Differentiating and characterizing geminal silanols in silicas by (29)Si NMR spectroscopy.

PubMed

Murray, David K

2010-12-01

Single and geminal hydroxyl species in silicas have been characterized using solid-state (29)Si NMR spectroscopy. Differentiating hydroxyl types is important in understanding their roles in chemical toxicity mechanisms for inhaled crystalline silicas responsible for silicosis. (1)H-(29)Si cross polarization NMR spectroscopy has been employed to obtain (29)Si NMR chemical shift data and signal accrual and relaxation characteristics. Spectral deconvolution is used to examine relative single and geminal hydroxyl resonance areas for a series of representative silicas and silica gels. Silicon-containing materials examined include 1878a quartz, and 1879a cristobalite from the National Institute for Science and Technology, kaolin, and several widely used respirable silicas and silica gels. Geminal hydroxyls were observed in every case, with relative resonance areas accounting for 21-65% of total hydroxyl signals. Factors affecting relative areas measured as a function of contact time, relaxation, and surface area are discussed. Subsequent (29)Si and (31)P NMR studies of a silica coated with various sodium hydrogen phosphates show preferential single silanol-phosphate interaction for basic phosphates, and oligomerization products for acidic phosphates. Geminal hydroxyl resonance areas displayed significant error (4-17%) for low surface area silicas, limiting this method to studies exhibiting major changes in chemical or spectroscopic properties. Published by Elsevier Inc.

Influences of internal resistance and specific surface area of electrode materials on characteristics of electric double layer capacitors

NASA Astrophysics Data System (ADS)

Suda, Yoshiyuki; Mizutani, Akitaka; Harigai, Toru; Takikawa, Hirofumi; Ue, Hitoshi; Umeda, Yoshito

2017-01-01

We fabricated electric double layer capacitors (EDLCs) using particulate and fibrous types of carbon nanomaterials with a wide range of specific surface areas and resistivity as an active material. The carbon nanomaterials used in this study are carbon nanoballoons (CNBs), onion-like carbon (OLC), and carbon nanocoils (CNCs). A commercially used activated carbon (AC) combined with a conductive agent was used as a comparison. We compared the EDLC performance using cyclic voltammetry (CV), galvanostatic charge/discharge testing, and electrochemical impedance spectroscopy (EIS). OLC showed a poor EDLC performance, although it has the lowest resistivity among the carbon nanomaterials. CNB, which has a 1/16 lower specific surface area than AC but higher specific surface area than CNC and OLC, had a higher specific capacitance than CNC and OLC. Moreover, at current densities of 1.5 Ag-1 and larger, the specific capacitance of the EDLC using CNB was almost the same as that using AC. Electrochemical impedance spectroscopy of the EDLCs revealed that the CNB and CNC electrodes had a much lower internal resistance than the AC electrode, which correlated with a low capacitance maintenance factor as the current density increased.

Preparation of porous Si and TiO 2 nanofibres using a sulphur-templating method for lithium storage

DOE PAGES

McCormac, Kathleen; Byrd, Ian; Brannen, Rodney; ...

2015-02-03

We prepared highly porous Si/TiO 2 composite nanofibres using a unique sulphur-templating method combined with electrospinning. The structure, morphology, surface area, phase and composition of these nanofibres were characterized using Raman spectroscopy, scanning electron microscopy, powder X-ray diffraction, surface area analyser and thermogravimetric analyser. The specific surface area of Si/TiO 2 porous NFs is as large as 387m 2g -1, whose silicon capacity can be maintained above 1580mAhg -1 in 180 cycles.

Studies of cartilaginous tissue using Raman spectroscopy method

NASA Astrophysics Data System (ADS)

Timchenko, Pavel E.; Timchenko, Elena V.; Volova, Larisa T.; Dolgyshkin, Dmitry A.; Markova, Maria D.; Kylabyhova, A. Y.; Kornilin, Dmitriy V.

2016-10-01

The work presents the results of studies of samples of human articular surface of the knee joint, obtained by Raman spectroscopy implementedduring endoprosthesis replacement surgery . The main spectral characteristics of articular surface areas with varying degrees of cartilage damage were detected at 956 cm-1, 1066 cm-1 wavenumbers, corresponding to phosphate and carbonate, and at 1660 cm-1, 1271 cm-1 wavenumbers, corresponding to amide I and amide III. Criteria allowing to identify the degree of articular hyaline cartilage damage were introduced.

Infrared spectroscopy and density functional theory investigation of calcite, chalk, and coccoliths--do we observe the mineral surface?

PubMed

Andersson, M P; Hem, C P; Schultz, L N; Nielsen, J W; Pedersen, C S; Sand, K K; Okhrimenko, D V; Johnsson, A; Stipp, S L S

2014-11-13

We have measured infrared spectra from several types of calcite: chalk, freshly cultured coccoliths produced by three species of algae, natural calcite (Iceland Spar), and two types of synthetic calcite. The most intense infrared band, the asymmetric carbonate stretch vibration, is clearly asymmetric for the coccoliths and the synthetic calcite prepared using the carbonation method. It can be very well fitted by two peaks: a narrow Lorenzian at lower frequency and a broader Gaussian at higher frequency. These two samples both have a high specific surface area. Density functional theory for bulk calcite and several calcite surface systems allows for assignment of the infrared bands. The two peaks that make up the asymmetric carbonate stretch band come from the bulk (narrow Lorenzian) and from a combination of two effects (broad Gaussian): the surface or near surface of calcite and line broadening from macroscopic dielectric effects. We detect water adsorbed on the high surface area synthetic calcite, which permits observation of the chemistry of thin liquid films on calcite using transmission infrared spectroscopy. The combination of infrared spectroscopy and density functional theory also allowed us to quantify the amount of polysaccharides associated with the coccoliths. The amount of polysaccharides left in chalk, demonstrated to be present in other work, is below the IR detection limit, which is 0.5% by mass.

Imaging fluorescence-correlation spectroscopy for measuring fast surface diffusion at liquid/solid interfaces.

PubMed

Cooper, Justin T; Harris, Joel M

2014-08-05

The development of techniques to probe interfacial molecular transport is important for understanding and optimizing surface-based analytical methods including surface-enhanced spectroscopies, biological assays, and chemical separations. Single-molecule-fluorescence imaging and tracking has been used to measure lateral diffusion rates of fluorescent molecules at surfaces, but the technique is limited to the study of slower diffusion, where molecules must remain relatively stationary during acquisition of an image in order to build up sufficient intensity in a spot to detect and localize the molecule. Although faster time resolution can be achieved by fluorescence-correlation spectroscopy (FCS), where intensity fluctuations in a small spot are related to the motions of molecules on the surface, long-lived adsorption events arising from surface inhomogeneity can overwhelm the correlation measurement and mask the surface diffusion of the moving population. Here, we exploit a combination of these two techniques, imaging-FCS, for measurement of fast interfacial transport at a model chromatographic surface. This is accomplished by rapid imaging of the surface using an electron-multiplied-charged-coupled-device (CCD) camera, while limiting the acquisition to a small area on the camera to allow fast framing rates. The total intensity from the sampled region is autocorrelated to determine surface diffusion rates of molecules with millisecond time resolution. The technique allows electronic control over the acquisition region, which can be used to avoid strong adsorption sites and thus minimize their contribution to the measured autocorrelation decay and to vary the acquisition area to resolve surface diffusion from adsorption and desorption kinetics. As proof of concept, imaging-FCS was used to measure surface diffusion rates, interfacial populations, and adsorption-desorption rates of 1,1'-dioctadecyl-3,3,3'3'-tetramethylindocarbocyanine (DiI) on planar C18- and C1-modified surfaces.

Surface Plasmon Resonance: An Introduction to a Surface Spectroscopy Technique

ERIC Educational Resources Information Center

Tang, Yijun; Zeng, Xiangqun; Liang, Jennifer

2010-01-01

Surface plasmon resonance (SPR) has become an important optical biosensing technology in the areas of biochemistry, biology, and medical sciences because of its real-time, label-free, and noninvasive nature. The high cost of commercial devices and consumables has prevented SPR from being introduced in the undergraduate laboratory. Here, we present…

Exploring Surface Analysis Techniques for the Detection of Molecular Contaminants on Spacecraft

NASA Technical Reports Server (NTRS)

Rutherford, Gugu N.; Seasly, Elaine; Thornblom, Mark; Baughman, James

2016-01-01

Molecular contamination is a known area of concern for spacecraft. To mitigate this risk, projects involving space flight hardware set requirements in a contamination control plan that establishes an allocation budget for the exposure of non-volatile residues (NVR) onto critical surfaces. The purpose of this work will focus on non-contact surface analysis and in situ monitoring to mitigate molecular contamination on space flight hardware. By using Scanning Electron Microscopy and Energy Dispersive Spectroscopy (SEM-EDS) with Raman Spectroscopy, an unlikely contaminant was identified on space flight hardware. Using traditional and surface analysis methods provided the broader view of the contamination sources allowing for best fit solutions to prevent any future exposure.

The Evolution of Silica Nanoparticle-polyester Coatings on Surfaces Exposed to Sunlight.

PubMed

Truong, Vi Khanh; Stefanovic, Miljan; Maclaughlin, Shane; Tobin, Mark; Vongsvivut, Jitraporn; Al Kobaisi, Mohammad; Crawford, Russell J; Ivanova, Elena P

2016-10-11

Corrosion of metallic surfaces is prevalent in the environment and is of great concern in many areas, including the military, transport, aviation, building and food industries, amongst others. Polyester and coatings containing both polyester and silica nanoparticles (SiO2NPs) have been widely used to protect steel substrata from corrosion. In this study, we utilized X-ray photoelectron spectroscopy, attenuated total reflection infrared micro-spectroscopy, water contact angle measurements, optical profiling and atomic force microscopy to provide an insight into how exposure to sunlight can cause changes in the micro- and nanoscale integrity of the coatings. No significant change in surface micro-topography was detected using optical profilometry, however, statistically significant nanoscale changes to the surface were detected using atomic force microscopy. Analysis of the X-ray photoelectron spectroscopy and attenuated total reflection infrared micro-spectroscopy data revealed that degradation of the ester groups had occurred through exposure to ultraviolet light to form COO·, -H2C·, -O·, -CO· radicals. During the degradation process, CO and CO2 were also produced.

Durable anti-fogging effect and adhesion improvement on polymer surfaces

NASA Astrophysics Data System (ADS)

Moser, E. M.; Gilliéron, D.; Henrion, G.

2010-01-01

The hydrophobic properties of polymeric surfaces may cause fogging in transparent packaging and poor adhesion to printing colours and coatings. Novel plasma processes for durable functionalization of polypropylene and polyethylene terephthalate substrates were developed and analysed using optical emission spectroscopy. A worm-like nano pattern was created on the polypropylene surface prior to the deposition of thin polar plasma polymerised layers. For both substrates, highly polar surfaces exhibiting a surface tension of up to 69 mN/m and a water contact angle of about 10° were produced - providing the anti-fogging effect. The deposition of thin plasma polymerised layers protects the increased surface areas and enables to tailoring the surface energy of the substrate in a wide range. Wetting characteristics were determined by dynamic contact angle measurements. Investigations of the chemical composition of several layers using X-ray photoelectron spectroscopy and FT-infrared spectroscopy were correlated with functional testing. The surface topography was investigated using atomic force microscopy. The weldability and peeling-off characteristics of the plasma treated polymer films could be adjusted by varying the process parameters. Global and specific migration analyses were undertaken in order to ensure the manufacturing of plasma treated polymer surfaces for direct food contact purposes.

Synthesis and electrochemical properties of polyaniline nanofibers by interfacial polymerization.

PubMed

Manuel, James; Ahn, Jou-Hyeon; Kim, Dul-Sun; Ahn, Hyo-Jun; Kim, Ki-Won; Kim, Jae-Kwang; Jacobsson, Per

2012-04-01

Polyaniline nanofibers were prepared by interfacial polymerization with different organic solvents such as chloroform and carbon tetrachloride. Field emission scanning electron microscopy and transmission electron microscopy were used to study the morphological properties of polyaniline nanofibers. Chemical characterization was carried out using Fourier transform infrared spectroscopy, UV-Vis spectroscopy, and X-ray diffraction spectroscopy and surface area was measured using BET isotherm. Polyaniline nanofibers doped with lithium hexafluorophosphate were prepared and their electrochemical properties were evaluated.

High surface area calcite

NASA Astrophysics Data System (ADS)

Schultz, L. N.; Andersson, M. P.; Dalby, K. N.; Müter, D.; Okhrimenko, D. V.; Fordsmand, H.; Stipp, S. L. S.

2013-05-01

Calcite (CaCO3) is important in many fields—in nature, because it is a component of aquifers, oil reservoirs and prospective CO2 storage sites, and in industry, where it is used in products as diverse as paper, toothpaste, paint, plastic and aspirin. It is difficult to obtain high purity calcite with a high surface area but such material is necessary for industrial applications and for fundamental calcite research. Commercial powder is nearly always contaminated with growth inhibitors such as sugars, citrate or pectin and most laboratory synthesis methods deliver large precipitates, often containing vaterite or aragonite. To address this problem, we (i) adapted the method of carbonating a Ca(OH)2 slurry with CO2 gas to develop the first simple, cheap, safe and reproducible procedure using common laboratory equipment, to obtain calcite that reproducibly had a surface area of 14-17 m2/g and (ii) conducted a thorough characterization of the product. Scanning electron microscopy (SEM) revealed nanometer scale, rhombohedral crystals. X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and infrared spectroscopy (IR) confirmed highly crystalline, pure calcite that more closely resembles the dimensions of the biogenic calcite produced by algae in coccoliths than other methods for synthesizing calcite. We suggest that this calcite is useful when purity and high surface area are important.

Non-activated high surface area expanded graphite oxide for supercapacitors

NASA Astrophysics Data System (ADS)

Vermisoglou, E. C.; Giannakopoulou, T.; Romanos, G. E.; Boukos, N.; Giannouri, M.; Lei, C.; Lekakou, C.; Trapalis, C.

2015-12-01

Microwave irradiation of graphite oxide constitutes a facile route toward production of reduced graphene oxide, since during this treatment both exfoliation and reduction of graphite oxide occurs. In this work, the effect of pristine graphite (type, size of flakes), pretreatment and oxidation cycles on the finally produced expanded material was examined. All the types of graphite that were tested afforded materials with high BET surface areas ranging from 940 m2/g to 2490 m2/g, without intervening an activation stage at elevated temperature. SEM and TEM images displayed exfoliated structures, where the flakes were significantly detached and curved. The quality of the reduced graphene oxide sheets was evidenced both by X-ray photoelectron spectroscopy and Raman spectroscopy. The electrode material capacitance was determined via electrochemical impedance spectroscopy and cyclic voltammetry. The materials with PEDOT binder had better performance (∼97 F/g) at low operation rates while those with PVDF binder performed better (∼20 F/g) at higher rates, opening up perspectives for their application in supercapacitors.

Activity of titania and zeolite samples dosed with triethylamine

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

Baker, Caitlin; Gole, James L.; Brauer, Jonathan

2016-01-01

Certain properties of titania and the ammonium- and proton-form of Y zeolites (silica/alumina ratio of 5.2) were explored before and after treatment by triethylamine (TEA). The effect of the triethylamine upon the physical and chemical properties of both titania and the zeolite were characterized by physical and chemical adsorption methods. BET surface area data showed enhanced surface area of the TEA-treated nanotitania over the untreated nanotitania whereas the TEA-treated zeolite showed a considerable decrease in surface area compared to the untreated zeolite. TPD of the TEA-treated Y zeolite showed that weakly adsorbed TEA left the surface between 150 and 300more » oC; strongly adsorbed TEA decomposed to ethylene and ammonia at higher temperatures. XPS, IR, and Raman spectroscopies, powder XRD, and 27Al MAS-NMR spectroscopy were used to further characterize the changes introduced by in-situ nitridation. Pre-adsorbed triethylamine decorated acid sites so as to neutralize these sites for the reaction of methanol to dimethylether. Carbon monoxide and ormaldehyde, products of the methanol probe reaction, were observed-- suggesting that basic sites are present in this treated zeolite and titania.« less

Nanoparticle Treated Stainless Steel Filters for Metal Vapor Sequestration

NASA Astrophysics Data System (ADS)

Murph, Simona E. Hunyadi; Larsen, George K.; Korinko, Paul; Coopersmith, Kaitlin J.; Summer, Ansley J.; Lewis, Rebecca

2017-02-01

The ability to sequester vapor phase radioactive compounds during industrial processes reduces the exposure of workers and the environment to dangerous radioactive materials. Nanomaterials have a lot of potential in this area because they typically demonstrate size- and shape-dependent properties with higher reactivity than bulk. This is due to the increased surface area-to-volume ratio and quantum size effects. In this report, we developed a gold nanomaterial-treated stainless steel filter, namely wools and coupons, that can be efficiently used for zinc vapor sequestration. Without nanoparticle modification, stainless steel coupons do not react or alloy with Zn. Gold nanomaterials were grown onto various stainless steel filters using solution chemistry that is amenable to scaling up. Materials were characterized by electron microscopy, inductively coupled plasma mass spectroscopy and dynamic light scattering before and after exposure to zinc vapors. X-ray diffraction, high-resolution transmission electron microscopy, energy dispersive x-ray spectroscopy mapping and ultraviolet-visible spectroscopy confirm the formation of gold-zinc alloys after Zn vapor exposure. The effect of surface topography on nanoparticle morphology, size and loading density were also investigated, and stainless steel surface defects were found to have an impact on the Au NP growth and subsequently Zn sequestration.

Multi-applicative tetragonal TiO2/SnO2 nanocomposites for photocatalysis and gas sensing

NASA Astrophysics Data System (ADS)

Patil, S. M.; Dhodamani, A. G.; Vanalakar, S. A.; Deshmukh, S. P.; Delekar, S. D.

