentration of DNA and mismatch sequences have been performed. This microdevice has demonstrated the suitability of oligonucleotide Self-assembled monolayers (SAMs) on gold as immobilization method. The DNA probes deposited on gold surface have been functional and able to detect changes in bases sequence in a 21-mer oligonucleotide.

Evidence for Natural Variability in Marine Stratocumulus Cloud Properties Due to Cloud-Aerosol

NASA Technical Reports Server (NTRS)

Albrecht, Bruce; Sharon, Tarah; Jonsson, Haf; Minnis, Patrick; Minnis, Patrick; Ayers, J. Kirk; Khaiyer, Mandana M.

2004-01-01

In this study, aircraft observations from the Interdisciplinary Remotely-Piloted Aircraft Studies (CIRPAS) Twin Otter are used to characterize the variability in drizzle, cloud, and aerosol properties associated with cloud rifts and the surrounding solid clouds observed off the coast of California. A flight made on 16 July 1999 provided measurements directly across an interface between solid and rift cloud conditions. Aircraft instrumentation allowed for measurements of aerosol, cloud droplet, and drizzle spectra. CCN concentrations were measured in addition to standard thermodynamic variables and the winds. A Forward Scatter Spectrometer Probe (FSSP) measured size distribution of cloud-sized droplets. A Cloud Imaging Probe (CIP) was used to measure distributions of drizzle-sized droplets. Aerosol distributions were obtained from a Cloud Aerosol Scatterprobe (CAS). The CAS probe measured aerosols, cloud droplets and drizzle-sized drops; for this study. The CAS probe was used to measure aerosols in the size range of 0.5 micron - 1 micron. Smaller aerosols were characterized using an Ultrafine Condensation Particle Counter (CPC) sensor. The CPC was used to measure particles with diameters greater than 0.003 micron. By subtracting different count concentrations measured with the CPC, this probe was capable of identifying ultrafine particles those falling in the size range of 3 nanometers - 7 nanometers that are believed to be associated with new particle production.

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

NASA Astrophysics Data System (ADS)

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

2018-06-01

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

Method for nanoscale spatial registration of scanning probes with substrates and surfaces

NASA Technical Reports Server (NTRS)

Wade, Lawrence A. (Inventor)

2010-01-01

Embodiments in accordance with the present invention relate to methods and apparatuses for aligning a scanning probe used to pattern a substrate, by comparing the position of the probe to a reference location or spot on the substrate. A first light beam is focused on a surface of the substrate as a spatial reference point. A second light beam then illuminates the scanning probe being used for patterning. An optical microscope images both the focused light beam, and a diffraction pattern, shadow, or light backscattered by the illuminated scanning probe tip of a scanning probe microscope (SPM), which is typically the tip of the scanning probe on an atomic force microscope (AFM). Alignment of the scanning probe tip relative to the mark is then determined by visual observation of the microscope image. This alignment process may be repeated to allow for modification or changing of the scanning probe microscope tip.

Spreading of Electrolyte Drops on Charged Surfaces: Electric Double Layer Effects on Drop Dynamics

NASA Astrophysics Data System (ADS)

Bae, Kyeong; Sinha, Shayandev; Chen, Guang; Das, Siddhartha

2015-11-01

Drop spreading is one of the most fundamental topics of wetting. Here we study the spreading of electrolyte drops on charged surfaces. The electrolyte solution in contact with the charged solid triggers the formation of an electric double layer (EDL). We develop a theory to analyze how the EDL affects the drop spreading. The drop dynamics is studied by probing the EDL effects on the temporal evolution of the contact angle and the base radius (r). The EDL effects are found to hasten the spreading behaviour - this is commensurate to the EDL effects causing a ``philic'' tendency in the drops (i.e., drops attaining a contact angle smaller than its equilibrium value), as revealed by some of our recent papers. We also develop scaling laws to illustrate the manner in which the EDL effects make the r versus time (t) variation deviate from the well known r ~tn variation, thereby pinpointing the attainment of different EDL-mediated spreading regimes.

Reactive molecular dynamics simulation of solid nitromethane impact on (010) surfaces induced and nonimpact thermal decomposition.

PubMed

Guo, Feng; Cheng, Xin-lu; Zhang, Hong

2012-04-12

Which is the first step in the decomposition process of nitromethane is a controversial issue, proton dissociation or C-N bond scission. We applied reactive force field (ReaxFF) molecular dynamics to probe the initial decomposition mechanisms of nitromethane. By comparing the impact on (010) surfaces and without impact (only heating) for nitromethane simulations, we found that proton dissociation is the first step of the pyrolysis of nitromethane, and the C-N bond decomposes in the same time scale as in impact simulations, but in the nonimpact simulation, C-N bond dissociation takes place at a later time. At the end of these simulations, a large number of clusters are formed. By analyzing the trajectories, we discussed the role of the hydrogen bond in the initial process of nitromethane decompositions, the intermediates observed in the early time of the simulations, and the formation of clusters that consisted of C-N-C-N chain/ring structures.

UV Signatures of Ices: Moons in the Solar System

NASA Astrophysics Data System (ADS)

Hendrix, A. R.; Hansen, C. J.; Retherford, K. D.; Vilas, F.

2017-12-01

Using Earth-orbiting telescopes such as the International Ultraviolet Explorer and the Hubble Space Telescope, significant advances have been made in the area of ultraviolet observations of solar system objects. More in-depth studies have been made using interplanetary probes such as Galileo, Cassini and Lunar Reconnaissance Orbiter (LRO). While the UV spectral range has traditionally been used to study atmospheric and auroral processes, there is much to be learned by examining solid surfaces in the UV, including surface composition, weathering processes and effects, and the generation of thin atmospheres. Here we focus on moons in the solar system, including Earth's moon and the Saturnian satellites. The diagnostic UV signature of H2O is used to study ice in the lunar polar regions as well as hydration at lower latitudes, in observations from LRO LAMP. The water ice signature is nearly ubiquitous in the Saturn system; Cassini UVIS datasets are used to study grain sizes, exogenic processes/effects and non-ice species.

OAST Space Theme Workshop. Volume 3: Working group summary. 3: Sensors (E-3). A. Statement. B. Technology needs (form 1). C. Priority assessment (form 2). D. Additional assessment

NASA Technical Reports Server (NTRS)

1976-01-01

Developments required to support the space power, SETI, solar system exploration and global services programs are identified. Instrumentation and calibration sensors (rather than scientific) are needed for the space power system. Highly sophisticated receivers for narrowband detection of microwave sensors and sensors for automated stellar cataloging to provide a mapping data base for SETI are needed. Various phases of solar system exploration require large area solid state imaging arrays from UV to IR; a long focal plane telescope; high energy particle detectors; advanced spectrometers; a gravitometer; and atmospheric distanalyzer; sensors for penetrometers; in-situ sensors for surface chemical analysis, life detection, spectroscopic and microscopic analyses of surface soils, and for meteorological measurements. Active and passive multiapplication sensors, advanced multispectral scanners with improved resolution in the UV and IR ranges, and laser techniques for advanced probing and oceanographic characterization will enhance for global services.

Development and characterization of a microheater array device for real-time DNA mutation detection

NASA Astrophysics Data System (ADS)

Williams, Layne; Okandan, Murat; Chagovetz, Alex; Blair, Steve

2008-04-01

DNA analysis, specifically single nucleotide polymorphism (SNP) detection, is becoming increasingly important in rapid diagnostics and disease detection. Temperature is often controlled to help speed reaction rates and perform melting of hybridized oligonucleotides. The difference in melting temperatures, Tm, between wild-type and SNP sequences, respectively, to a given probe oligonucleotide, is indicative of the specificity of the reaction. We have characterized Tm's in solution and on a solid substrate of three sequences from known mutations associated with Cystic Fibrosis. Taking advantage of Tm differences, a microheater array device was designed to enable individual temperature control of up to 18 specific hybridization events. The device was fabricated at Sandia National Laboratories using surface micromachining techniques. The microheaters have been characterized using an IR camera at Sandia and show individual temperature control with minimal thermal cross talk. Development of the device as a real-time DNA detection platform, including surface chemistry and associated microfluidics, is described.