2018-04-01

TiO2-based mixed metal oxide heteronanostructures have multiple applications in photocatalysis and gas sensing because of their charge transport properties. In this study, we prepared tetragonal TiO2/SnO2 nanocomposites (NCs) with different weight percentages using a simple wet impregnation method. The physicochemical properties of the NCs were investigated using X-ray diffraction, Fourier transform-infrared spectroscopy, ultraviolet-visible spectroscopy, field-emission scanning electron microscopy, energy dispersive X-ray spectroscopy, transmission electron microscopy, and Brunauer-Emmett-Teller surface area analysis. The results showed that the surface area of the NCs increased significantly and the anatase TiO2 was sensitized after the addition of a small amount of cassiterite SnO2 NPs. We systematically studied the as-prepared NCs during the photocatalytic degradation of Congo Red dye under visible light irradiation (λ > 420 nm) and NH3 gas sensing, which demonstrated the efficient photocatalytic performance and the superior sensing response of the catalyst with a weight composition of 25% SnO2 in TiO2 (4:1) compared with the other NCs or the bare individual nanoparticles. The improved photocatalytic and gas sensing performance of the TiO2/SnO2 (4:1) NCs may be attributed to the increased active surface area, the increased adsorption of the dye and target gas molecules, as well as efficient electron-hole charge separation and transfer.

Effects of Al(3+) doping on the structure and properties of goethite and its adsorption behavior towards phosphate.

PubMed

Li, Wei; Wang, Longjun; Liu, Fan; Liang, Xiaoliang; Feng, Xionghan; Tan, Wenfeng; Zheng, Lirong; Yin, Hui

2016-07-01

Al substitution in goethite is common in soils, and has strong influence on the structure and physicochemical properties of goethite. In this research, a series of Al-doped goethites were synthesized, and characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FT-IR) and extended X-ray absorption fine structure (EXAFS) spectroscopy. The adsorption behavior of these samples towards PO4(3-) was also investigated. Characterization results demonstrated that increasing Al content in goethite led to a reduction in crystallinity, increase in specific surface area (SSA), and morphology change from needle-like to granular. Rietveld structure refinement revealed that the lattice parameter a remained almost constant and b slightly decreased, but c was significantly reduced, and the calculated crystal density increased. EXAFS analysis demonstrated that the Fe(Al)-O distance in the structure of the doped goethites was almost the same, but the Fe-Fe(Al) distance decreased with increasing Al content. Surface analysis showed that, with increasing Al content, the content of OH groups on the mineral surface increased. The adsorption of phosphate per unit mass of Al-doped goethite increased, while adsorption per unit area decreased owing to the decrease of the relative proportion of (110) facets in the total surface area of the minerals. The results of this research facilitate better understanding of the effect of Al substitution on the structure and properties of goethite and the cycling of phosphate in the environment. Copyright © 2016. Published by Elsevier B.V.

Differentiation of dental restorative materials combining energy-dispersive X-ray fluorescence spectroscopy and post-mortem CT.

PubMed

Merriam, Tim; Kaufmann, Rolf; Ebert, Lars; Figi, Renato; Erni, Rolf; Pauer, Robin; Sieberth, Till

2018-06-01

Today, post-mortem computed tomography (CT) is routinely used for forensic identification. Mobile energy-dispersive X-ray fluorescence (EDXRF) spectroscopy of a dentition is a method of identification that has the potential to be easier and cheaper than CT, although it cannot be used with every dentition. In challenging cases, combining both techniques could facilitate the process of identification and prove to be advantageous over chemical analyses. Nine dental restorative material brands were analyzed using EDXRF spectroscopy. Their differentiability was assessed by comparing each material's x-ray fluorescence spectrum and then comparing the spectra to previous research investigating differentiability in CT. To verify EDXRF's precision and accuracy, select dental specimens underwent comparative electron beam excited x-ray spectroscopy (EDS) scans, while the impact of the restorative surface area was studied by scanning a row of dental specimens with varying restorative surface areas (n = 10). EDXRF was able to differentiate all 36 possible pairs of dental filling materials; however, dual-energy CT was only able to differentiate 33 out of 36. The EDS scans showed correlating x-ray fluorescence peaks on the x-ray spectra compared to our EDXRF. In addition, the surface area showed no influence on the differentiability of the dental filling materials. EDXRF has the potential to facilitate corpse identification by differentiating and comparing restorative materials, providing more information compared to post-mortem CT alone. Despite not being able to explicitly identify a brand without a control sample or database, its fast and mobile use could accelerate daily routines or mass victim identification processes. To achieve this goal, further development of EDXRF scanners for this application and further studies evaluating the method within a specific routine need to be performed.

Surface modification of layered perovskite Sr2TiO4 for improved CO2 photoreduction with H2O to CH4.

PubMed

Kwak, Byeong Sub; Do, Jeong Yeon; Park, No-Kuk; Kang, Misook

2017-11-27

Layered perovskite Sr 2 TiO 4 photocatalyst was synthesized by using sol-gel method with citric acid. In order to increase the surface area of layered perovskite Sr 2 TiO 4 , and thus to improve its photocatalytic activity for CO 2 reduction, its surface was modified via hydrogen treatment or exfoliation. The physical and chemical properties of the prepared catalysts were characterized by X-ray diffraction, high-resolution transmission electron microscopy, elemental mapping analysis, energy-dispersive X-ray spectroscopy, N 2 adsorption-desorption, UV-Vis spectroscopy, X-ray photoelectron spectroscopy, photoluminescence, and electrophoretic light scattering. CO 2 photoreduction was performed in a closed reactor under 6 W/cm 2 UV irradiation. The gaseous products were analyzed using a gas chromatograph equipped with flame ionization and thermal conductivity detectors. The exfoliated Sr 2 TiO 4 catalyst (E-Sr 2 TiO 4 ) exhibited a narrow band gap, a large surface area, and high dispersion. Owing to these advantageous properties, E-Sr 2 TiO 4 photocatalyst showed an excellent catalytic performance for CO 2 photoreduction reaction. The rate of CH 4 production from the photoreduction of CO 2 with H 2 O using E-Sr 2 TiO 4 was about 3431.77 μmol/g cat after 8 h.

Enhancement of surface area and wettability properties of boron doped diamond by femtosecond laser-induced periodic surface structuring

DOE PAGES

Granados, Eduardo; Calderon, Miguel Martinez; Krzywinski, Jacek; ...

2017-08-28

We demonstrate the formation of laser-induced periodic surface structures (LIPSS) in boron-doped diamond (BDD) by irradiation with femtosecond near-IR laser pulses. The results show that the obtained LIPSS are perpendicular to the laser polarization, and the ripple periodicity is on the order of half of the irradiation wavelength. The surface structures and their electrochemical properties were characterized using Raman micro-spectroscopy, in combination with scanning electron and atomic force microscopies. The textured BDD surface showed a dense and large surface area with no change in its structural characteristics. The effective surface area of the textured BDD electrode was approximately 50% largermore » than that of a planar substrate, while wetting tests showed that the irradiated area becomes highly hydrophilic. Lastly, our results indicate that LIPSS texturing of BDD is a straightforward and simple technique for enhancing the surface area and wettability properties of the BDD electrodes, which could enable higher current efficiency and lower energy consumption in the electrochemical oxidation of toxic organics.« less

Enhancement of surface area and wettability properties of boron doped diamond by femtosecond laser-induced periodic surface structuring

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

Granados, Eduardo; Calderon, Miguel Martinez; Krzywinski, Jacek

We demonstrate the formation of laser-induced periodic surface structures (LIPSS) in boron-doped diamond (BDD) by irradiation with femtosecond near-IR laser pulses. The results show that the obtained LIPSS are perpendicular to the laser polarization, and the ripple periodicity is on the order of half of the irradiation wavelength. The surface structures and their electrochemical properties were characterized using Raman micro-spectroscopy, in combination with scanning electron and atomic force microscopies. The textured BDD surface showed a dense and large surface area with no change in its structural characteristics. The effective surface area of the textured BDD electrode was approximately 50% largermore » than that of a planar substrate, while wetting tests showed that the irradiated area becomes highly hydrophilic. Lastly, our results indicate that LIPSS texturing of BDD is a straightforward and simple technique for enhancing the surface area and wettability properties of the BDD electrodes, which could enable higher current efficiency and lower energy consumption in the electrochemical oxidation of toxic organics.« less

Emerging technology: applications of Raman spectroscopy for prostate cancer.

PubMed

Kast, Rachel E; Tucker, Stephanie C; Killian, Kevin; Trexler, Micaela; Honn, Kenneth V; Auner, Gregory W

2014-09-01

There is a need in prostate cancer diagnostics and research for a label-free imaging methodology that is nondestructive, rapid, objective, and uninfluenced by water. Raman spectroscopy provides a molecular signature, which can be scaled from micron-level regions of interest in cells to macroscopic areas of tissue. It can be used for applications ranging from in vivo or in vitro diagnostics to basic science laboratory testing. This work describes the fundamentals of Raman spectroscopy and complementary techniques including surface enhanced Raman scattering, resonance Raman spectroscopy, coherent anti-Stokes Raman spectroscopy, confocal Raman spectroscopy, stimulated Raman scattering, and spatially offset Raman spectroscopy. Clinical applications of Raman spectroscopy to prostate cancer will be discussed, including screening, biopsy, margin assessment, and monitoring of treatment efficacy. Laboratory applications including cell identification, culture monitoring, therapeutics development, and live imaging of cellular processes are discussed. Potential future avenues of research are described, with emphasis on multiplexing Raman spectroscopy with other modalities.

Development of large-surface Nafion-metal composite actuator and its electrochemical characterization

NASA Astrophysics Data System (ADS)

Noh, Taegeun; Tak, Yong Suk; Nam, Jaedo; Jeon, Jaewook; Kim, Hunmo; Choi, Hyoukryeol; Bae, Sang Sik

2001-07-01

Behaviors of nafion-based actuators are significantly affected by interfacial area between electrode and polymer electrolyte. Replication method was utilized to manufacture a large surface-area composite actuator. Etched aluminum foil was used as a template for replication using liquid nafion solution. Measurement of double layer charging and scanning electron microscopy indicated that interfacial area was greatly increased by replication method. Higher surface area induced a better bending performance of ionic polymer metal composite (IPMC). In parallel, the effect of cations on IPMC was interpreted with constant current experiment, linear sweep voltammetry and electrochemical impedance spectroscopy. For univalent cations, ion size is the most influencing parameter on ionic mobility inside membrane. However, ion-ion interaction affects an ionic mobility for divalent cations.

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

Perras, Frederic A.; Wang, Lin-Lin; Manzano, J. Sebastian

The efficacy of dynamic nuclear polarization (DNP) surface-enhanced NMR spectroscopy (SENS) is reviewed for alumina, silica, and ordered mesoporous carbon (OMC) materials, with vastly different surface areas, as a function of the biradical concentration. Importantly, our studies show that the use of a “one-size-fits-all” biradical concentration should be avoided when performing DNP SENS experiments and instead an optimal concentration should be selected as appropriate for the type of material studied as well as its surface area. In general, materials with greater surface areas require higher radical concentrations for best possible DNP performance. This result is explained with the use ofmore » a thermodynamic model wherein radical-surface interactions are expected to lead to an increase in the local concentration of the polarizing agent at the surface. We also show, using plane-wave density functional theory calculations, that weak radical-surface interactions are the cause of the poor performance of DNP SENS for carbonaceous materials.« less

Evolution of porous structure and texture in nanoporous SiO2/Al2O3 materials during calcination

NASA Astrophysics Data System (ADS)

Glazkova, Elena A.; Bakina, Olga V.

2016-11-01

The study focuses on the evolution of porous structure and texture of silica/alumina xerogels during calcination in the temperature range from 500 to 1200°C. The xerogel was prepared via sol-gel method using subcritical drying. The silica/alumina xerogels were examined using transmission electron microscopy-energy dispersive spectroscopy (TEM-EDS), Brunauer Emmett Teller-Barrett Joyner Halenda (BET-BJH), differential scanning calorimetry (DSC), and Fourier transform infrared (FTIR) spectroscopy. SiO2 primary particles of size about 10 nm are connected with each other to form a porous xerogel structure. Alumina is uniformly distributed over the xerogel volume. The changes of textural characteristics under heat treatment of samples are radical; the specific surface area and pore size attain their maximum at 500-700°C. The heat treatment of samples causes dehydroxylation of the xerogel surface, and at 1200°C the sample is sintered, loses mesoporosity, and its specific surface area reduces considerably down to 78 m2/g.

Synthesis of porous nanocrystalline NiO with hexagonal sheet-like morphology by homogeneous precipitation method

NASA Astrophysics Data System (ADS)

Sharma, Ravi Kant; Ghose, Ranjana

2015-04-01

Porous nanocrystalline NiO has been synthesized by a simple homogeneous precipitation method in short time at low calcination temperature without using any surfactant, chelating or gelating agents. The porous nanocrystalline NiO with a hexagonal sheet-like morphology were obtained by calcination of Ni(OH)2 nanoflakes at 500 °C. The calcination temperature strongly influences the morphology, crystallite size, specific surface area, pore volume and optical band gap of the samples. The samples were characterized using powder X-ray diffraction, thermal gravimetric analysis, FT-IR spectroscopy, UV-Visible diffuse reflectance spectroscopy, surface area measurements, field emission scanning electron microscopy coupled with energy dispersive X-ray analysis and transmission electron microscopy. The chemical activity of the samples was tested by catalytic reduction of 4-nitrophenol with NaBH4.

Infrared photothermal imaging spectroscopy for detection of trace explosives on surfaces.

PubMed

Kendziora, Christopher A; Furstenberg, Robert; Papantonakis, Michael; Nguyen, Viet; Byers, Jeff; Andrew McGill, R

2015-11-01

We are developing a technique for the standoff detection of trace explosives on relevant substrate surfaces using photothermal infrared (IR) imaging spectroscopy (PT-IRIS). This approach leverages one or more compact IR quantum cascade lasers, which are tuned to strong absorption bands in the analytes and directed to illuminate an area on a surface of interest. An IR focal plane array is used to image the surface and detect increases in thermal emission upon laser illumination. The PT-IRIS signal is processed as a hyperspectral image cube comprised of spatial, spectral, and temporal dimensions as vectors within a detection algorithm. The ability to detect trace analytes at standoff on relevant substrates is critical for security applications but is complicated by the optical and thermal analyte/substrate interactions. This manuscript describes a series of PT-IRIS experimental results and analysis for traces of RDX, TNT, ammonium nitrate, and sucrose on steel, polyethylene, glass, and painted steel panels. We demonstrate detection at surface mass loadings comparable with fingerprint depositions ( 10μg/cm2 to 100μg/cm2) from an area corresponding to a single pixel within the thermal image.

Characterization of organo-modified bentonite sorbents: The effect of modification conditions on adsorption performance

NASA Astrophysics Data System (ADS)

Parolo, María E.; Pettinari, Gisela R.; Musso, Telma B.; Sánchez-Izquierdo, María P.; Fernández, Laura G.

2014-11-01

The organic modification of a natural bentonite was evaluated using two methods: exchanging the interlayer cations by hexadecyltrimethylammonium (HDTMA) and grafting with vinyltrimethoxysilane (VTMS) and γ-methacryloyloxy propyl trimethoxysilane (TMSPMA) on montmorillonite surface. The physicochemical characterization of all materials was made by X-ray diffraction (XRD), IR spectroscopy, thermogravimetric analysis (TGA) and Brunauer-Emmett-Teller (BET) surface area techniques. HDTMA cations and organosilanes were intercalated into the interlayer space of montmorillonite, as deduced from the increase of the basal spacing. IR spectroscopy, TGA and BET area give evidence of successful organic modification. The studies show a decrease in the IR absorption band intensity at 3465 cm-1 with surfactant modification, and also a decrease of mass loss due to adsorbed water observed in two samples: the organoclay and functionalized bentonites, which are evidences of a lower interlayer hydrophilicity. The efficiency of aniline removal onto natural bentonite, organobentonite and functionalized bentonites from aqueous solutions was evaluated. Aniline sorption on natural bentonite was studied using batch experiments, XRD and IR spectroscopy. The hydrophobic surface of organobentonite and functionalized bentonites increased the retention capacity for nonionic organic substances such as aniline on bentonites. The sorption properties of modified bentonite, through different modification methods, enhanced the potential industrial applications of bentonites in water decontamination.

Nanoparticle treated stainless steel filters for metal vapor sequestration

DOE PAGES

Murph, Simona E. Hunyadi; Larsen, George K.; Korinko, Paul; ...

2016-12-07

The ability to sequester vapor phase radioactive compounds during industrial processes reduces the exposure of workers and the environment to dangerous radioactive materials. Nanomaterials have a lot of potential in this area because they typically demonstrate size- and shape-dependent properties with higher reactivity than bulk. This is due to the increased surface area-to-volume ratio and quantum size effects. In this report, we developed a gold nanomaterial-treated stainless steel filter, namely wools and coupons, that can be efficiently used for zinc vapor sequestration. Without nanoparticle modification, stainless steel coupons do not react or alloy with Zn. Gold nanomaterials were grown ontomore » various stainless steel filters using solution chemistry that is amenable to scaling up. Materials were characterized by electron microscopy, inductively coupled plasma mass spectroscopy and dynamic light scattering before and after exposure to zinc vapors. X-ray diffraction, high-resolution transmission electron microscopy, energy dispersive x-ray spectroscopy mapping and ultraviolet-visible spectroscopy confirm the formation of gold-zinc alloys after Zn vapor exposure. Furthermore, the effect of surface topography on nanoparticle morphology, size and loading density were also investigated, and stainless steel surface defects were found to have an impact on the Au NP growth and subsequently Zn sequestration.« less

Nanoparticle treated stainless steel filters for metal vapor sequestration

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

Murph, Simona E. Hunyadi; Larsen, George K.; Korinko, Paul

The ability to sequester vapor phase radioactive compounds during industrial processes reduces the exposure of workers and the environment to dangerous radioactive materials. Nanomaterials have a lot of potential in this area because they typically demonstrate size- and shape-dependent properties with higher reactivity than bulk. This is due to the increased surface area-to-volume ratio and quantum size effects. In this report, we developed a gold nanomaterial-treated stainless steel filter, namely wools and coupons, that can be efficiently used for zinc vapor sequestration. Without nanoparticle modification, stainless steel coupons do not react or alloy with Zn. Gold nanomaterials were grown ontomore » various stainless steel filters using solution chemistry that is amenable to scaling up. Materials were characterized by electron microscopy, inductively coupled plasma mass spectroscopy and dynamic light scattering before and after exposure to zinc vapors. X-ray diffraction, high-resolution transmission electron microscopy, energy dispersive x-ray spectroscopy mapping and ultraviolet-visible spectroscopy confirm the formation of gold-zinc alloys after Zn vapor exposure. Furthermore, the effect of surface topography on nanoparticle morphology, size and loading density were also investigated, and stainless steel surface defects were found to have an impact on the Au NP growth and subsequently Zn sequestration.« less

Evaluation of light detector surface area for functional Near Infrared Spectroscopy.