Development and characterization of a microheater array device for real-time DNA mutation detection

NASA Astrophysics Data System (ADS)

Williams, Layne; Okandan, Murat; Chagovetz, Alex; Blair, Steve

2008-02-01

DNA analysis, specifically single nucleotide polymorphism (SNP) detection, is becoming increasingly important in rapid diagnostics and disease detection. Temperature is often controlled to help speed reaction rates and perform melting of hybridized oligonucleotides. The difference in melting temperatures, Tm, between wild-type and SNP sequences, respectively, to a given probe oligonucleotide, is indicative of the specificity of the reaction. We have characterized Tm's in solution and on a solid substrate of three sequences from known mutations associated with Cystic Fibrosis. Taking advantage of Tm differences, a microheater array device was designed to enable individual temperature control of up to 18 specific hybridization events. The device was fabricated at Sandia National Laboratories using surface micromachining techniques. The microheaters have been characterized using an IR camera at Sandia and show individual temperature control with minimal thermal cross talk. Development of the device as a real-time DNA detection platform, including surface chemistry and associated microfluidics, is described.

Measuring Fluxes Of Heat To A Plasma-Arc Anode

NASA Technical Reports Server (NTRS)

Sankovic, John M.; Menart, James A.; Pfender, Emil; Heberlein, Joachim

1995-01-01

Three probes constructed to provide measurements indicative of conductive, convective, and radiative transfer of heat from free-burning plasma arc to water-cooled copper anode used in generating arc. Each probe consists mainly of copper body with two thermocouples embedded at locations 4 mm apart along length. Thermocouples provide measure of rate of conduction of heat along probe and transfers of heat from plasma to sensing surface at tip of probe. Probes identical except sensing surface of one uncoated and other two coated with different materials to make them sensitive to different components of overall flux of heat.

Scanning probe recognition microscopy investigation of tissue scaffold properties

PubMed Central

Fan, Yuan; Chen, Qian; Ayres, Virginia M; Baczewski, Andrew D; Udpa, Lalita; Kumar, Shiva

2007-01-01

Scanning probe recognition microscopy is a new scanning probe microscopy technique which enables selective scanning along individual nanofibers within a tissue scaffold. Statistically significant data for multiple properties can be collected by repetitively fine-scanning an identical region of interest. The results of a scanning probe recognition microscopy investigation of the surface roughness and elasticity of a series of tissue scaffolds are presented. Deconvolution and statistical methods were developed and used for data accuracy along curved nanofiber surfaces. Nanofiber features were also independently analyzed using transmission electron microscopy, with results that supported the scanning probe recognition microscopy-based analysis. PMID:18203431

Scanning probe recognition microscopy investigation of tissue scaffold properties.

PubMed

Fan, Yuan; Chen, Qian; Ayres, Virginia M; Baczewski, Andrew D; Udpa, Lalita; Kumar, Shiva

2007-01-01

Scanning probe recognition microscopy is a new scanning probe microscopy technique which enables selective scanning along individual nanofibers within a tissue scaffold. Statistically significant data for multiple properties can be collected by repetitively fine-scanning an identical region of interest. The results of a scanning probe recognition microscopy investigation of the surface roughness and elasticity of a series of tissue scaffolds are presented. Deconvolution and statistical methods were developed and used for data accuracy along curved nanofiber surfaces. Nanofiber features were also independently analyzed using transmission electron microscopy, with results that supported the scanning probe recognition microscopy-based analysis.

Surface films and metallurgy related to lubrication and wear. Ph.D. Thesis - Tokyo Inst. of Technology

NASA Technical Reports Server (NTRS)

Buckley, D. H.

1981-01-01

The nature of the tribological surface is identified and characterized with respect to adhesion, friction, wear, and lubricating properties. Surface analysis is used to identify the role of environmental constituents on tribological behavior. The effect of solid to solid interactions for metals in contact with metals, ceramics, semiconductors, carbons, and polymers is discussed. The data presented indicate that the tribological surface is markedly different than an ideal solid surface. The environment is shown to affect strongly the behavior of two solids in contact. Results also show that small amounts of alloying elements in base metals can alter markedly adhesion, friction, and wear by segregating to the solid surface.

Evidence for weakly bound electrons in non-irradiated alkane crystals: The electrons as a probe of structural differences in crystals.