PubMed

Wang, Lei; Ayaz, Hasan; Izzetoglu, Meltem; Onaral, Banu

2017-10-01

Functional Near Infrared Spectroscopy (fNIRS) is an emerging neuroimaging technique that utilizes near infrared light to detect cortical concentration changes of oxy-hemoglobin and deoxy-hemoglobin non-invasively. Using light sources and detectors over the scalp, multi-wavelength light intensities are recorded as time series and converted to concentration changes of hemoglobin via modified Beer-Lambert law. Here, we describe a potential source for systematic error in the calculation of hemoglobin changes and light intensity measurements. Previous system characterization and analysis studies looked into various fNIRS parameters such as type of light source, number and selection of wavelengths, distance between light source and detector. In this study, we have analyzed the contribution of light detector surface area to the overall outcome. Results from Monte Carlo based digital phantoms indicated that selection of detector area is a critical system parameter in minimizing the error in concentration calculations. The findings here can guide the design of future fNIRS sensors. Copyright © 2017 Elsevier Ltd. All rights reserved.

Combining total internal reflection sum frequency spectroscopy spectral imaging and confocal fluorescence microscopy.

PubMed

Allgeyer, Edward S; Sterling, Sarah M; Gunewardene, Mudalige S; Hess, Samuel T; Neivandt, David J; Mason, Michael D

2015-01-27

Understanding surface and interfacial lateral organization in material and biological systems is critical in nearly every field of science. The continued development of tools and techniques viable for elucidation of interfacial and surface information is therefore necessary to address new questions and further current investigations. Sum frequency spectroscopy (SFS) is a label-free, nonlinear optical technique with inherent surface specificity that can yield critical organizational information on interfacial species. Unfortunately, SFS provides no spatial information on a surface; small scale heterogeneities that may exist are averaged over the large areas typically probed. Over the past decade, this has begun to be addressed with the advent of SFS microscopy. Here we detail the construction and function of a total internal reflection (TIR) SFS spectral and confocal fluorescence imaging microscope directly amenable to surface investigations. This instrument combines, for the first time, sample scanning TIR-SFS imaging with confocal fluorescence microscopy.

The origin of high electrolyte-electrode interfacial resistances in lithium cells containing garnet type solid electrolytes.

PubMed

Cheng, Lei; Crumlin, Ethan J; Chen, Wei; Qiao, Ruimin; Hou, Huaming; Franz Lux, Simon; Zorba, Vassilia; Russo, Richard; Kostecki, Robert; Liu, Zhi; Persson, Kristin; Yang, Wanli; Cabana, Jordi; Richardson, Thomas; Chen, Guoying; Doeff, Marca

2014-09-14

Dense LLZO (Al-substituted Li7La3Zr2O12) pellets were processed in controlled atmospheres to investigate the relationships between the surface chemistry and interfacial behavior in lithium cells. Laser induced breakdown spectroscopy (LIBS), scanning electron microscopy (SEM), X-ray diffraction (XRD), Raman spectroscopy, synchrotron X-ray photoelectron spectroscopy (XPS) and soft X-ray absorption spectroscopy (XAS) studies revealed that Li2CO3 was formed on the surface when LLZO pellets were exposed to air. The distribution and thickness of the Li2CO3 layer were estimated by a combination of bulk and surface sensitive techniques with various probing depths. First-principles thermodynamic calculations confirmed that LLZO has an energetic preference to form Li2CO3 in air. Exposure to air and the subsequent formation of Li2CO3 at the LLZO surface is the source of the high interfacial impedances observed in cells with lithium electrodes. Surface polishing can effectively remove Li2CO3 and dramatically improve the interfacial properties. Polished samples in lithium cells had an area specific resistance (ASR) of only 109 Ω cm(2) for the LLZO/Li interface, the lowest reported value for Al-substituted LLZO. Galvanostatic cycling results obtained from lithium symmetrical cells also suggest that the quality of the LLZO/lithium interface has a significant impact on the device lifetime.

Revealing Anisotropic Spinel Formation on Pristine Li- and Mn-Rich Layered Oxide Surface and Its Impact on Cathode Performance

DOE PAGES

Kuppan, Saravanan; Shukla, Alpesh Khushalchand; Membreno, Daniel; ...

2017-01-06

Surface properties of cathode particles play important roles in the transport of ions and electrons and they may ultimately dominate cathode's performance and stability in lithium-ion batteries. Through the use of carefully prepared Li 1.2Ni 0.13Mn 0.54Co 0.13O 2 crystal samples with six distinct morphologies, surface transition-metal redox activities and crystal structural transformation are investigated as a function of surface area and surface crystalline orientation. Complementary depth-profiled core-level spectroscopy, namely, X-ray absorption spectroscopy, electron energy loss spectroscopy, and atomic-resolution scanning transmission electron microscopy, are applied in the study, presenting a fine example of combining advanced diagnostic techniques with a well-definedmore » model system of battery materials. Here, we report the following findings: (1) a thin layer of defective spinel with reduced transition metals, similar to what is reported on cycled conventional secondary particles in the literature, is found on pristine oxide surface even before cycling, and (2) surface crystal structure and chemical composition of both pristine and cycled particles are facet dependent. Oxide structural and cycling stabilities improve with maximum expression of surface facets stable against transition-metal reduction. Finally, the intricate relationships among morphology, surface reactivity and structural transformation, electrochemical performance, and stability of the cathode materials are revealed.« less

Investigation of surface properties of pristine and γ-irradiated PAN-based carbon fibers: Effects of fiber instinct structure and radiation medium

NASA Astrophysics Data System (ADS)

Liu, Liangsen; Wu, Fan; Yao, Hongwei; Shi, Jie; Chen, Lei; Xu, Zhiwei; Deng, Hui

2015-05-01

The different rules for γ-ray modifications of carbon fiber (CF) surface were found in previous literature, and the contributing factors were not clear. To investigate the effects of fiber instinct structure and radiation medium on surface modification of CFs in γ-ray irradiation, argon atmosphere (Ar) and epoxy chloropropane (ECP) were chosen as the irradiation media for T300, T400, T700, T800 and T1000, respectively. Based on the Raman spectroscopy and specific surface area results, changes of surface graphitization and roughness depended on the fiber instinct structure after irradiation. The graphitization of T300, T400 and T800 with low graphitization and rough surface was increased after irradiation, while that of T700 and T1000 with high graphite degree and smooth surface was decreased. Specific surface areas of low-graphitization CFs (T300, T400 and T800) were changed clearly, while those of high-graphitization CFs (T700 and T1000) remained almost unchanged after irradiation. X-ray photoelectron spectroscopy provided the evidence that the surface chemistry change after irradiation was determined by the type of the irradiation medium. The oxygen ratio of CFs irradiated in Ar was decreased while that of CFs irradiated in ECP was increased with Cl element detected. Surface free energy of all CFs was improved obviously after irradiation, and CFs irradiated in ECP had higher surface free energy compared with CFs irradiated in Ar.

Investigation on single walled carbon nanotube thin films deposited by Langmuir Blodgett method

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

Vishalli,, E-mail: vishalli-2008@yahoo.com; Dharamvir, Keya; Kaur, Ramneek

2015-05-15

Langmuir Blodgett is a technique to deposit a homogeneous film with a fine control over thickness and molecular organization. Thin films of functionalized SWCNTs have been prepared by Langmuir Blodgett method. The good surface spreading properties of SWCNTs at air/water interface are indicated by surface pressure-area isotherm and the monolayer formed on water surface is transferred onto the quartz substrate by vertical dipping. A multilayer film is thus obtained in a layer by layer manner. The film is characterized by Atomic Force Microscope (AFM), UV-Vis-NIR spectroscopy and FTIR.AFM shows the surface morphology of the deposited film. UV-Vis-NIR spectroscopy shows themore » characteristic peaks of semiconducting SWCNTs. The uniformity of LB film can be used further in understanding the optical and electrical behavior of these materials.« less

Electrochemical Hydrogen Evolution at Ordered Mo 7 Ni 7

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

Csernica, Peter M.; McKone, James R.; Mulzer, Catherine R.

2017-04-11

Ni–Mo alloys containing up to ~15 mol % Mo are excellent non-noble electrocatalysts for the hydrogen evolution reaction (HER) in alkaline aqueous electrolytes. To date, studies have not addressed the details of HER activity of ordered Ni–Mo intermetallic compounds, which can contain a significantly larger fraction of Mo (up to 50 mol %) than can be accessed through high-temperature alloying. Here, we present a straightforward and facile synthesis of three phase-pure electrocatalyst powders using a precipitation–reduction approach: ordered Mo7Ni7, disordered Ni0.92Mo0.08, and pure Ni. The Ni0.92Mo0.08 alloy exhibited a nearly 10-fold higher mass-specific HER activity than either pure Ni ormore » Mo7Ni7, where much of the difference could be attributed to relative surface area. Therefore, we attempted to quantify and account for differences in surface areas using electron microscopy, impedance spectroscopy, and gas adsorption measurements. These data suggest that Ni–Mo alloys and intermetallic compounds exhibit substantial pseudocapacitance at potentials near the onset of hydrogen evolution, which can cause impedance spectroscopy to overestimate the interfacial capacitance, and thus the electrochemically active surface area, of these materials. From these observations, we postulate Mo redox activity as the chemical basis for the observed pseudocapacitance of Ni–Mo composites. Furthermore, using gas adsorption measurements, rather than capacitance, to estimate active surface area, we find that ordered Mo7Ni7 is more intrinsically active than the Ni0.92Mo0.08 alloy, implying that Mo7Ni7 intermetallics with high surface area will also give higher mass-specific activities than alloys with comparable roughness.« less

Optimal sample formulations for DNP SENS: The importance of radical-surface interactions

DOE PAGES

Perras, Frederic A.; Wang, Lin-Lin; Manzano, J. Sebastian; ...

2017-11-15

The efficacy of dynamic nuclear polarization (DNP) surface-enhanced NMR spectroscopy (SENS) is reviewed for alumina, silica, and ordered mesoporous carbon (OMC) materials, with vastly different surface areas, as a function of the biradical concentration. Importantly, our studies show that the use of a “one-size-fits-all” biradical concentration should be avoided when performing DNP SENS experiments and instead an optimal concentration should be selected as appropriate for the type of material studied as well as its surface area. In general, materials with greater surface areas require higher radical concentrations for best possible DNP performance. This result is explained with the use ofmore » a thermodynamic model wherein radical-surface interactions are expected to lead to an increase in the local concentration of the polarizing agent at the surface. We also show, using plane-wave density functional theory calculations, that weak radical-surface interactions are the cause of the poor performance of DNP SENS for carbonaceous materials.« less

Field spectroscopy sampling strategies for improved measurement of Earth surface reflectance

NASA Astrophysics Data System (ADS)

Mac Arthur, A.; Alonso, L.; Malthus, T. J.; Moreno, J. F.

2013-12-01

Over the last two decades extensive networks of research sites have been established to measure the flux of carbon compounds and water vapour between the Earth's surface and the atmosphere using eddy covariance (EC) techniques. However, contributing Earth surface components cannot be determined and (as the ';footprints' are spatially constrained) these measurements cannot be extrapolated to regional cover using this technique. At many of these EC sites researchers have been integrating spectral measurements with EC and ancillary data to better understand light use efficiency and carbon dioxide flux. These spectroscopic measurements could also be used to assess contributing components and provide support for imaging spectroscopy, from airborne or satellite platforms, which can provide unconstrained spatial cover. Furthermore, there is an increasing interest in ';smart' database and information retrieval systems such as that proposed by EcoSIS and OPTIMISE to store, analyse, QA and merge spectral and biophysical measurements and provide information to end users. However, as Earth surfaces are spectrally heterogeneous and imaging and field spectrometers sample different spatial extents appropriate field sampling strategies require to be adopted. To sample Earth surfaces spectroscopists adopt either single; random; regular grid; transect; or 'swiping' point sampling strategies, although little comparative work has been carried out to determine the most appropriate approach; the work by Goetz (2012) is a limited exception. Mac Arthur et al (2012) demonstrated that, for two full wavelength (400 nm to 2,500 nm) field spectroradiometers, the measurement area sampled is defined by each spectroradiometer/fore optic system's directional response function (DRF) rather than the field-of-view (FOV) specified by instrument manufacturers. Mac Arthur et al (2012) also demonstrated that each reflecting element within the sampled area was not weighted equally in the integrated measurement recorded. There were non-uniformities of spectral response with the spectral ';weighting' per wavelength interval being positionally dependent and unique to each spectroradiometer/fore optic system investigated. However, Mac Arthur et al (2012) did not provide any advice on how to compensate for these systematic errors or advise on appropriate sampling strategies. The work reported here will provide the first systematic study of the effect of field spectroscopy sampling strategies for a range of different Earth surface types. Synthetic Earth surface hyperspectral data cubes for each surface type were generated and convolved with a range of the spectrometer/fore optic system directional response functions generated by Mac Arthur et al 2013, to simulate spectroscopic measurements of Earth surfaces. This has enabled different field sampling strategies to be directly compared and their suitability for each measurement purpose and surface type to be assessed and robust field spectroscopy sampling strategy recommendations to be made. This will be particularly of interest to the carbon and water vapour flux communities and assist the development of sampling strategies for field spectroscopy from rotary-wing Unmanned Aerial Vehicles, which will aid acquiring measurements in the spatial domain, and generally further the use of field spectroscopy for quantitative Earth observation.

Foreword: The 12th International Conference on Vibrations at Surfaces (VAS 12) (Erice, 20 26 July 2007)

NASA Astrophysics Data System (ADS)

Benedek, Giorgio; Vattuone, Luca

2008-06-01

The 12th International Conference on Vibrations at Surfaces (VAS 12) took place from 20 26 July 2007 as an event of the International School of Solid State Physics at the Ettore Majorana Foundation and Centre for Scientific Culture, Erice (Italy). The format and special environment of the conference have contributed to its transition from a traditional, medium-size conference into a more effective workshop, with a series of lectures reporting the most recent developments in the field, two poster sessions presenting recent results and even works in progress being discussed. The papers collected in this issue cover the highlights of the conference very thoroughly. Quite a few novel aspects concerning vibrations at surfaces are represented here, for example: new aspects in surface phonon spectroscopy, such as the very recent progress in inelastic x-ray scattering, the first observation of the boson peak in disordered surfaces, progress in the theory of atom scattering inelastic resonances, the action spectroscopy, the study of polycrystalline surfaces with electron energy-loss spectroscopy etc; parallel developments in experimental vibrational studies of adsorbed phases, either inorganic or organic, with those in ab initio theoretical simulations; the theory of enhanced electron--phonon interaction in low dimensions (2D and 1D); the extension from the traditional realm of surface vibrations and spectroscopy to other aspects of surface dynamics, like friction and various nonlinear effects, and to relevant dynamical phenomena occurring at interfaces. Other novelties presented at the conference, but already published in recent issues of the Journal of Physics: Condensed Matter, are also worth mentioning: the spin-echo spectroscopy with 3He allowing for slow-dynamics spectroscopy at very high, unprecedented resolutions (2007 J. Phys.: Cond. Matter 19 300301 and 305010; the first demonstration of dissociative surface trapping of molecules (2007 J. Phys.: Cond. Matter 19 305003; the discovery of optical surface phonons in metals, solving a quarter of a century old controversy about surface acoustic resonances (2007 J. Phys.: Cond. Matter 19 305011). Future development of the VAS conference series could involve extending it to new areas directly involving surface vibrations which have traditionally been covered by other scientific communities. These are nonlinear optics (second-harmonic generation, femtosecond pump and probe experiments), surface acoustic waves (SAW) in THz domains with extension to dispersion effects and optical phonons, THz SAW applications to sensors and other devices, etc. The mature field of surface vibrations has many new branches into a wide range of applicative, mostly nanotechnological areas. The present VAS edition was intended to renew the conference and stimulate its evolution into new challenging directions. We believe that this special issue of the Journal of Physics: Condensed Matter will meet with the same large consensus gained at the 12th International Conference on Vibrations at Surfaces, and will foster new progress in the fields of surface dynamical phenomena and their applications. The next International Conference on Vibrations at Surfaces (VAS 13) will take place in the fall of 2009 in Orlando, Florida, and will be chaired by Professor Talat S Rahman, University of Central Florida. We gratefully acknowledge the Ettore Majorana Foundation and Centre for Scientific Culture, Erice (Italy) and its staff for excellent hospitality and support, and SPECS and Varian for financial aid.

Determination of specific capacitance of modified candlenut shell based carbon as electrode material for supercapacitor

NASA Astrophysics Data System (ADS)

Zakir, M.; Budi, P.; Raya, I.; Karim, A.; Wulandari, R.; Sobrido, A. B. J.

2018-03-01

Surface modification of candlenut shell carbon (CSC) using three chemicals: nitric acid (HNO3), hydrogen peroxide (H2O2), and sulfuric acid (H2SO4) has been carried out. Activation of CSC was performed using H3PO4 solution with different ratio between CSC and activator. Carbon surface area was determined by methylene blue adsorption method. Surface characterization was performed using FTIR spectroscopy and Boehm titration method. Specific capacitance of electrode prepared from CSAC (candlenuts shell activated carbon) materials was quantified by Cyclic Voltammetry (CV) measurement. The surface area before and after activation are 105,127 m2/g, 112,488 m2/g, 124,190 m2/g, and 135,167 m2/g, respectively. Surface modification of CSAC showed the improvement in the chemical functionality of CSAC surface. Analyses using FTIR spectroscopy and Boehm titration showed that modifications with HNO3, H2SO4 and H2O2 on the surface of the CSAC increased the number of oxygen functional groups. As a consequence, the specific capacitance of CSAC modified with 65% HNO3 attained the highest value (127 μF/g). There is an incredible increase by a factor of 298% from electrode which was constructed with un-modified CSAC material. This increase correlates to the largest number of oxygen functional groups of CSAC modified with nitric acid (HNO3).

Correlating Humidity-Dependent Ionically Conductive Surface Area with Transport Phenomena in Proton-Exchange Membranes

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

He, Qinggang; Kusoglu, Ahmet; Lucas, Ivan T.

2011-08-01

The objective of this effort was to correlate the local surface ionic conductance of a Nafion? 212 proton-exchange membrane with its bulk and interfacial transport properties as a function of water content. Both macroscopic and microscopic proton conductivities were investigated at different relative humidity levels, using electrochemical impedance spectroscopy and current-sensing atomic force microscopy (CSAFM). We were able to identify small ion-conducting domains that grew with humidity at the surface of the membrane. Numerical analysis of the surface ionic conductance images recorded at various relative humidity levels helped determine the fractional area of ion-conducting active sites. A simple square-root relationshipmore » between the fractional conducting area and observed interfacial mass-transport resistance was established. Furthermore, the relationship between the bulk ionic conductivity and surface ionic conductance pattern of the Nafion? membrane was examined.« less

Surface and Bulk Phase Separations in Block Copolymers and Their Blends.

DTIC Science & Technology

1984-03-01

research effort in _. the biomedical area to study polymeric surfaces which may be applied where biocompatibility (particularly, blood compatibilty) is...elasticity(thermoplastic) and good biocompatibility . Two such commercially available polyurethanes-, Avcothane and Biomer, have been used in this...the biocompatible properties depended considerably on the rate of evaporation of solvent during the film preparation. ATR-IR spectroscopy showed that

BSA adsorption onto nanospheres: Influence of surface curvature as probed by electrophoretic light scattering and UV/vis spectroscopy

NASA Astrophysics Data System (ADS)

Sánchez-Pérez, Julio A.; Gallardo-Moreno, Amparo M.; González-Martín, M. Luisa; Vadillo-Rodríguez, Virginia

2015-10-01

The influence of surface curvature on the adsorption of bovine serum albumin (BSA) was evaluated through the combination of two fairly simple techniques: electrophoretic light scattering and UV/vis spectroscopy. Measurements were carried out for a range of protein concentrations (0-320 μg/ml) at pH 3.5, 4.5 and 7 using hydrophobic polystyrene nanospheres of 38.8, 82 and 220 nm in diameter. The results obtained demonstrate that the charge of the BSA molecules in solution dictates the pH-dependent behavior of the protein-coated nanospheres, indicating in all cases a significant adsorption of BSA molecules. At a fixed pH, however, it is the zeta potential that characterizes the uncoated nanospheres normalized by their surface area that primarily controls protein adsorption. In particular, it is found that the rate at which BSA interact with the different nanospheres increases as their negative zeta potential per unit area (or diameter) increases (decreases) regardless of the pH. Moreover, provided that adsorption occurs away from the isoelectric point of the protein, highly curved surfaces are found to stabilize the native-like conformation of BSA upon adsorption by likely reducing lateral interactions between adsorbed molecules.

Laser writing of single-crystalline gold substrates for surface enhanced Raman spectroscopy

NASA Astrophysics Data System (ADS)

Singh, Astha; Sharma, Geeta; Ranjan, Neeraj; Mittholiya, Kshitij; Bhatnagar, Anuj; Singh, B. P.; Mathur, Deepak; Vasa, Parinda

2017-07-01

Surface enhanced Raman scattering (SERS) spectroscopy, a powerful contemporary tool for studying low-concentration analytes via surface plasmon induced enhancement of local electric field, is of utility in biochemistry, material science, threat detection, and environmental studies. We have developed a simple, fast, scalable, and relatively low-cost optical method of fabricating and characterizing large-area, reusable and broadband SERS substrates with long storage lifetime. We use tightly focused, intense infra-red laser pulses to write gratings on single-crystalline, Au (1 1 1) gold films on mica which act as SERS substrates. Our single-crystalline SERS substrates compare favourably, in terms of surface quality and roughness, to those fabricated in poly-crystalline Au films. Tests show that our SERS substrates have the potential of detecting urea and 1,10-phenantroline adulterants in milk and water, respectively, at 0.01 ppm (or lower) concentrations.

Chiral surface waves for enhanced circular dichroism

NASA Astrophysics Data System (ADS)

Pellegrini, Giovanni; Finazzi, Marco; Celebrano, Michele; Duò, Lamberto; Biagioni, Paolo

2017-06-01

We present a novel chiral sensing platform that combines a one-dimensional photonic crystal design with a birefringent surface defect. The platform sustains simultaneous transverse electric and transverse magnetic surface modes, which are exploited to generate chiral surface waves. The present design provides homogeneous and superchiral fields of both handednesses over arbitrarily large areas in a wide spectral range, resulting in the enhancement of the circular dichroism signal by more than two orders of magnitude, thus paving the road toward the successful combination of surface-enhanced spectroscopies and electromagnetic superchirality.

Synthesis of rose-like boron nitride particles with a high specific surface area

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

Yu, Hongming; Huang, Xiaoxiao; Wen, Guangwu, E-mail: wgw@hitwh.edu.cn

2010-08-15

Novel rose-like BN nanostructures were synthesized on a large scale via a two-step procedure. The products were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, X-ray photoelectron spectrometer and nitrogen porosimetry. The results show that the obtained rose-like nanostructures are composed of a large amount of h-BN crystalline flakes and have a surface area of 90.31 m{sup 2}/g. A mechanism was proposed to explain the formation process of the rose-like BN nanostructures.

Synthesis and characterization of TiO2/graphitic carbon nanocomposites with enhanced photocatalytic performance

NASA Astrophysics Data System (ADS)

Wanag, Agnieszka; Kusiak-Nejman, Ewelina; Kowalczyk, Łukasz; Kapica-Kozar, Joanna; Ohtani, Bunsho; Morawski, Antoni W.

2018-04-01

In this paper titanium dioxide carbon modification with benzene as a carbon source is presented. A TiO2/graphitic carbon nanocomposites were synthesized by thermal modification in the presence of benzene vapours at different temperature (300-700 °C). The new materials were characterized by a various techniques, such as: X-ray diffraction (XRD), scanning electron microscopy (SEM), diffuse reflectance spectroscopy (UV-vis/DR), surface-enhanced Raman spectroscopy. BET specific surface area was also measured. The photocatalytic activity of obtained nanocomposites was measured by the decomposition of acetic acid and methylene blue under UV-vis irradiation. The results show that photocatalytic activity increasing with increase in carbon concentration and temperature of modification. It can be noted that adsorption degree has a very high impact on methylene blue decomposition. The highest photocatalytic activity was found for the photocatalyst modified at 600 °C contains 1.13 wt% of carbon. It should be noted that, the influence of crystallite size, crystal structure changes and specific surface area for photocatalytic activity are presented.

Folding and stacking defects of graphene flakes probed by electron nanobeam

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

Persichetti, L.; Fanfoni, M.; Sgarlata, A.

2011-07-25

Combining nanoscale imaging with local electron spectroscopy and diffraction has provided direct information on folding and stacking defects of graphene flakes produced by unrolled multi-walled carbon nanotubes. Structural data obtained by nanoarea electron diffraction complemented with systematic electron energy loss spectroscopy measurements of the surface plasmon losses of single flakes show the presence of flat bilayer regions coexisting with folded areas where the topology of buckled graphene resembles that of warped carbon nanostructures.

Fabrication of meso-porous BiOI sensitized zirconia nanoparticles with enhanced photocatalytic activity under simulated solar light irradiation

NASA Astrophysics Data System (ADS)

Vignesh, K.; Suganthi, A.; Min, Bong-Ki; Kang, Misook

2015-01-01

In this present work, BiOI sensitized zirconia (BiOI-ZrO2) nanoparticles were fabricated using a precipitation-deposition method. The physicochemical characteristics of BiOI/ZrO2 were studied through X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), BET-surface area, X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectroscopy (UV-vis-DRS) and photoluminescence (PL) spectroscopy techniques. The absorption maximum of ZrO2 was shifted to the visible region after sensitization with BiOI. BET-surface area results inferred that the prepared hetero-junctions were meso-porous in nature. The photocatalytic activity of BiOI-ZrO2 for the degradation of methyl violet (MV) dye under simulated solar light irradiation was investigated in detail. 3% BiOI-ZrO2 exhibited the highest photocatalytic performance (98% of MV degradation) when compared with ZrO2 and BiOI. The enhancement in the photocatalytic activity of BiOI-ZrO2 is ascribed to the sensitization effect of BiOI, suppression of electron-hole recombination and the formation of p-n hetero-junction.

Real-time specific surface area measurements via laser-induced breakdown spectroscopy

USGS Publications Warehouse

Washburn, Kathryn E.; Birdwell, Justin E.; Howard, James E.

2017-01-01

From healthcare to cosmetics to environmental science, the specific surface area (SSA) of micro- and mesoporous materials or products can greatly affect their chemical and physical properties. SSA results are also widely used to examine source rocks in conventional and unconventional petroleum resource plays. Despite its importance, current methods to measure SSA are often cumbersome, time-consuming, or require cryogenic consumables (e.g., liquid nitrogen). These methods are not amenable to high-throughput environments, have stringent sample preparation requirements, and are not practical for use in the field. We present a new application of laser-induced breakdown spectroscopy for rapid measurement of SSA. This study evaluates geological samples, specifically organic-rich oil shales, but the approach is expected to be applicable to many other types of materials. The method uses optical emission spectroscopy to examine laser-generated plasma and quantify the amount of argon adsorbed to a sample during an inert gas purge. The technique can accommodate a wide range of sample sizes and geometries and has the potential for field use. These advantages for SSA measurement combined with the simultaneous acquisition of composition information make this a promising new approach for characterizing geologic samples and other materials.

A microwave resonator for limiting depth sensitivity for electron paramagnetic resonance spectroscopy of surfaces.

PubMed

Sidabras, Jason W; Varanasi, Shiv K; Mett, Richard R; Swarts, Steven G; Swartz, Harold M; Hyde, James S

2014-10-01

A microwave Surface Resonator Array (SRA) structure is described for use in Electron Paramagnetic Resonance (EPR) spectroscopy. The SRA has a series of anti-parallel transmission line modes that provides a region of sensitivity equal to the cross-sectional area times its depth sensitivity, which is approximately half the distance between the transmission line centers. It is shown that the quarter-wave twin-lead transmission line can be a useful element for design of microwave resonators at frequencies as high as 10 GHz. The SRA geometry is presented as a novel resonator for use in surface spectroscopy where the region of interest is either surrounded by lossy material, or the spectroscopist wishes to minimize signal from surrounding materials. One such application is in vivo spectroscopy of human finger-nails at X-band (9.5 GHz) to measure ionizing radiation dosages. In order to reduce losses associated with tissues beneath the nail that yield no EPR signal, the SRA structure is designed to limit depth sensitivity to the thickness of the fingernail. Another application, due to the resonator geometry and limited depth penetration, is surface spectroscopy in coating or material science. To test this application, a spectrum of 1.44 μM of Mg(2+) doped polystyrene 1.1 mm thick on an aluminum surface is obtained. Modeling, design, and simulations were performed using Wolfram Mathematica (Champaign, IL; v. 9.0) and Ansys High Frequency Structure Simulator (HFSS; Canonsburg, PA; v. 15.0). A micro-strip coupling circuit is designed to suppress unwanted modes and provide a balanced impedance transformation to a 50 Ω coaxial input. Agreement between simulated and experimental results is shown.

A microwave resonator for limiting depth sensitivity for electron paramagnetic resonance spectroscopy of surfaces

PubMed Central

Sidabras, Jason W.; Varanasi, Shiv K.; Mett, Richard R.; Swarts, Steven G.; Swartz, Harold M.; Hyde, James S.

2014-01-01

A microwave Surface Resonator Array (SRA) structure is described for use in Electron Paramagnetic Resonance (EPR) spectroscopy. The SRA has a series of anti-parallel transmission line modes that provides a region of sensitivity equal to the cross-sectional area times its depth sensitivity, which is approximately half the distance between the transmission line centers. It is shown that the quarter-wave twin-lead transmission line can be a useful element for design of microwave resonators at frequencies as high as 10 GHz. The SRA geometry is presented as a novel resonator for use in surface spectroscopy where the region of interest is either surrounded by lossy material, or the spectroscopist wishes to minimize signal from surrounding materials. One such application is in vivo spectroscopy of human finger-nails at X-band (9.5 GHz) to measure ionizing radiation dosages. In order to reduce losses associated with tissues beneath the nail that yield no EPR signal, the SRA structure is designed to limit depth sensitivity to the thickness of the fingernail. Another application, due to the resonator geometry and limited depth penetration, is surface spectroscopy in coating or material science. To test this application, a spectrum of 1.44 μM of Mg2+ doped polystyrene 1.1 mm thick on an aluminum surface is obtained. Modeling, design, and simulations were performed using Wolfram Mathematica (Champaign, IL; v. 9.0) and Ansys High Frequency Structure Simulator (HFSS; Canonsburg, PA; v. 15.0). A micro-strip coupling circuit is designed to suppress unwanted modes and provide a balanced impedance transformation to a 50 Ω coaxial input. Agreement between simulated and experimental results is shown. PMID:25362434

A microwave resonator for limiting depth sensitivity for electron paramagnetic resonance spectroscopy of surfaces

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

Sidabras, Jason W.; Varanasi, Shiv K.; Hyde, James S.

2014-10-15

A microwave Surface Resonator Array (SRA) structure is described for use in Electron Paramagnetic Resonance (EPR) spectroscopy. The SRA has a series of anti-parallel transmission line modes that provides a region of sensitivity equal to the cross-sectional area times its depth sensitivity, which is approximately half the distance between the transmission line centers. It is shown that the quarter-wave twin-lead transmission line can be a useful element for design of microwave resonators at frequencies as high as 10 GHz. The SRA geometry is presented as a novel resonator for use in surface spectroscopy where the region of interest is eithermore » surrounded by lossy material, or the spectroscopist wishes to minimize signal from surrounding materials. One such application is in vivo spectroscopy of human finger-nails at X-band (9.5 GHz) to measure ionizing radiation dosages. In order to reduce losses associated with tissues beneath the nail that yield no EPR signal, the SRA structure is designed to limit depth sensitivity to the thickness of the fingernail. Another application, due to the resonator geometry and limited depth penetration, is surface spectroscopy in coating or material science. To test this application, a spectrum of 1.44 μM of Mg{sup 2+} doped polystyrene 1.1 mm thick on an aluminum surface is obtained. Modeling, design, and simulations were performed using Wolfram Mathematica (Champaign, IL; v. 9.0) and Ansys High Frequency Structure Simulator (HFSS; Canonsburg, PA; v. 15.0). A micro-strip coupling circuit is designed to suppress unwanted modes and provide a balanced impedance transformation to a 50 Ω coaxial input. Agreement between simulated and experimental results is shown.« less

Chemical modifications of Au/SiO2 template substrates for patterned biofunctional surfaces.

PubMed

Briand, Elisabeth; Humblot, Vincent; Landoulsi, Jessem; Petronis, Sarunas; Pradier, Claire-Marie; Kasemo, Bengt; Svedhem, Sofia

2011-01-18

The aim of this work was to create patterned surfaces for localized and specific biochemical recognition. For this purpose, we have developed a protocol for orthogonal and material-selective surface modifications of microfabricated patterned surfaces composed of SiO(2) areas (100 μm diameter) surrounded by Au. The SiO(2) spots were chemically modified by a sequence of reactions (silanization using an amine-terminated silane (APTES), followed by amine coupling of a biotin analogue and biospecific recognition) to achieve efficient immobilization of streptavidin in a functional form. The surrounding Au was rendered inert to protein adsorption by modification by HS(CH(2))(10)CONH(CH(2))(2)(OCH(2)CH(2))(7)OH (thiol-OEG). The surface modification protocol was developed by testing separately homogeneous SiO(2) and Au surfaces, to obtain the two following results: (i) SiO(2) surfaces which allowed the grafting of streptavidin, and subsequent immobilization of biotinylated antibodies, and (ii) Au surfaces showing almost no affinity for the same streptavidin and antibody solutions. The surface interactions were monitored by quartz crystal microbalance with dissipation monitoring (QCM-D), and chemical analyses were performed by polarization modulation-reflexion absorption infrared spectroscopy (PM-RAIRS) and X-ray photoelectron spectroscopy (XPS) to assess the validity of the initial orthogonal assembly of APTES and thiol-OEG. Eventually, microscopy imaging of the modified Au/SiO(2) patterned substrates validated the specific binding of streptavidin on the SiO(2)/APTES areas, as well as the subsequent binding of biotinylated anti-rIgG and further detection of fluorescent rIgG on the functionalized SiO(2) areas. These results demonstrate a successful protocol for the preparation of patterned biofunctional surfaces, based on microfabricated Au/SiO(2) templates and supported by careful surface analysis. The strong immobilization of the biomolecules resulting from the described protocol is advantageous in particular for micropatterned substrates for cell-surface interactions.

Influence of the adsorption geometry of PTCDA on Ag(111) on the tip-molecule forces in non-contact atomic force microscopy.

PubMed

Langewisch, Gernot; Falter, Jens; Schirmeisen, André; Fuchs, Harald

2014-01-01

Perylene-3,4,9,10-tetracarboxylic dianhydride (PTCDA) adsorbed on a metal surface is a prototypical organic-anorganic interface. In the past, scanning tunneling microscopy and scanning tunneling spectroscopy studies of PTCDA adsorbed on Ag(111) have revealed differences in the electronic structure of the molecules depending on their adsorption geometry. In the work presented here, high-resolution 3D force spectroscopy measurements at cryogenic temperatures were performed on a surface area that contained a complete PTCDA unit cell with the two possible geometries. At small tip-molecule separations, deviations in the tip-sample forces were found between the two molecule orientations. These deviations can be explained by a different electron density in both cases. This result demonstrates the capability of 3D force spectroscopy to detect even small effects in the electronic properties of organic adsorbates.

High Surface Area Dendrite Nanoelectrodes for Electrochemistry

NASA Astrophysics Data System (ADS)

Nesbitt, Nathan; Glover, Jennifer; Goyal, Saurabh; Simidjiysky, Svetoslav; Naughton, Michael

2014-03-01

Solution-based electrodeposition of metal using a low ion concentration, surface passivation agents, and/or electrochemical crystal conditioning has allowed for the formation of high surface area metal electrodes, useful for Raman spectroscopy and electrochemical sensors. Additionally, high frequency electrical oscillations have been used to electrically connect co-planar electrodes, a process called directed electrochemical nanowire assembly (DENA). These approaches aim to control the crystal face that metal atoms in solution will nucleate onto, thus causing anisotropic growth of metal crystals. However, DENA has not been used to create high surface area electrodes, and no study has been conducted on the effect of micron-scale surface topography on the initial nucleation of metal crystals on the electrode surface. When DENA is used to create a high surface area electrode, such a texture has a strong impact on the subsequent topography of the three dimensional dendritic structures by limiting the areal density of crystals on the electrode surface. Such structures both demonstrate unique physics concerning the nucleation of metal dendrites, and offer a unique and highly facile fabrication method of high surface area electrodes, useful for chemical and biological sensing. This material is based upon work supported by the National Science Foundation Graduate Research Fellowship under Grant No. (DGE-1258923).