PubMed

Pietrow, M; Gagoś, M; Misiak, L E; Kornarzyński, K; Szurkowski, J; Rochowski, P; Grzegorczyk, M

2015-02-14

It is generally assumed that weakly bound (trapped) electrons in organic solids come only from radiolytical (or photochemical) processes like ionization caused by an excited positron entering the sample. This paper presents evidence for the presence of these electrons in non-irradiated samples of docosane. This can be due to the triboelectrification process. We argue that these electrons can be located (trapped) either in interlamellar gaps or in spaces made by non-planar conformers. Electrons from the former ones are bound more weakly than electrons from the latter ones. The origin of Vis absorption for the samples is explained. These spectra can be used as a probe indicating differences in the solid structures of hydrocarbons.

Self-Nulling Eddy Current Probe for Surface and Subsurface Flaw Detection

NASA Technical Reports Server (NTRS)

Wincheski, B.; Fulton, J. P.; Nath, S.; Namkung, M.; Simpson, J. W.

1994-01-01

An eddy current probe which provides a null-signal in the presence of unflawed material without the need for any balancing circuitry has been developed at NASA Langley Research Center. Such a unique capability of the probe reduces set-up time, eliminates tester configuration errors, and decreases instrumentation requirements. The probe is highly sensitive to surface breaking fatigue cracks, and shows excellent resolution for the measurement of material thickness, including material loss due to corrosion damage. The presence of flaws in the material under test causes an increase in the extremely stable and reproducible output voltage of the probe. The design of the probe and some examples illustrating its flaw detection capabilities are presented.

Unusual dynamic dewetting behavior of smooth perfluorinated hybrid films: potential advantages over conventional textured and liquid-infused perfluorinated surfaces.

PubMed

Urata, Chihiro; Masheder, Benjamin; Cheng, Dalton F; Hozumi, Atsushi

2013-10-08

From a viewpoint of reducing the burden on the environment and human health, an alternative method for preparing liquid-repellent surfaces without relying on the long perfluorocarbons (C((X-1)/2)F(X), X ≥ 17) has been strongly demanded lately. In this study, we have successfully demonstrated that dynamic dewettability toward various probe liquids (polar and nonpolar liquids with high or low surface tension) can be tuned by not only controlling surface chemistries (surface energies) but also the physical (solid-like or liquid-like) nature of the surface. We prepared smooth and transparent organic-inorganic hybrid films exhibiting unusual dynamic dewetting behavior toward various probe liquids using a simple sol-gel reaction based on the co-hydrolysis and co-condensation of a mixture including a range of perfluoroalkylsilanes (FASX, C((X-1)/2)F(X)CH2CH2Si(OR)3, where X = 3, 9, 13, and 17) and tetramethoxysilane (Si(OCH3)4, TMOS). Dynamic contact angle (CA) and substrate tilt angle (TA) measurements confirmed that our FASX-hybrid films exhibited excellent dynamic dewetting properties and were mostly independent of the length of perfluoroalkyl (Rf) groups. For example, 10 μL droplets of ultralow surface tension liquids (e.g., diethyl ether (γ = 16.26 dyn/cm) and n-pentane (γ = 15.51 dyn/cm)) could move easily on our FAS9-, FAS13-, and FAS17-hybrid film surfaces at low substrate TAs (<4°) without pinning. This is comparable or superior to the best perfluorinated textured and flat surfaces reported so far. This exceptional dynamic dewetting behavior appeared only when TMOS molecules were added to the precursor solutions; we assume this is due to co-condensed TMOS-derived silica species working as spacers between the neighboring Rf chains, enabling them to rotate freely and in doing so provide a surface with liquid-like properties. This led to the distinguished dynamic dewettability of our hybrid films, regardless of the small static CAs. Our FASX-hybrid films also displayed excellent chemical and physical durability against thermal stress (~250 °C), high-temperature (150 °C) oil vapor, and various other media (perfluoro liquid, boiling water, and weak acid) without degrading their dynamic dewettability. Such exceptional durability has been rarely seen on conventional perfluorinated surfaces reported so far.