Volumetric and infrared measurements on amorphous ice structure

NASA Astrophysics Data System (ADS)

Manca, C.; Martin, C.; Roubin, P.

2004-05-01

We have simultaneously used adsorption isotherm volumetry and Fourier transform infrared spectroscopy in order to take the investigations on amorphous ice structure a step further, especially concerning porosity and annealing-induced modifications. We have studied surface reorganization during annealing and found that the number of surface sites decreases before crystallization, their relative ratios being different for amorphous and crystalline ice. We also present results confirming that ice can have a large specific surface area and nevertheless be non-microporous.

Effects of pretreatment on the surface chemistry and pore size properties of nitrogen functionalized and alkylated granular activated carbon

NASA Astrophysics Data System (ADS)

Chen, Jiajun; Zhai, Yunbo; Chen, Hongmei; Li, Caiting; Zeng, Guangming; Pang, Daoxiong; Lu, Pei

2012-12-01

In this paper, granular activated carbon (GAC) from coconut shell was pretreated by HNO3, H2O2 and urea-formaldehyde resin, respectively. Then the obtained materials were functionalized in the same way for nitrogen group, and then alkylated. Effects of pretreatment on the surface chemistry and pore size of modified GACs were studied. Surface area and micropore volume of modified GAC which pretreated by HNO3 were 723.88 m2/g and 0.229 cm3/g, respectively, while virgin GAC were 742.34 m2/g and 0.276 cm3/g. Surface area and micropore volume decrease of the modified GACs which pretreated by the others two methods were more drastically. The types of groups presented were analyzed by electrophoresis, Fourier transform infrared spectroscopy (FTIR), and X-ray photoelectron spectroscopy (XPS). Nsbnd CH3 group and Cdbnd N group were detected on the surfaces of these three kinds of modified GACs. Results of XPS showed that the nitrogen functions of modified GAC which pretreated by H2O2 was 4.07%, it was more than that of the others two pretreatment methods. However, the modified GAC which pretreated by urea-formaldehyde resin was fixed more pyridine structure, which structure percentage was 45.88%, in addition, there were more basic groups or charge on the surface than the others.

Solution nuclear magnetic resonance spectroscopy on a nanostructured diamond chip.

PubMed

Kehayias, P; Jarmola, A; Mosavian, N; Fescenko, I; Benito, F M; Laraoui, A; Smits, J; Bougas, L; Budker, D; Neumann, A; Brueck, S R J; Acosta, V M

2017-08-04

Sensors using nitrogen-vacancy centers in diamond are a promising tool for small-volume nuclear magnetic resonance (NMR) spectroscopy, but the limited sensitivity remains a challenge. Here we show nearly two orders of magnitude improvement in concentration sensitivity over previous nitrogen-vacancy and picoliter NMR studies. We demonstrate NMR spectroscopy of picoliter-volume solutions using a nanostructured diamond chip with dense, high-aspect-ratio nanogratings, enhancing the surface area by 15 times. The nanograting sidewalls are doped with nitrogen-vacancies located a few nanometers from the diamond surface to detect the NMR spectrum of roughly 1 pl of fluid lying within adjacent nanograting grooves. We perform 1 H and 19 F nuclear magnetic resonance spectroscopy at room temperature in magnetic fields below 50 mT. Using a solution of CsF in glycerol, we determine that 4 ± 2 × 10 12 19 F spins in a 1 pl volume can be detected with a signal-to-noise ratio of 3 in 1 s of integration.Nitrogen vacancy (NV) centres in diamond can be used for NMR spectroscopy, but increased sensitivity is needed to avoid long measurement times. Kehayias et al. present a nanostructured diamond grating with a high density of NV centres, enabling NMR spectroscopy of picoliter-volume solutions.

Role of Raman spectroscopy and surface enhanced Raman spectroscopy in colorectal cancer

PubMed Central

Jenkins, Cerys A; Lewis, Paul D; Dunstan, Peter R; Harris, Dean A

2016-01-01

Colorectal cancer (CRC) is the fourth most common cancer in the United Kingdom and is the second largest cause of cancer related death in the United Kingdom after lung cancer. Currently in the United Kingdom there is not a diagnostic test that has sufficient differentiation between patients with cancer and those without cancer so the current referral system relies on symptomatic presentation in a primary care setting. Raman spectroscopy and surface enhanced Raman spectroscopy (SERS) are forms of vibrational spectroscopy that offer a non-destructive method to gain molecular information about biological samples. The techniques offer a wide range of applications from in vivo or in vitro diagnostics using endoscopic probes, to the use of micro-spectrometers for analysis of biofluids. The techniques have the potential to detect molecular changes prior to any morphological changes occurring in the tissue and therefore could offer many possibilities to aid the detection of CRC. The purpose of this review is to look at the current state of diagnostic technology in the United Kingdom. The development of Raman spectroscopy and SERS in clinical applications relation for CRC will then be discussed. Finally, future areas of research of Raman/SERS as a clinical tool for the diagnosis of CRC are also discussed. PMID:27190582

Surface and Interface Study of PdCr/SiC Schottky Diode Gas Sensor Annealed at 425 C

NASA Technical Reports Server (NTRS)

Chen, Liang-Yu; Hunter, Gary W.; Neudeck, Philip G.; Knight, Dak

1998-01-01

The surface and interface properties of Pd(sub 0.9)Cr(sub 0.1/SiC Schottky diode gas sensor both before and after annealing are investigated using Auger Electron Spectroscopy (AES), Scanning Electron Microscopy (SEM), and Energy Dispersive Spectroscopy (EDS). At room temperature the alloy reacted with SiC and formed Pd(sub x)Si only in a very narrow interfacial region. After annealing for 250 hours at 425 deg. C, the surface of the Schottky contact area has much less silicon and carbon contamination than that found on the surface of an annealed Pd/SiC structure. Pd(sub x)Si formed at a broadened interface after annealing, but a significant layer of alloy film is still free of silicon and carbon. The chromium concentration with respect to palladium is quite uniform down to the deep interface region. A stable catalytic surface and a clean layer of Pd(sub 0.9)Cr(sub 0.1) film are likely responsible for significantly improved device sensitivity.

Surface and Interface Properties of PdCr/SiC Schottky Diode Gas Sensor Annealed at 425 C

NASA Technical Reports Server (NTRS)

Chen, Liang-Yu; Hunter, Gary W.; Neudeck, Philip G.; Knight, Dak

1998-01-01

The surface and interface properties of Pd(0.9,)Cr(0.1)/SiC Schottky diode gas sensors both before and after annealing are investigated using Auger electron spectroscopy (AES), scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDS). At room temperature the alloy reacted with SiC and formed Pd,Si only in a very narrow interfacial region. After annealing for 250 h ,It 425 C, the surface of the Schottky contact area his much less silicon and carbon contamination than that found on the surface of an annealed Pd/SiC structure. Palladium silicides (Pd(x)Si) formed at a broadened interface after annealing, but a significant layer of alloy film is still free of silicon and carbon. The chromium concentration with respect to palladium is quite uniform down to the deep interface region. A stable catalytic surface and a clean layer of Pd(0.9)Cr(0.1) film are likely responsible for significantly improved device sensitivity.

Surface and Interface Properties of PdCr/SiC Schottky Diode Gas Sensor Annealed at 425 C

NASA Technical Reports Server (NTRS)

Chen, Liang-Yu; Hunter, Gary W.; Neudeck, Philip G.; Knight, Dak

1998-01-01

The surface and interface properties of Pd(0.9)Cr(0.1)/SiC Schottky diode gas sensors both before and after annealing are investigated using Auger Electron Spectroscopy (AES), Scanning Electron Microscopy (SEM), and Energy Dispersive Spectroscopy (EDS). At room temperature the alloy reacted with SiC and formed Pd(x)Si only in a very narrow interfacial region. After annealing for 250 hours at 425 C, the surface of the Schottky contact area has much less silicon and carbon contamination than that found on the surface of an annealed Pd/SiC structure. Palladium silicides (Pd(x)Si) formed at a broadened interface after annealing, but a significant layer of alloy film is still free of silicon and carbon. The chromium concentration with respect to palladium is quite uniform down to the deep interface region. A stable catalytic surface and a clean layer of Pd(0.9)Cr(0.1) film are likely responsible for significantly improved device sensitivity.

Quantitative analysis of trace levels of surface contamination by X-ray photoelectron spectroscopy Part I: statistical uncertainty near the detection limit.

PubMed

Hill, Shannon B; Faradzhev, Nadir S; Powell, Cedric J

2017-12-01

We discuss the problem of quantifying common sources of statistical uncertainties for analyses of trace levels of surface contamination using X-ray photoelectron spectroscopy. We examine the propagation of error for peak-area measurements using common forms of linear and polynomial background subtraction including the correlation of points used to determine both background and peak areas. This correlation has been neglected in previous analyses, but we show that it contributes significantly to the peak-area uncertainty near the detection limit. We introduce the concept of relative background subtraction variance (RBSV) which quantifies the uncertainty introduced by the method of background determination relative to the uncertainty of the background area itself. The uncertainties of the peak area and atomic concentration and of the detection limit are expressed using the RBSV, which separates the contributions from the acquisition parameters, the background-determination method, and the properties of the measured spectrum. These results are then combined to find acquisition strategies that minimize the total measurement time needed to achieve a desired detection limit or atomic-percentage uncertainty for a particular trace element. Minimization of data-acquisition time is important for samples that are sensitive to x-ray dose and also for laboratories that need to optimize throughput.

Physical and Chemical Characterization of Therapeutic Iron Containing Materials: A Study of Several Superparamagnetic Drug Formulations with the β-FeOOH or Ferrihydrite Structure

NASA Astrophysics Data System (ADS)

Funk, Felix; Long, Gary J.; Hautot, Dimitri; Büchi, Ruth; Christl, Iso; Weidler, Peter G.

2001-03-01

The effectiveness of therapeutically used iron compounds is related to their physical and chemical properties. Four different iron compounds used in oral, intravenous, and intramuscular therapy have been examined by X-ray powder diffraction, iron-57 Mössbauer spectroscopy, transmission electron microscopy, BET surface area measurement, potentiometric titration and studied through dissolution kinetics determinations using acid, reducing and chelating agents. All compounds are nanosized with particle diameters, as determined by X-ray diffraction, ranging from 1 to 4.1 nm. The superparamagnetic blocking temperatures, as determined by Mössbauer spectroscopy, indicate that the relative diameters of the aggregates range from 2.5 to 4.1 nm. Three of the iron compounds have an akaganeite-like structure, whereas one has a ferrihydrite-like structure. As powders the particles form large and dense aggregates which have a very low surface area on the order of 1 m2 g-1. There is evidence, however, that in a colloidal solution the surface area is increased by two to three orders of magnitude, presumably as a result of the break up of the aggregates. Iron release kinetics by acid, chelating and reducing agents reflect the high surface area, the size and crystallinity of the particles, and the presence of the protective carbohydrate layer coating the iron compound. Within a physiologically relevant time period, the iron release produced by acid or large chelating ligands is small. In contrast, iron is rapidly mobilized by small organic chelating agents, such as oxalate, or by chelate-forming reductants, such as thioglycolate.

Note: Micro-channel array crucible for isotope-resolved laser spectroscopy of high-temperature atomic beams

DOE PAGES

Lebedev, Vyacheslav; Bartlett, Joshua H.; Malyzhenkov, Alexander; ...

2017-12-06

Here, we present a novel compact design for a multichannel atomic oven which generates collimated beams of refractory atoms for fieldable laser spectroscopy. Using this resistively heated crucible, we demonstrate spectroscopy of an erbium sample at 1300 °C with improved isotopic resolution with respect to a single-channel design. In addition, our oven has a high thermal efficiency. By minimizing the surface area of the crucible, we achieve 2000 °C at 140 W of applied electrical power. As a result, the design does not require any active cooling and is compact enough to allow for its incorporation into fieldable instruments.

Note: Micro-channel array crucible for isotope-resolved laser spectroscopy of high-temperature atomic beams

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

Lebedev, Vyacheslav; Bartlett, Joshua H.; Malyzhenkov, Alexander

Here, we present a novel compact design for a multichannel atomic oven which generates collimated beams of refractory atoms for fieldable laser spectroscopy. Using this resistively heated crucible, we demonstrate spectroscopy of an erbium sample at 1300 °C with improved isotopic resolution with respect to a single-channel design. In addition, our oven has a high thermal efficiency. By minimizing the surface area of the crucible, we achieve 2000 °C at 140 W of applied electrical power. As a result, the design does not require any active cooling and is compact enough to allow for its incorporation into fieldable instruments.

Insights into the Interactions of Amino Acids and Peptides with Inorganic Materials Using Single-Molecule Force Spectroscopy.

PubMed

Das, Priyadip; Duanias-Assaf, Tal; Reches, Meital

2017-03-06

The interactions between proteins or peptides and inorganic materials lead to several interesting processes. For example, combining proteins with minerals leads to the formation of composite materials with unique properties. In addition, the undesirable process of biofouling is initiated by the adsorption of biomolecules, mainly proteins, on surfaces. This organic layer is an adhesion layer for bacteria and allows them to interact with the surface. Understanding the fundamental forces that govern the interactions at the organic-inorganic interface is therefore important for many areas of research and could lead to the design of new materials for optical, mechanical and biomedical applications. This paper demonstrates a single-molecule force spectroscopy technique that utilizes an AFM to measure the adhesion force between either peptides or amino acids and well-defined inorganic surfaces. This technique involves a protocol for attaching the biomolecule to the AFM tip through a covalent flexible linker and single-molecule force spectroscopy measurements by atomic force microscope. In addition, an analysis of these measurements is included.

A three-dimensional microelectrode array composed of vertically aligned ultra-dense carbon nanotube networks

NASA Astrophysics Data System (ADS)

Nick, C.; Yadav, S.; Joshi, R.; Schneider, J. J.; Thielemann, C.

2015-07-01

Electrodes based on carbon nanotubes are a promising approach to manufacture highly sensitive sensors with a low limit of signal detection and a high signal-to-noise ratio. This is achieved by dramatically increasing the electrochemical active surface area without increasing the overall geometrical dimensions. Typically, carbon nanotube electrodes are nearly planar and composed of randomly distributed carbon nanotube networks having a limited surface gain for a specific geometrical surface area. To overcome this limitation, we have introduced vertically aligned carbon nanotube (VACNT) networks as electrodes, which are arranged in a microelectrode pattern of 60 single electrodes. Each microelectrode features a very high aspect ratio of more than 300 and thus a dramatically increased surface area. These microelectrodes composed of VACNT networks display dramatically decreased impedance over the entire frequency range compared to planar microelectrodes caused by the enormous capacity increase. This is experimentally verified by electrochemical impedance spectroscopy and cyclic voltammetry.

Davisson-Germer Prize in Atomic or Surface Physics Talk: Soft X-Ray Studies of Surfaces, Interfaces and Thin Films: From Spectroscopy to Ultrafast Nanoscale Movies

NASA Astrophysics Data System (ADS)

Stöhr, Joachim

2011-03-01

My talk will review the development of soft x-ray spectroscopy and microscopy and its impact on our understanding of chemical bonding, magnetism and dynamics at surfaces and interfaces. I will first outline important soft x-ray spectroscopy and microscopy techniques that have been developed over the last 30 years and their key strengths such as elemental and chemical specificity, sensitivity to small atomic concentrations, separation of charge and spin properties, spatial resolution down to the nanometer scale, and temporal resolution down to the intrinsic femtosecond timescale of atomic and electronic motions. I will then present scientific breakthroughs based on soft x-ray studies in three selected areas: the nature of molecular bonding and reactivity on metal surfaces, the molecular origin of liquid crystal alignment on surfaces, and the microscopic origin of interface-mediated spin alignments in modern magnetic devices. My talk will also cover the use of soft x-rays for revealing the temporal evolution of electronic structure, addressing the key problem of ``function,'' down to the intrinsic femtosecond time scale of charge and spin configuration changes. As examples I will present the formation and breaking of chemical bonds in surface complexes and the motion of the magnetization in magnetic devices. Work supported by the Office of Basic Energy Science of the US Department of Energy.

Reciprocal-space and real-space neutron investigation of nanostructured Mo 2C and WC

NASA Astrophysics Data System (ADS)

Page, Katharine; Li, Jun; Savinelli, Robert; Szumila, Holly N.; Zhang, Jinping; Stalick, Judith K.; Proffen, Thomas; Scott, Susannah L.; Seshadri, Ram

2008-11-01

As possible substitute materials for platinum group metal heterogeneous catalysts, high surface area carbides of the early transition metals Mo and W are of great interest. Here we report nanostructured, high surface area Mo 2C and WC prepared by decomposing and carburizing ammonium paramolybdate [(NH 4) 6Mo 7O 24·4H 2O] and ammonium paratungstate [(NH 4) 10W 12O 41·5H 2O] in flowing 50%CH 4/50%H 2. Surface areas as high as 52 m 2/g for Mo 2C and 24 m 2/g for WC were obtained, with both structures crystallizing in structures appropriate for catalytic activity. We have studied these materials using a combination of neutron diffraction Rietveld refinement, X-ray photoelectron spectroscopy, surface area measurements, and scanning transmission electron microscopy. In addition, we have used pair-distribution function (PDF) analysis of the neutron total scattering data as a means of establishing the presence of graphitic carbon in the as-prepared materials.

Synthesis and structural characteristics of high surface area TiO2 aerogels by ultrasonic-assisted sol-gel method

NASA Astrophysics Data System (ADS)

Qingge, Feng; Huidong, Cai; Haiying, Lin; Siying, Qin; Zheng, Liu; Dachao, Ma; Yuyang, Ye

2018-02-01

TiO2 aerogel is a unique three-dimensional porous nano-particle material with the characteristics of high specific surface area and good light transmittance. In this paper, a novel method involving ultrasonic-assisted sol-gel, solvent exchange, and vacuum drying was successfully developed to synthesis the TiO2 aerogel. The morphology and properties of the prepared TiO2 aerogels were characterized by the Brunauer-Emmett-Teller theory (BET), x-ray diffraction, field-emission scanning electron microscopy, energy dispersive spectroscopy, thermogravimetric analysis-differential thermal analysis, Fourier transform infrared spectroscopy, and Raman spectroscopy. The adsorption and photocatalytic activity of TiO2 aerogels was evaluated by monitoring the degradation of Rhodamine B solution. Our results indicated that: (1) with an optimum ratio of Ti:H2O = 8:1 the BET surface area, average pore diameter, and total pore volume of TiO2 aerogel are enhanced to 563.6 m2 g-1, 3.01 nm, and 0.42 cm3 g-1, respectively; (2) the TiO2 aerogels possessed controllable crystal form depending on the thermal treatments conditions. The crystal face (101) of anatase, complete anatase, mixed state of anatase and rutile, and rutile were obtained by increasing the temperature from 200 °C-300 °C, from 400 °C-500 °C, 600 °C, and from 700 °C-1000 °C, respectively; and (3) the excellent catalytic activity of the as-prepared TiO2 aerogels for the ultraviolet photolytic degradation of Rhodamine B had attributed to the synergistic effect of adsorption and photoactivity.

Structural investigation of Langmuir and Langmuir-Blodgett monolayers of semifluorinated alkanes.

PubMed

Dynarowicz Łatka, Patrycja; Pérez-Morales, Marta; Muñoz, Eulogia; Broniatowski, Marcin; Martín-Romero, María T; Camacho, Luis

2006-03-30

The behavior of a semi-fluorinated alkane (C(10)F(21)C(19)H(39)) has been studied at the air-water interface by using surface pressure and surface potential-area isotherms as well as infrared spectroscopy for the Langmuir-Blodgett films. In addition, based on the quantum chemical PM3 semiempirical approach, the dimer structure was investigated, and the double helix was found to be the most stable conformation of the dimer. The obtained results allow us to imply that the phase transition observed in the course of the surface pressure/area isotherm is due to a conformational change originating from the double helix to a vertical, single helix configuration.

Tailored Rh surface facilitates, enhancement of Raman scattering in trimetallic AuPt core/Rh shell composites: Experimental and theoretical evidences

NASA Astrophysics Data System (ADS)

Loganathan, B.; Chandraboss, V. L.; Senthilvelan, S.; Karthikeyan, B.

2016-01-01

We present a detailed analysis of surface-enhanced Raman scattering of 7-azaindole and L-cysteine adsorbed on a tailored Rh surface by using experimental and density functional theoretical (DFT) calculations. DFT with the B3LYP/Lanl2DZ basis set was used for the optimization of the ground state geometries and simulation of the surface-enhanced Raman spectrum of probe molecules adsorbed on Rh6 cluster. 7-azaindole and L-cysteine adsorption at the shell interface was ascertained from first-principles. In addition, characterization of synthesized trimetallic AuPt core/Rh shell colloidal nanocomposites has been analyzed by UV-visible spectroscopy, high-resolution transmission and scanning electron microscopy, selected area electron diffraction pattern analysis, energy-dispersive X-ray spectroscopy, atomic force, confocal Raman microscopy, FT-Raman and surface-enhanced Raman spectroscopic analysis. This analysis serves as the first step in gaining an accurate understanding of specific interactions at the interface of organic and biomolecules and to gain knowledge on the surface composition of trimetallic Au/Pt/Rh colloidal nanocomposites.

Carbon Nanotubes and Algal Polysaccharides To Enhance the Enzymatic Properties of Urease in Lipid Langmuir-Blodgett Films.

PubMed

Rodrigues, Raul T; Morais, Paulo V; Nordi, Cristina S F; Schöning, Michael J; Siqueira, José R; Caseli, Luciano

2018-03-06

Algal polysaccharides (extracellular polysaccharides) and carbon nanotubes (CNTs) were adsorbed on dioctadecyldimethylammonium bromide Langmuir monolayers to serve as a matrix for the incorporation of urease. The physicochemical properties of the supramolecular system as a monolayer at the air-water interface were investigated by surface pressure-area isotherms, surface potential-area isotherms, interfacial shear rheology, vibrational spectroscopy, and Brewster angle microscopy. The floating monolayers were transferred to hydrophilic solid supports, quartz, mica, or capacitive electrolyte-insulator-semiconductor (EIS) devices, through the Langmuir-Blodgett (LB) technique, forming mixed films, which were investigated by quartz crystal microbalance, fluorescence spectroscopy, and field emission gun scanning electron microscopy. The enzyme activity was studied with UV-vis spectroscopy, and the feasibility of the thin film as a urea sensor was essayed in an EIS sensor device. The presence of CNT in the enzyme-lipid LB film not only tuned the catalytic activity of urease but also helped to conserve its enzyme activity. Viability as a urease sensor was demonstrated with capacitance-voltage and constant capacitance measurements, exhibiting regular and distinctive output signals over all concentrations used in this work. These results are related to the synergism between the compounds on the active layer, leading to a surface morphology that allowed fast analyte diffusion owing to an adequate molecular accommodation, which also preserved the urease activity. This work demonstrates the feasibility of employing LB films composed of lipids, CNT, algal polysaccharides, and enzymes as EIS devices for biosensing applications.

La and Al co-doped CaMnO3 perovskite oxides: From interplay of surface properties to anion exchange membrane fuel cell performance

NASA Astrophysics Data System (ADS)

Dzara, Michael J.; Christ, Jason M.; Joghee, Prabhuram; Ngo, Chilan; Cadigan, Christopher A.; Bender, Guido; Richards, Ryan M.; O'Hayre, Ryan; Pylypenko, Svitlana

2018-01-01

This work reports the first account of perovskite oxide and carbon composite oxygen reduction reaction (ORR) catalysts integrated into anion exchange membrane fuel cells (AEMFCs). Perovskite oxides with a theoretical stoichiometry of Ca0.9La0.1Al0.1Mn0.9O3-δ are synthesized by an aerogel method and calcined at various temperatures, resulting in a set of materials with varied surface chemistry and surface area. Material composition is evaluated by X-ray diffraction, energy dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy. The perovskite oxide calcined at 800 °C shows the importance of balance between surface area, purity of the perovskite phase, and surface composition, resulting in the highest ORR mass activity when evaluated in rotating disk electrodes. Integration of this catalyst into AEMFCs reveals that the best AEMFC performance is obtained when using composites with 30:70 perovskite oxide:carbon composition. Doubling the loading leads to an increase in the power density from 30 to 76 mW cm-2. The AEMFC prepared with a composite based on perovskite oxide and N-carbon achieves a power density of 44 mW cm-2, demonstrating an ∼50% increase when compared to the highest performing composite with undoped carbon at the same loading.

Finely Tuned SnO2 Nanoparticles for Efficient Detection of Reducing and Oxidizing Gases: The Influence of Alkali Metal Cation on Gas-Sensing Properties.

PubMed

Lee, Szu-Hsuan; Galstyan, Vardan; Ponzoni, Andrea; Gonzalo-Juan, Isabel; Riedel, Ralf; Dourges, Marie-Anne; Nicolas, Yohann; Toupance, Thierry

2018-03-28

Tin dioxide (SnO 2 ) nanoparticles were straightforwardly synthesized using an easily scaled-up liquid route that involves the hydrothermal treatment, either under acidic or basic conditions, of a commercial tin dioxide particle suspension including potassium counterions. After further thermal post-treatment, the nanomaterials have been thoroughly characterized by Fourier transform infrared and Raman spectroscopy, powder X-ray diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy, and nitrogen sorption porosimetry. Varying pH conditions and temperature of the thermal treatment provided cassiterite SnO 2 nanoparticles with crystallite sizes ranging from 7.3 to 9.7 nm and Brunauer-Emmett-Teller surface areas ranging from 61 to 106 m 2 ·g -1 , acidic conditions favoring potassium cation removal. Upon exposure to a reducing gas (H 2 , CO, and volatile organic compounds such as ethanol and acetone) or oxidizing gas (NO 2 ), layers of these SnO 2 nanoparticles led to highly sensitive, reversible, and reproducible responses. The sensing results were discussed in regard to the crystallite size, specific area, valence band energy, Debye length, and chemical composition. Results highlight the impact of the counterion residuals, which affect the gas-sensing performance to an extent much higher than that of size and surface area effects. Tin dioxide nanoparticles prepared under acidic conditions and calcined in air showed the best sensing performances because of lower amount of potassium cations and higher crystallinity, despite the lower surface area.

Synthesis of Cr3+-doped TiO2 nanoparticles: characterization and evaluation of their visible photocatalytic performance and stability.

PubMed

Mendiola-Alvarez, Sandra Yadira; Guzmán-Mar, Jorge Luis; Turnes-Palomino, Gemma; Maya-Alejandro, Fernando; Caballero-Quintero, Adolfo; Hernández-Ramírez, Aracely; Hinojosa-Reyes, Laura

2017-09-28

Cr 3+ -doped TiO 2 nanoparticles (Ti-Cr) were synthesized by microwave-assisted sol-gel method. The Ti-Cr catalyst was characterized by X-ray diffraction, ultraviolet-visible diffuse reflectance spectroscopy, N 2 adsorption-desorption analysis, Raman spectroscopy, scanning electron microscopy, transmission electron microscopy, photoluminescence spectroscopy, X-ray photoelectron spectroscopy (XPS) and zetametry. The anatase mesoporous Ti-Cr material exhibited a specific surface area of 54.5 m 2 /g. XPS analysis confirmed the proper substitution of Ti 4+ cations by Cr 3+ cations in the TiO 2 matrix. The particle size was of average size of 17 nm for the undoped TiO 2 but only 9.5 nm for Ti-Cr. The Cr atoms promoted the formation of hydroxyl radicals and modified the surface adsorptive properties of TiO 2 due to the increase in surface acidity of the material. The photocatalytic evaluation demonstrated that the Ti-Cr catalyst completely degraded (4-chloro-2-methylphenoxy) acetic acid under visible light irradiation, while undoped TiO 2 and P25 allowed 45.7% and 31.1%, respectively. The rate of degradation remained 52% after three cycles of catalyst reuse. The higher visible light photocatalytic activity of Ti-Cr was attributed to the beneficial effect of Cr 3+ ions on the TiO 2 surface creating defects within the TiO 2 crystal lattice, which can act as charge-trapping sites, reducing the electron-hole recombination process.

Additively Manufactured and Surface Biofunctionalized Porous Nitinol.

PubMed

Gorgin Karaji, Z; Speirs, M; Dadbakhsh, S; Kruth, J-P; Weinans, H; Zadpoor, A A; Amin Yavari, S

2017-01-18

Enhanced bone tissue regeneration and improved osseointegration are among the most important goals in design of multifunctional orthopedic biomaterials. In this study, we used additive manufacturing (selective laser melting) to develop multifunctional porous nitinol that combines superelasticity with a rationally designed microarchitecture and biofunctionalized surface. The rational design based on triply periodic minimal surfaces aimed to properly adjust the pore size, increase the surface area (thereby amplifying the effects of surface biofunctionalization), and resemble the curvature characteristics of trabecular bone. The surface of additively manufactured (AM) porous nitinol was biofunctionalized using polydopamine-immobilized rhBMP2 for better control of the release kinetics. The actual morphological properties of porous nitinol measured by microcomputed tomography (e.g., open/close porosity, and surface area) closely matched the design values. The superelasticity originated from the austenite phase formed in the nitinol porous structure at room temperature. Polydopamine and rhBMP2 signature peaks were confirmed by X-ray photoelectron spectroscopy and Fourier transform infrared spectroscopy tests. The release of rhBMP2 continued until 28 days. The early time and long-term release profiles were found to be adjustable independent of each other. In vitro cell culture showed improved cell attachment, cell proliferation, cell morphology (spreading, spindle-like shape), and cell coverage as well as elevated levels of ALP activity and increased calcium content for biofunctionalized surfaces as compared to as-manufactured specimens. The demonstrated functionalities of porous nitinol could be used as a basis for deployable orthopedic implants with rationally designed microarchitectures that maximize bone tissue regeneration performance by release of biomolecules with adjustable and well-controlled release profiles.

Enhanced Hydrogen Evolution Reactions on Nanostructured Cu2ZnSnS4 (CZTS) Electrocatalyst

NASA Astrophysics Data System (ADS)

Digraskar, Renuka V.; Mulik, Balaji B.; Walke, Pravin S.; Ghule, Anil V.; Sathe, Bhaskar R.

2017-08-01

A novel and facile one-step sonochemical method is used to synthesize Cu2ZnSnS4 (CZTS) nanoparticles (2.6 ± 0.4 nm) as cathode electrocatalyst for hydrogen evolution reactions. The detailed morphology, crystal and surface structure, and composition of the CZTS nanostructures were characterized by high resolution transmission electron microscopy (HR-TEM), Selected area electron diffraction (SAED), X-ray diffraction, Raman spectroscopy, FTIR analysis, Brunauer-Emmett-Teller (BET) surface area measurements, Electron dispersive analysis, X-ray photoelectron spectroscopy respectively. Electrocatalytic abilities of the nanoparticles toward Hydrogen Evolution Reactions (HER) were verified through cyclic voltammograms (CV) and Linear sweep voltammetry (LSV), electrochemical impedance spectroscopy (EIS), and Tafel polarization measurements. It reveals enhanced activity at lower onset potential 300 mV v/s RHE, achieved at exceptionally high current density -130 mA/cm2, which is higher than the existing non-nobel metal based cathodes. Further result exhibits Tafel slope of 85 mV/dec, exchange current density of 882 mA/cm2, excellent stability (> 500 cycles) and lower charge transfer resistance. This sonochemically fabricated CZTSs nanoparticles are leading to significantly reduce cell cost and simplification of preparation process over existing high efficiency Pt and other nobel metal-free cathode electrocatalyst.

Effects of simulated inflammation on the corrosion of 316L stainless steel.

PubMed

Brooks, Emily K; Brooks, Richard P; Ehrensberger, Mark T

2017-02-01

Stainless steel alloys, including 316L, find use in orthopaedics, commonly as fracture fixation devices. Invasive procedures involved in the placement of these devices will provoke a local inflammatory response that produces hydrogen peroxide (H 2 O 2 ) and an acidic environment surrounding the implant. This study assessed the influence of a simulated inflammatory response on the corrosion of 316L stainless steel. Samples were immersed in an electrolyte representing either normal or inflammatory physiological conditions. After 24h of exposure, electrochemical impedance spectroscopy (EIS) and inductively coupled plasma mass spectroscopy (ICPMS) were used to evaluate differences in corrosion behavior and ion release induced by the inflammatory conditions. Scanning electron microscopy (SEM) and energy-dispersive x-ray spectroscopy (EDX) were used to evaluate surface morphology and corrosion products formed on the sample surface. Inflammatory conditions, involving the presence of H 2 O 2 and an acidic pH, significantly alter the corrosion processes of 316L stainless steel, promoting aggressive and localized corrosion. It is demonstrated that particular consideration should be given to 316L stainless steel implants with crevice susceptible areas (ex. screw-head/plate interface), as those areas may have an increased probability of rapid and aggressive corrosion when exposed to inflammatory conditions. Copyright © 2016 Elsevier B.V. All rights reserved.

Attenuated Total Reflection Fourier Transform Infrared Spectroscopy (ATR FT-IR) Applied to Study the Distribution of Ink Components in Printed Newspapers.

PubMed

Gómez, Nuria; Molleda, Cristina; Quintana, Ester; Carbajo, José M; Rodríguez, Alejandro; Villar, Juan C

2016-09-01

A new method was developed to study how the oil and cyan pigments of cold-set ink are distributed in newspaper thickness. The methodology involved laboratory printing followed by delamination of the printed paper. The unprinted side, printed side, and resulting layers were analyzed using attenuated total reflection Fourier transform infrared spectroscopy (ATR FT-IR). Three commercial newspapers and black and cyan cold-set inks were chosen for the study. Attenuated total reflection Fourier transform infrared spectroscopy enabled the proportion of oil and cyan pigment on the printed surface and throughout the sheet thickness to be measured. Oil percentage was evaluated as the area increment of the region from 2800 cm(-1) to 3000 cm(-1) The relative amount of cyan pigment was determined as the area of the absorption band at 730 cm(-1) The ink oil was found mainly below half the paper thickness, whereas the pigment was detected at the layers closer to the printed surface, at a depth penetration of less than 15 µm (20% of thickness). Distribution of these two components in paper thickness depended on the type of cold-set ink, the amount of ink transferred, and the newspaper properties. © The Author(s) 2016.

Large area planar stanene epitaxially grown on Ag(1 1 1)

NASA Astrophysics Data System (ADS)

Yuhara, Junji; Fujii, Yuya; Nishino, Kazuki; Isobe, Naoki; Nakatake, Masashi; Xian, Lede; Rubio, Angel; Le Lay, Guy

2018-04-01

Artificial post-graphene elemental 2D materials have received much attention recently. Especially, stanene, the tin analogue of graphene, is expected to be a robust 2D topological insulator, even above room temperature. We have grown epitaxial 2D stanene on a Ag(1 1 1) single crystal template and determined its crystalline structure synergetically by scanning tunneling microscopy, high-resolution synchrotron radiation photoemission spectroscopy, and advanced first principles calculations. From the STM images, we show that stanene forms a nearly planar structure in large domains. A detailed core-level spectroscopy analysis as well as DFT calculations reveal that the stanene sheet lays over an ordered 2D Ag2Sn surface alloy, but not directly on a bulk-terminated Ag(1 1 1) surface. The electronic structure exhibits a characteristic 2D band with parabolic dispersion due to the non-negligible interaction with the underlying surface alloy.

Growth of carbon nanotubes in arc plasma treated graphite disc: microstructural characterization and electrical conductivity study

NASA Astrophysics Data System (ADS)

Nayak, B. B.; Sahu, R. K.; Dash, T.; Pradhan, S.

2018-03-01

Circular graphite discs were treated in arc plasma by varying arcing time. Analysis of the plasma treated discs by field emission scanning electron microscope revealed globular grain morphologies on the surfaces, but when the same were observed at higher magnification and higher resolution under transmission electron microscope, growth of multiwall carbon nanotubes of around 2 nm diameter was clearly seen. In situ growth of carbon nanotube bundles/bunches consisting of around 0.7 nm tube diameter was marked in the case of 6 min treated disc surface. Both the untreated and the plasma treated graphite discs were characterized by X-ray diffraction, energy dispersive spectra of X-ray, X-ray photoelectron spectroscopy, transmission electron microscopy, micro Raman spectroscopy and BET surface area measurement. From Raman spectra, BET surface area and microstructure observed in transmission electron microscope, growth of several layers of graphene was identified. Four-point probe measurements for electrical resistivity/conductivity of the graphite discs treated under different plasma conditions showed significant increase in conductivity values over that of untreated graphite conductivity value and the best result, i.e., around eightfold increase in conductivity, was observed in the case of 6 min plasma treated sample exhibiting carbon nanotube bundles/bunches grown on disc surface. By comparing the microstructures of the untreated and plasma treated graphite discs, the electrical conductivity increase in graphite disc is attributed to carbon nanotubes (including bundles/bunches) growth on disc surface by plasma treatment.