Distinct ice patterns on solid surfaces with various wettabilities

PubMed Central

Liu, Jie; Zhu, Chongqin; Liu, Kai; Jiang, Ying; Song, Yanlin; Francisco, Joseph S.; Zeng, Xiao Cheng; Wang, Jianjun

2017-01-01

No relationship has been established between surface wettability and ice growth patterns, although ice often forms on top of solid surfaces. Here, we report experimental observations obtained using a process specially designed to avoid the influence of nucleation and describe the wettability-dependent ice morphology on solid surfaces under atmospheric conditions and the discovery of two growth modes of ice crystals: along-surface and off-surface growth modes. Using atomistic molecular dynamics simulation analysis, we show that these distinct ice growth phenomena are attributable to the presence (or absence) of bilayer ice on solid surfaces with different wettability; that is, the formation of bilayer ice on hydrophilic surface can dictate the along-surface growth mode due to the structural match between the bilayer hexagonal ice and the basal face of hexagonal ice (ice Ih), thereby promoting rapid growth of nonbasal faces along the hydrophilic surface. The dramatically different growth patterns of ice on solid surfaces are of crucial relevance to ice repellency surfaces. PMID:29073045

Distinct ice patterns on solid surfaces with various wettabilities.

PubMed

Liu, Jie; Zhu, Chongqin; Liu, Kai; Jiang, Ying; Song, Yanlin; Francisco, Joseph S; Zeng, Xiao Cheng; Wang, Jianjun

2017-10-24

No relationship has been established between surface wettability and ice growth patterns, although ice often forms on top of solid surfaces. Here, we report experimental observations obtained using a process specially designed to avoid the influence of nucleation and describe the wettability-dependent ice morphology on solid surfaces under atmospheric conditions and the discovery of two growth modes of ice crystals: along-surface and off-surface growth modes. Using atomistic molecular dynamics simulation analysis, we show that these distinct ice growth phenomena are attributable to the presence (or absence) of bilayer ice on solid surfaces with different wettability; that is, the formation of bilayer ice on hydrophilic surface can dictate the along-surface growth mode due to the structural match between the bilayer hexagonal ice and the basal face of hexagonal ice (ice I h ), thereby promoting rapid growth of nonbasal faces along the hydrophilic surface. The dramatically different growth patterns of ice on solid surfaces are of crucial relevance to ice repellency surfaces. Published under the PNAS license.

Simulation of municipal solid waste degradation in aerobic and anaerobic bioreactor landfills.

PubMed

Patil, Bhagwan Shamrao; C, Agnes Anto; Singh, Devendra Narain

2017-03-01

Municipal solid waste generation is huge in growing cities of developing nations such as India, owing to the rapid industrial and population growth. In addition to various methods for treatment and disposal of municipal solid waste (landfills, composting, bio-methanation, incineration and pyrolysis), aerobic/anaerobic bioreactor landfills are gaining popularity for economical and effective disposal of municipal solid waste. However, efficiency of municipal solid waste bioreactor landfills primarily depends on the municipal solid waste decomposition rate, which can be accelerated through monitoring moisture content and temperature by using the frequency domain reflectometry probe and thermocouples, respectively. The present study demonstrates that these landfill physical properties of the heterogeneous municipal solid waste mass can be monitored using these instruments, which facilitates proper scheduling of the leachate recirculation for accelerating the decomposition rate of municipal solid waste.

Optical analysis of the star-tracker telescope for Gravity Probe

NASA Technical Reports Server (NTRS)

Zissa, D. E.

1984-01-01

A ray tracing modeling of the star tracker telescope for Gravity Probe was used to predict the character of the output signal and its sensitivity to fabrication errors. In particular, the impact of the optical subsystem on the requirement of 1 milliarc second signal linearity over a + or - 50 milliarc second range was examined. Photomultiplier and solid state detector options were considered. Recommendations are made.

How Properties of Solid Surfaces Modulate the Nucleation of Gas Hydrate

PubMed Central

Bai, Dongsheng; Chen, Guangjin; Zhang, Xianren; Sum, Amadeu K.; Wang, Wenchuan

2015-01-01

Molecular dynamics simulations were performed for CO2 dissolved in water near silica surfaces to investigate how the hydrophilicity and crystallinity of solid surfaces modulate the local structure of adjacent molecules and the nucleation of CO2 hydrates. Our simulations reveal that the hydrophilicity of solid surfaces can change the local structure of water molecules and gas distribution near liquid-solid interfaces, and thus alter the mechanism and dynamics of gas hydrate nucleation. Interestingly, we find that hydrate nucleation tends to occur more easily on relatively less hydrophilic surfaces. Different from surface hydrophilicity, surface crystallinity shows a weak effect on the local structure of adjacent water molecules and on gas hydrate nucleation. At the initial stage of gas hydrate growth, however, the structuring of molecules induced by crystalline surfaces are more ordered than that induced by amorphous solid surfaces. PMID:26227239