Near infrared reflectance spectroscopy studies of Chinese giant salamanders in aquaculture production

USDA-ARS?s Scientific Manuscript database

NIR spectra were collected at three surface locations for Chinese giant salamanders to ascertain whether spectral signatures could be separated by anatomical, presumably physiologically-based, locations. The first location was the smooth area immediately above the cloaca on the animal’s abdomen, whi...

Study of Surface Cleaning Methods and Pyrolysis Temperature on Nano-Structured Carbon Films using X-ray Photoelectron Spectroscopy

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

Kerber, Pranita B.; Porter, Lisa M.; McCullough, L. A.

2012-10-12

Nanostructured carbon (ns-C) films fabricated by stabilization and pyrolysis of di-block copolymers are of interest for a variety of electrical/electronic applications due to their chemical inertness, high-temperature insensitivity, very high surface area, and tunable electrical resistivity over a wide range [Kulkarni et al., Synth. Met. 159, (2009) 177]. Because of their high porosity and associated high specific surface area, controlled surface cleaning studies are important for fabricating electronic devices from these films. In this study, quantification of surface composition and surface cleaning studies on ns-C films synthesized by carbonization of di-block copolymers of polyacrylonitrile-b-poly(n-butyl acrylate) (PAN-b-PBA) at two different temperaturesmore » were carried out. X-ray photoelectron spectroscopy was used for elemental analysis and to determine the efficacy of various surface cleaning methods for ns-C films and to examine the polymer residues in the films. The in-situ surface cleaning methods included: HF vapor treatment, vacuum annealing, and exposure to UV-ozone. Quantitative analysis of high-resolution XPS scans showed 11 at. % of nitrogen present in the films pyrolyzed at 600 °C, suggesting incomplete denitrogenation of the copolymer films. The nitrogen atomic concentration reduced significantly for films pyrolyzed at 900 °C confirming extensive denitrogenation at that temperature. Furthermore, quantitative analysis of nitrogen sub-peaks indicated higher loss of nitrogen atoms residing at the edge of graphitic clusters relative to that of nitrogen atoms within the graphitic cluster, suggesting higher graphitization with increasing pyrolysis temperature. Of the surface cleaning methods investigated, in-situ annealing of the films at 300 °C for 40 min was found to be the most efficacious in removing adventitious carbon and oxygen impurities from the surface.« less

Study of surface cleaning methods and pyrolysis temperatures on nanostructured carbon films using x-ray photoelectron spectroscopy

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

Kerber, Pranita; Porter, Lisa M.; McCullough, Lynne A.

2012-11-15

Nanostructured carbon (ns-C) films fabricated by stabilization and pyrolysis of diblock copolymers are of interest for a variety of electrical/electronic applications due to their chemical inertness, high-temperature insensitivity, very high surface area, and tunable electrical resistivity over a wide range [Kulkarni et al., Synth. Met. 159, 177 (2009)]. Because of their high porosity and associated high specific surface area, controlled surface cleaning studies are important for fabricating electronic devices from these films. In this study, quantification of surface composition and surface cleaning studies on ns-C films synthesized by carbonization of diblock copolymers of polyacrylonitrile-b-poly(n-butyl acrylate) at two different temperatures weremore » carried out. X-ray photoelectron spectroscopy was used for elemental analysis and to determine the efficacy of various surface cleaning methods for ns-C films and to examine the polymer residues in the films. The in-situ surface cleaning methods included HF vapor treatment, vacuum annealing, and exposure to UV-ozone. Quantitative analysis of high-resolution XPS scans showed 11 at. % nitrogen was present in the films pyrolyzed at 600 Degree-Sign C, suggesting incomplete denitrogenation of the copolymer films. The nitrogen atomic concentration decreased significantly for films pyrolyzed at 900 Degree-Sign C confirming extensive denitrogenation at that temperature. Furthermore, quantitative analysis of nitrogen subpeaks indicated higher loss of nitrogen atoms residing at the edge of graphitic clusters relative to that of nitrogen atoms within the graphitic clusters, suggesting higher graphitization with increasing pyrolysis temperature. Of the surface cleaning methods investigated, in-situ annealing of the films at 300 Degree-Sign C for 40 min was found to be the most efficacious in removing adventitious carbon and oxygen impurities from the surface.« less

Biosilica from Living Diatoms: Investigations on Biocompatibility of Bare and Chemically Modified Thalassiosira weissflogii Silica Shells

PubMed Central

Cicco, Stefania Roberta; Vona, Danilo; Gristina, Roberto; Sardella, Eloisa; Ragni, Roberta; Lo Presti, Marco; Farinola, Gianluca Maria

2016-01-01

In the past decade, mesoporous silica nanoparticles (MSNs) with a large surface area and pore volume have attracted considerable attention for their application in drug delivery and biomedicine. Here we propose biosilica from diatoms as an alternative source of mesoporous materials in the field of multifunctional supports for cell growth: the biosilica surfaces were chemically modified by traditional silanization methods resulting in diatom silica microparticles functionalized with 3-mercaptopropyl-trimethoxysilane (MPTMS) and 3-aminopropyl-triethoxysilane (APTES). Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy analyses revealed that the –SH or –NH2 were successfully grafted onto the biosilica surface. The relationship among the type of functional groups and the cell viability was established as well as the interaction of the cells with the nanoporosity of frustules. These results show that diatom microparticles are promising natural biomaterials suitable for cell growth, and that the surfaces, owing to the mercapto groups, exhibit good biocompatibility. PMID:28952597

Synthesis of Mesoporous Nanocrystalline Zirconia by Surfactant-Assisted Hydrothermal Approach.

PubMed

Nath, Soumav; Biswas, Ashik; Kour, Prachi P; Sarma, Loka S; Sur, Ujjal Kumar; Ankamwar, Balaprasad G

2018-08-01

In this paper, we have reported the chemical synthesis of thermally stable mesoporous nanocrystalline zirconia with high surface area using a surfactant-assisted hydrothermal approach. We have employed different type of surfactants such as CTAB, SDS and Triton X-100 in our synthesis. The synthesized nanocrystalline zirconia multistructures exhibit various morphologies such as rod, mortar-pestle with different particle sizes. We have characterized the zirconia multistructures by X-ray diffraction study, Field emission scanning electron microscopy, Attenuated total refection infrared spectroscopy, UV-Vis spectroscopy and photoluminescence spectroscopy. The thermal stability of as synthesized zirconia multistructures was studied by thermo gravimetric analysis, which shows the high thermal stability of nanocrystalline zirconia around 900 °C temperature.

Plasma-assisted reduction of silver ions impregnated into a natural zeolite framework

NASA Astrophysics Data System (ADS)

Osonio, Airah P.; Vasquez, Magdaleno R.

2018-02-01

A green, dry, and energy-efficient method for the fabrication of silver-zeolite (AgZ) composite via 13.56 MHz radio-frequency plasma reduction is demonstrated. Impregnation by soaking and ion-exchange deposition were performed to load the silver ions (Ag+) into the sodium-zeolite samples. Characterization was performed by optical emission spectroscopy, Fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy, X-ray photoelectron spectroscopy, and Brunauer-Emmett-Teller analyses. Results indicate the successful reduction of Ag+ to its metallic state on the surface of the zeolite with a mean diameter of 165 nm. This plasma-induced reduction technique opens possibilities in several areas including catalysis, adsorption, water treatment, and medicine.

Radiolytic hydrogen generation at silicon carbide-water interfaces

NASA Astrophysics Data System (ADS)

Schofield, Jennifer; Reiff, Sarah C.; Pimblott, Simon M.; LaVerne, Jay A.

2016-02-01

While many of the proposed uses of SiC in the nuclear industry involve systems that are assumed to be dry, almost all materials have dissociated chemisorbed water associated with their surface, which can undergo chemistry in radiation fields. Silicon carbide α-phase and β-phase nanoparticles with water were irradiated with γ-rays and 5 MeV 4He ions followed by the determination of the production of molecular hydrogen, H2, and characterization of changes in the particle surface. The yields of H2 from SiC-water slurries were always greater than expected from a simple mixture rule indicating that the presence of SiC was influencing the production of H2 from water, probably through an energy transfer from the solid to liquid phase. Although the increase in H2 yields was modest, a decrease in the water mass percentage led to an increase in H2 yields, especially for very low amounts of water. Surface analysis techniques included diffuse reflectance infrared Fourier transform spectroscopy (DRIFT), nitrogen absorption with the Brunauer - Emmett - Teller (BET) methodology for surface area determination, X-ray diffraction (XRD), Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS). Little change in the SiC surface was observed following radiolysis except for some conversion of β-phase SiC to the α-phase and the formation of SiO2 with He ion radiolysis.

Novel mesoporous FeAl bimetal oxides for As(III) removal: Performance and mechanism.

PubMed

Ding, Zecong; Fu, Fenglian; Cheng, Zihang; Lu, Jianwei; Tang, Bing

2017-02-01

In this study, novel mesoporous FeAl bimetal oxides were successfully synthesized, characterized, and employed for As(III) removal. Batch experiments were conducted to investigate the effects of Fe/Al molar ratio, dosage, and initial solution pH values on As(III) removal. The results showed that the FeAl bimetal oxide with Fe/Al molar ratio 4:1 (shorten as FeAl-4) can quickly remove As(III) from aqueous solution in a wide pH range. The FeAl-4 before and after reaction with As(III) was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HR-TEM) and selected area electron diffraction (SAED), Brunauer-Emmett-Teller (BET) surface area measurement, and X-ray photoelectron spectroscopy (XPS). The BET results showed that the original FeAl-4 with a high surface area of 223.9 m 2 /g was a mesoporous material. XPS analysis indicated that the surface of FeAl-4 possessed a high concentration of M-OH (where M represents Fe and Al), which was beneficial to the immobility of As(III). The excellent performance of FeAl-4 makes it a potentially attractive material for As(III) removal from aqueous solution. Copyright © 2016 Elsevier Ltd. All rights reserved.

An electrochemical impedance spectroscopy study of polymer electrolyte membrane fuel cells electrocatalyst single wall carbon nanohorns-supported.

PubMed

Brandão, Lúcia; Boaventura, Marta; Passeira, Carolina; Gattia, Daniele Mirabile; Marazzi, Renzo; Antisari, Marco Vittori; Mendes, Adélio

2011-10-01

Electrochemical impedance spectroscopy (EIS) was used to study the polymer electrolyte membrane fuel cells (PEMFC) performance when using single wall carbon nanohorns (SWNH) to support Pt nanoparticles. Additionally, as-prepared and oxidized SWNH Pt-supports were compared with conventional carbon black. Two different oxidizing treatments were considered: oxygen flow at 500 degrees C and reflux in an acid solution at 85 degrees C. Both oxidizing treatments increased SWNH surface area; oxygen treatment increased surface area 4 times while acid treatment increased 2.6 times. The increase in surface area should be related to the opening access to the inner tube of SWNH. Acid treatment of SWNH increased chemical fragility and decreased electrocatalyst load in comparison with as-prepared SWNH. On the other hand, the oxygen treated SWNH sample allowed to obtain the highest electrocatalyst load. The use of as-prepared and oxygen treated SWNH showed in both cases catalytic activities 60% higher than using conventional carbon black as electrocatalyst support in PEMFC. Moreover, EIS analysis indicated that the major improvement in performance is related to the cathode kinetics in the as-prepared SWNH sample, while concerning the oxidized SWNH sample, the improvements are related to the electrokinetics in both anode and cathode electrodes. These improvements should be related with differences in the hydrophobic character between SWNH and carbon black.

Pyrolytic synthesis and characterization of N-doped carbon nanoflakes for electrochemical applications

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

Savilov, S.V., E-mail: savilov@chem.msu.ru; N.S. Kurnakov Institute of General and Inorganic Chemistry Of Russian Academy of Sciences, Leninsky avenue, 31, Moscow 119991; Arkhipova, E.A.

2015-09-15

Highlights: • Carbon nanoflakes doped with nitrogen were produced by a pyrolytic technique. • Quarternary, pyrrolic and pyridinic types of nitrogen are confirmed by XPS. • Nitrogen content depends on precursor used and temperature processed. • Specific surface area values decrease with increasing of synthesis duration. • N-doped carbon nanoflakes may be suitable for electrochemical applications. - Abstract: Nitrogen doped carbon nanoflakes, which are very important for many electrochemical applications, were synthesized by pyrolysis of nitrogen containing organic compounds over metal oxide template. Acetonitrile, pyridine and butylamine, which are of different volatility were tested as N-containing precursors. Morphology, structure andmore » chemical composition of the as-synthesized materials were investigated by scanning electron microscopy (SEM), high resolution transmission electron microscopy (TEM), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). It was found that materials are highly defective and consist of a few malformed graphene layers. X-ray photoelectron spectra reflect the dominant graphitic and pyridinic N-bonding configuration. It was also noted that specific surface area depends on the duration and temperature of the reaction. Increase in duration and temperature led to decrease of the specific surface area from 1000 to 160 m{sup 2}/g, 1170 to 210 m{sup 2}/g and 1180 to 480 m{sup 2}/g for acetonitrile, butylamine and pyridine precursors, respectively.« less

Synthesis, optical properties and efficient photocatalytic activity of CdO/ZnO hybrid nanocomposite

NASA Astrophysics Data System (ADS)

Reddy, Ch Venkata; Babu, B.; Shim, Jaesool

2018-01-01

Pure CdO, ZnO and CdO/ZnO hybrid nanocomposite photocatalyst were synthesized using simple co-precipitation technique and studied in detail. The synthesized photocatalysts were characterized using several measurements such as X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), surface analysis (BET), diffuse reflectance UV-vis spectroscopy, X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, FT-IR, TG-DTA and photoluminescence (PL). The XRD results revealed that the hexagonal and cubic crystal structure of CdO and ZnO nanoparticles. The optical response for the composite showed the presence of separate absorption signature for CdO and ZnO in the visible region at about 510 nm and 360 nm respectively. The CdO/ZnO hybrid nanocomposite photocatalyst exhibited enhanced photocatalytic degradation activity compared to pristine CdO and ZnO. The enhanced photocatalytic activity may be due to the higher specific surface area and significantly reduced the electron-hole recombination rate.

Area-Selective Atomic Layer Deposition of Metal Oxides on Noble Metals through Catalytic Oxygen Activation

PubMed Central

2017-01-01

Area-selective atomic layer deposition (ALD) is envisioned to play a key role in next-generation semiconductor processing and can also provide new opportunities in the field of catalysis. In this work, we developed an approach for the area-selective deposition of metal oxides on noble metals. Using O2 gas as co-reactant, area-selective ALD has been achieved by relying on the catalytic dissociation of the oxygen molecules on the noble metal surface, while no deposition takes place on inert surfaces that do not dissociate oxygen (i.e., SiO2, Al2O3, Au). The process is demonstrated for selective deposition of iron oxide and nickel oxide on platinum and iridium substrates. Characterization by in situ spectroscopic ellipsometry, transmission electron microscopy, scanning Auger electron spectroscopy, and X-ray photoelectron spectroscopy confirms a very high degree of selectivity, with a constant ALD growth rate on the catalytic metal substrates and no deposition on inert substrates, even after 300 ALD cycles. We demonstrate the area-selective ALD approach on planar and patterned substrates and use it to prepare Pt/Fe2O3 core/shell nanoparticles. Finally, the approach is proposed to be extendable beyond the materials presented here, specifically to other metal oxide ALD processes for which the precursor requires a strong oxidizing agent for growth. PMID:29503508

Capability of insulator study by photoemission electron microscopy at SPring-8.

PubMed

Ohkochi, Takuo; Kotsugi, Masato; Yamada, Keisuke; Kawano, Kenji; Horiba, Koji; Kitajima, Fumio; Oura, Masaki; Shiraki, Susumu; Hitosugi, Taro; Oshima, Masaharu; Ono, Teruo; Kinoshita, Toyohiko; Muro, Takayuki; Watanabe, Yoshio

2013-07-01

The observation method of photoemission electron microscopy (PEEM) on insulating samples has been established in an extremely simple way. Surface conductivity is induced locally on an insulating surface by continuous radiation of soft X-rays, and Au films close to the area of interest allow the accumulated charges on the insulated area to be released to ground level. Magnetic domain observations of a NiZn ferrite, local X-ray absorption spectroscopy of sapphire, high-resolution imaging of a poorly conducting Li0.9CoO2 film surface, and Au pattern evaporation on a fine rock particle are demonstrated. Using this technique, all users' experiments on poorly conducting samples have been performed successfully at the PEEM experimental station of SPring-8.

Tip enhanced Raman spectroscopy, DFT and PED calculations of 4″-trimethylsilylethylsulfanyl-4,4‧-di(phenyleneethynylene)benzene thiol adsorbed on silver

NASA Astrophysics Data System (ADS)

Fletcher, Melissa C.; Alexson, Dimitri M.; Moore, Martin M.; Prokes, S. M.; Glembocki, Orest; Vivoni, Alberto; McCoy, Rhonda; Mishra, Soni; Tandon, Poonam; Hosten, Charles M.

2015-11-01

Monolayers of α,ω-dithiol oligo(phenyleneethynlene) molecules are critical to the field of molecular electronics because of their abilities to form bonds with many metallic surfaces and rectify current. In this study Fourier Transformation-Raman, surface-enhanced Raman scattering (SERS) spectroscopy and Tip-enhanced Raman Spectroscopy (TERS) were used to characterize a selectively oriented self-assembled monolayer of 4″-trimethylsilylethylsulfanyl-4,4‧-bis-(phenyleneethynylene)benzenethiol (OPE‧) on silver coated nanospheres. Selective orientation was achieved by synthesizing 4″-trimethylsilylethylsulfanyl-4,4‧-bis-(phenyleneethynylene)benzene disulfide, which undergoes oxidative dissociation and covalently bonds to the metal surface. The Ag coated nanosphere surfaces were characterized by scanning electron microscopy (SEM), which showed a large area of surface charging. The SERS and TERS spectra show similar results; however, a greater enhancement was achieved with the TERS relative to the SERS spectra. Assignments of vibrational bands were based on DFT calculations performed at the B3LYP level with good agreement between theoretical and experimental values. An average percent difference of 2.5 cm-1 was obtained for the non-CH stretching frequencies and a scaling factor was not applied to theoretically generated frequencies. A red shift of the ν(C-S) peak at 1087 cm-1 was observed when OPE‧ was adsorbed on a Ag surface. Vibrations specific to the trimethylsilylethyl (TMSE) group were visible in the TERS spectra, and disappear upon deprotection.