Characterization of Pharmaceutical Cocrystals and Salts by Dynamic Nuclear Polarization-Enhanced Solid-State NMR Spectroscopy

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

Zhao, Li; Hanrahan, Michael P.; Chakravarty, Paroma

Multicomponent solids such as cocrystals have emerged as a way to control and engineer the stability, solubility and manufacturability of solid active pharmaceutical ingredients (APIs). Cocrystals are typically formed by solution- or solid-phase reactions of APIs with suitable cocrystal coformers, which are often weak acids. One key structural question about a given multicomponent solid is whether it should be classified as a salt, where the basic API is protonated by the acid, or as a cocrystal, where the API and coformer remain neutral and engage in hydrogen bonding interactions. It has previously been demonstrated that solid-state NMR spectroscopy is amore » powerful probe of structure in cocrystals and salts of APIs, however, the poor sensitivity of solid-state NMR spectroscopy usually restricts the types of experiments that can be performed. Here relayed dynamic nuclear polarization (DNP) was applied to reduce solid-state NMR experiments by one to two orders of magnitude for salts and cocrystals of a complex API. The large sensitivity gains from DNP facilitates rapid acquisition of natural isotopic abundance 13C and 15N solid-state NMR spectra. Critically, DNP enables double resonance 1H-15N solid-state NMR experiments such as 2D 1H-15N HETCOR, 1H-15N CP-build up, 15N{1H} J-resolved/attached proton tests, 1H-15N DIPSHIFT and 1H-15N PRESTO. The latter two experiments allow 1H-15N dipolar coupling constants and H-N bond lengths to be accurately measured, providing an unambiguous assignment of nitrogen protonation state and definitive classification of the multi-component solids as cocrystals or salts. In conclusion, these types of measurements should also be extremely useful in the context of polymorph discrimination, NMR crystallography structure determination and for probing hydrogen bonding in a variety of organic materials.« less

Characterization of Pharmaceutical Cocrystals and Salts by Dynamic Nuclear Polarization-Enhanced Solid-State NMR Spectroscopy

DOE PAGES

Zhao, Li; Hanrahan, Michael P.; Chakravarty, Paroma; ...

2018-02-15

Multicomponent solids such as cocrystals have emerged as a way to control and engineer the stability, solubility and manufacturability of solid active pharmaceutical ingredients (APIs). Cocrystals are typically formed by solution- or solid-phase reactions of APIs with suitable cocrystal coformers, which are often weak acids. One key structural question about a given multicomponent solid is whether it should be classified as a salt, where the basic API is protonated by the acid, or as a cocrystal, where the API and coformer remain neutral and engage in hydrogen bonding interactions. It has previously been demonstrated that solid-state NMR spectroscopy is amore » powerful probe of structure in cocrystals and salts of APIs, however, the poor sensitivity of solid-state NMR spectroscopy usually restricts the types of experiments that can be performed. Here relayed dynamic nuclear polarization (DNP) was applied to reduce solid-state NMR experiments by one to two orders of magnitude for salts and cocrystals of a complex API. The large sensitivity gains from DNP facilitates rapid acquisition of natural isotopic abundance 13C and 15N solid-state NMR spectra. Critically, DNP enables double resonance 1H-15N solid-state NMR experiments such as 2D 1H-15N HETCOR, 1H-15N CP-build up, 15N{1H} J-resolved/attached proton tests, 1H-15N DIPSHIFT and 1H-15N PRESTO. The latter two experiments allow 1H-15N dipolar coupling constants and H-N bond lengths to be accurately measured, providing an unambiguous assignment of nitrogen protonation state and definitive classification of the multi-component solids as cocrystals or salts. In conclusion, these types of measurements should also be extremely useful in the context of polymorph discrimination, NMR crystallography structure determination and for probing hydrogen bonding in a variety of organic materials.« less