X-ray Photoelectron Spectroscopy study of CaV1-xMoxO3-δ

NASA Astrophysics Data System (ADS)

Belyakov, S. A.; Kuznetsov, M. V.; Shkerin, S. N.

2018-06-01

An investigation was carried out on perovskite-based derivatives of CaV1-xMoxO3-δ using X-ray Photoelectron Spectroscopy (XPS). According to the XRD pattern, the area of homogeneity covers the region from x = 0 to x = 0.6. Wide XPS-peaks of Ca, V, Mo and O are observed, signalling that elements are presented in multiple states. A model for explaining the large chemical shifts of XPS peaks due to different charging effects on different parts of the sample surface is proposed.

The effect of PECVD plasma decomposition on the wettability and dielectric constant changes in silicon modified DLC films for potential MEMS and low stiction applications

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

Ogwu, A. A.; Okpalugo, T. I. T.; Nanotechnology Institute, School of Electrical and Mechanical Engineering, University of Ulster, Northern Ireland

We have carried out investigations aimed at understanding the mechanism responsible for a water contact angle increase of up to ten degrees and a decrease in dielectric constant in silicon modified hydrogenated amorphous carbon films compared to unmodified hydrogenated amorphous carbon films. Our investigations based on surface chemical constituent analysis using Raman spectroscopy, x-ray photoelectron spectroscopy (XPS), SIMS, FTIR, contact angle / surface energy measurements and spectroscopic ellipsometry suggests the presence of hydrophobic chemical entities on the surface of the films. This observation is consistent with earlier theoretical plasma chemistry predictions and observed Raman peak shifts in the films. Thesemore » surface hydrophobic entities also have a lower polarizability than the bonds in the un-modified films thereby reducing the dielectric constant of the silicon modified films measured by spectroscopic ellipsometry. Ellipsometric dielectric constant measurement is directly related to the surface energy through Hamaker's constant. Our current finding is expected to be of benefit to understanding stiction, friction and lubrication in areas that range from nano-tribology to microfluidics.« less

The effect of PECVD plasma decomposition on the wettability and dielectric constant changes in silicon modified DLC films for potential MEMS and low stiction applications

NASA Astrophysics Data System (ADS)

Ogwu, A. A.; Okpalugo, T. I. T.; McLaughlin, J. A. D.

2012-09-01

We have carried out investigations aimed at understanding the mechanism responsible for a water contact angle increase of up to ten degrees and a decrease in dielectric constant in silicon modified hydrogenated amorphous carbon films compared to unmodified hydrogenated amorphous carbon films. Our investigations based on surface chemical constituent analysis using Raman spectroscopy, x-ray photoelectron spectroscopy (XPS), SIMS, FTIR, contact angle / surface energy measurements and spectroscopic ellipsometry suggests the presence of hydrophobic chemical entities on the surface of the films. This observation is consistent with earlier theoretical plasma chemistry predictions and observed Raman peak shifts in the films. These surface hydrophobic entities also have a lower polarizability than the bonds in the un-modified films thereby reducing the dielectric constant of the silicon modified films measured by spectroscopic ellipsometry. Ellipsometric dielectric constant measurement is directly related to the surface energy through Hamaker's constant. Our current finding is expected to be of benefit to understanding stiction, friction and lubrication in areas that range from nano-tribology to microfluidics.

Spectroscopic Study of the Thermal Degradation of PVP-capped Rh and Pt Nanoparticles in H2 and O2 Environments

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

Borodko, Yuri; Lee, Hyun Sook; Joo, Sang Hoon

2009-09-15

Poly(N-vinylpyrrolidone) (PVP) capped platinum and rhodium nanoparticles (7-12 nm) have been studied with UV-VIS, FTIR and Raman spectroscopy. The absorption bands in the region 190-900 nm are shown to be sensitive to the electronic structure of surface Rh and Pt atoms as well as to the aggregation of the nanoparticles. In-situ FTIR-DRIFT spectroscopy of the thermal decay of PVP stabilized Rh and Pt nanoparticles in H{sub 2} and O{sub 2} atmospheres in temperatures ranging from 30 C-350 C reveal that decomposition of PVP above 200 C, PVP transforms into a 'polyamidpolyene' - like material that is in turn converted intomore » a thin layer of amorphous carbon above 300 C. Adsorbed carbon monoxide was used as a probing molecule to monitor changes of electronic structure of surface Rh and Pt atoms and accessible surface area. The behavior of surface Rh and Pt atoms with ligated CO and amide groups of pyrrolidones resemble that of surface coordination compounds.« less

Motion Trajectories for Wide-area Surveying with a Rover-based Distributed Spectrometer

NASA Technical Reports Server (NTRS)

Tunstel, Edward; Anderson, Gary; Wilson, Edmond

2006-01-01

A mobile ground survey application that employs remote sensing as a primary means of area coverage is highlighted. It is distinguished from mobile robotic area coverage problems that employ contact or proximity-based sensing. The focus is on a specific concept for performing mobile surveys in search of biogenic gases on planetary surfaces using a distributed spectrometer -- a rover-based instrument designed for wide measurement coverage of promising search areas. Navigation algorithms for executing circular and spiral survey trajectories are presented for widearea distributed spectroscopy and evaluated based on area covered and distance traveled.

Paramagnetic iron-doped hydroxyapatite nanoparticles with improved metal sorption properties. A bioorganic substrates-mediated synthesis.

PubMed

Mercado, D Fabio; Magnacca, Giuliana; Malandrino, Mery; Rubert, Aldo; Montoneri, Enzo; Celi, Luisella; Bianco Prevot, Alessandra; Gonzalez, Mónica C

2014-03-26

This paper describes the synthesis of paramegnetic iron-containing hydroxyapatite nanoparticles and their increased Cu(2+) sorbent capacity when using Ca(2+) complexes of soluble bioorganic substrates from urban wastes as synthesis precursors. A thorough characterization of the particles by TEM, XRD, FTIR spectroscopy, specific surface area, TGA, XPS, and DLS indicates that loss of crystallinity, a higher specific area, an increased surface oxygen content, and formation of surface iron phases strongly enhance Cu(2+) adsorption capacity of hydroxyapatite-based materials. However, the major effect of the surface and morphologycal modifications is the size diminution of the aggregates formed in aqueous solutions leading to an increased effective surface available for Cu(2+) adsorption. Maximum sorption values of 550-850 mg Cu(2+) per gram of particles suspended in an aqueous solution at pH 7 were determined, almost 10 times the maximum values observed for hydroxyapatite nanoparticles suspensions under the same conditions.

Degradation of all-vanadium redox flow batteries (VRFB) investigated by electrochemical impedance and X-ray photoelectron spectroscopy: Part 2 electrochemical degradation

NASA Astrophysics Data System (ADS)

Derr, Igor; Bruns, Michael; Langner, Joachim; Fetyan, Abdulmonem; Melke, Julia; Roth, Christina

2016-09-01

Electrochemical degradation (ED) of carbon felt electrodes was investigated by cycling of a flow through all-vanadium redox flow battery (VRFB) and conducting half-cell measurements with two reference electrodes inside the test bench. ED was detected using half-cell and full-cell electrochemical impedance spectroscopy (EIS) at different states of charge (SOC). Reversing the polarity of the battery to recover cell performance was performed with little success. Renewing the electrolyte after a certain amount of cycles restored the capacity of the battery. X-ray photoelectron spectroscopy (XPS) reveals that the amount of surface functional increases by more than a factor of 3 for the negative side as well as for the positive side. Scanning electron microscope (SEM) images show a peeling of the fiber surface after cycling the felts, which leads to a loss of electrochemically active surface area (ECSA). Long term cycling shows that ED has a stronger impact on the negative half-cell [V(II)/V(III)] than the positive half-cell [V(IV)/V(V)] and that the negative half-cell is the rate-determining half-cell for the VRFB.

Fabrication of graphene/titanium carbide nanorod arrays for chemical sensor application.

PubMed

Fu, Chong; Li, Mingji; Li, Hongji; Li, Cuiping; Qu, Changqing; Yang, Baohe

2017-03-01

Vertically stacked graphene nanosheet/titanium carbide nanorod array/titanium (graphene/TiC nanorod array) wires were fabricated using a direct current arc plasma jet chemical vapor deposition (DC arc plasma jet CVD) method. The graphene/TiC nanorod arrays were characterized by scanning electron microscopy, transmission electron microscopy, Raman spectroscopy, X-ray photoelectron spectroscopy, and X-ray diffraction spectroscopy. The TiO 2 nanotube array was reduced to the TiC nanorod array, and using those TiC nanorods as nucleation sites, the vertical graphene layer was formed on the TiC nanorod surface. The multi-target response mechanisms of the graphene/TiC nanorod array were investigated for ascorbic acid (AA), dopamine (DA), uric acid (UA), and hydrochlorothiazide (HCTZ). The vertically stacked graphene sheets facilitated the electron transfer and reactant transport with a unique porous surface, high surface area, and high electron transport network of CVD graphene sheets. The TiC nanorod array facilitated the electron transfer and firmly held the graphene layer. Thus, the graphene/TiC nanorod arrays could simultaneously respond to trace biomarkers and antihypertensive drugs. Copyright © 2016 Elsevier B.V. All rights reserved.

Fabrication of large area plasmonic nanoparticle grating structure on silver halide based transmission electron microscope film and its application as a surface enhanced Raman spectroscopy substrate

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

Sudheer,, E-mail: sudheer@rrcat.gov.in; Tiwari, P.; Singh, M. N.

The plasmonic responses of silver nanoparticle grating structures of different periods made on silver halide based electron microscope film are investigated. Raster scan of the conventional scanning electron microscope (SEM) is used to carry out electron beam lithography for fabricating the plasmonic nanoparticle grating (PNG) structures. Morphological characterization of the PNG structures, carried out by the SEM and the atomic force microscope, indicates that the depth of the groove decreases with a decrease in the grating period. Elemental characterization performed by the energy dispersive spectroscopy and the x-ray diffraction shows the presence of nanoparticles of silver in the PNG grating.more » The optical characterization of the gratings shows that the localized surface plasmon resonance peak shifts from 366 to 378 nm and broadens with a decrease in grating period from 10 to 2.5 μm. The surface enhanced Raman spectroscopy of the Rhodamine-6G dye coated PNG structure shows the maximum enhancement by two orders of magnitude in comparison to the randomly distributed silver nanoparticles having similar size and shape as the PNG structure.« less

Investigation of biomineralization by Raman spectroscopy

NASA Astrophysics Data System (ADS)

Fatscher, Robert William

Biomineralization is a process in which living organism grow composite materials consisting of inorganic and organic materials. This produces a composite material consisting of both inorganic and organic components, with superior mechanical properties. In the human body bone and dentin are both examples of biominerals. In this research Raman spectroscopy was used to characterize dentin from mice and human teeth, to determine composition. In the mouse tooth samples areas of irregular dentin were found, along the inside of the tooth, to be in the process of mineralization. By analyzing the samples along these areas we were able to determine the composition of dentin and track how it changed in these area. By analysis of the mineral to matrix ratio the areas of irregular dentin were determined to have less mineral present. Observations of other organic components and collagen in increased concentrations in this area suggested these area were in the process of biomineralization. The understanding of the structure of dentin and its biomineralization process is of crucial importance when trying reproduce dentin. Scientists and engineers are able to produce dentin minerals in vitro by culturing various dental stem cells. The ability to create dentin mineral from cells could lead to methods of repairing dentin in patients, or even lead to the creation of a completely engineered tooth. While dentin-like materials can be produced in a laboratory environment, analysis and comparison of the composition of these materials must be performed to ensure the mineral produced is consistent with dentin. Mineralized nodules from six different dental stem cell lines were cultured to produce a mineralized deposit. Utilizing Raman spectroscopy, we were able to determine cell source dependent differences in a variety of dental stem cells, and compare the mineral produced to native dentin. Orthopedic implants are implants used to replace damaged bone, examples include knee, hip and dental implants. These implants are designed to osteointegrate with the native healthy tissues in order to create a functionally stable and structural interface. Biomaterials such as hydroxyapatite and titania are known to increase the rate of bone regeneration in vivo.1 By accelerating the early response of bone forming cells to these implants, better fixation is achieved between the implant and the bone, shortening recovery times and increasing the viability of these implants. In the last part of this research an investigation of osteoblasts cultured at 14 days on five different heat-treated titania substrates was investigated by Raman spectroscopy, in order to observe the initial cellular response to the titania substrates. The heat-treatment of titania changes the amount of oxygen on it's surface which in turn effects the surface energy. A change in the surface energy of a material will affect the cellular response, by culturing cells on various heat-treated titania substrates a relationship between the surface energy and cellular response can be investigated. A faster cellular response would lead to an increased rate of bone regeneration shortening healing times and allowing for better fixation of the implant.

Sonochemical fabrication of fluorinated mesoporous titanium dioxide microspheres

NASA Astrophysics Data System (ADS)

Yu, Changlin; Yu, Jimmy C.; Chan, Mui

2009-05-01

A sonochemical-hydrothermal method for preparing fluorinated mesoporous TiO 2 microspheres was developed. Formation of mesoporous TiO 2 and doping of fluorine was achieved by sonication and then hydrothermal treatment of a solution containing titanium isopropoxide, template, and sodium fluoride. The as-synthesized TiO 2 microspheres were characterized by X-ray diffraction (XRD), Fourier translation infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray (EDX) spectroscopy, photoluminescence spectroscopy (PL), and BET surface areas. The P123 template was removed completely during the hydrothermal and washing steps, which was different from the conventional calcination treatment. The as- synthesized TiO 2 microspheres had good crystallinity and high stability. Results from the photocatalytic degradation of methylene blue (MB) showed that fluorination could remarkably improve the photocatalytic activity of titanium dioxide.

Surface characterization of stainless HP-40 steel using laser induced μ-breakdown spectroscopy (μ -LIBS)

NASA Astrophysics Data System (ADS)

Pinto, M.; Calderón, X.; Mejía Ospino, E.; Cabanzo, R.; Poveda, Juan C.

2016-02-01

In the present study, optical microscopy in stereoscopic mode coupled to laser- induced p-breakdown spectroscopy (μ-LIBS) was applied for analysing HP-40 steel samples. microLIBS (μ-LIBS) is a new growing area that employs low energy laser pulses for the generation of plasma emission, which allow the realization of localized microanalysis [1]. This new LIBS instrument was used for the surface characterization of the steel samples in the spectral range from 356 to 401nm. Elements such as Cr, Ni, Fe, Nb, Pb, Mo, C, Mn and Si in the steel samples were investigated. The results allowed the construction of elemental distribution profiles of the samples. Complementary the HP-40 steel samples were superficially characterized by Scanning Electron Microscope (SEM).

Tetracyanoethylene oxide-functionalized graphene and graphite characterized by Raman and Auger spectroscopy

DOE PAGES

Frolova, Liliya V.; Magedov, Igor V.; Harper, Aaron; ...

2014-09-28

The tetracyanoethylene oxide (TCNEO) functionalization of chemical vapor deposition grown large area graphene and graphite was performed using reaction of TCNEO with carbon surface in chlorobenzene. The successful functionalization has been confirmed by Raman and Auger spectroscopy, and by numerical modeling of the structure and vibrational modes of TCNEO-functionalized graphene. Raman spectra of TCNEO-functionalized graphene and graphite show several groups of lines corresponding to vibrations of attached carbonyl ylide. Lastly, one of key signatures of TCNEO attachment is the high intensity Raman band at ~1450 cm ₋1, which represents the C-C=C in plane vibrations in functionalization-distorted graphene. We find Ramanmore » spectra indicate the existence of central (pristine) attachment of TCNEO to graphene surface.« less

A doped activated carbon prepared from polyaniline for high performance supercapacitors

NASA Astrophysics Data System (ADS)

Li, Limin; Liu, Enhui; Li, Jian; Yang, Yanjing; Shen, Haijie; Huang, Zhengzheng; Xiang, Xiaoxia; Li, Wen

A novel doped activated carbon has been prepared from H 2SO 4-doped polyaniline which is prepared by the oxypolymerization of aniline. The morphology, surface chemical composition and surface area of the carbon have been investigated by scanning electron microscope, X-ray photoelectron spectroscopy and Brunaner-Emmett-Teller measurement, respectively. Electrochemical properties of the doped activated carbon have been studied by cyclic voltammograms, galvanostatic charge/discharge, and electrochemical impedance spectroscopy measurements in 6 mol l -1 KOH. The specific capacitance of the carbon is as high as 235 F g -1, the specific capacitance hardly decreases at a high current density 11 A g -1 after 10,000 cycles, which indicates that the carbon possesses excellent cycle durability and may be a promising candidate for supercapacitors.

Development of a neurofeedback protocol targeting the frontal pole using near-infrared spectroscopy.

PubMed

Kinoshita, Akihide; Takizawa, Ryu; Yahata, Noriaki; Homae, Fumitaka; Hashimoto, Ryuichiro; Sakakibara, Eisuke; Kawasaki, Shingo; Nishimura, Yukika; Koike, Shinsuke; Kasai, Kiyoto

2016-11-01

Neurofeedback has been studied with the aim of controlling cerebral activity. Near-infrared spectroscopy is a non-invasive neuroimaging technique used for measuring hemoglobin concentration changes in cortical surface areas with high temporal resolution. Thus, near-infrared spectroscopy may be useful for neurofeedback, which requires real-time feedback of repeated brain activation measurements. However, no study has specifically targeted neurofeedback, using near-infrared spectroscopy, in the frontal pole cortex. We developed an original near-infrared spectroscopy neurofeedback system targeting the frontal pole cortex. Over a single day of testing, each healthy participant (n = 24) received either correct or incorrect (Sham) feedback from near-infrared spectroscopy signals, based on a crossover design. Under correct feedback conditions, significant activation was observed in the frontal pole cortex (P = 0.000073). Additionally, self-evaluation of control and metacognitive beliefs were associated with near-infrared spectroscopy signals (P = 0.006). The neurofeedback system developed in this study might be useful for developing control of frontal pole cortex activation. © 2016 The Authors. Psychiatry and Clinical Neurosciences © 2016 Japanese Society of Psychiatry and Neurology.

Solvent free tin oxide nanoparticle for gas sensing application

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

Ranjan, Pranay, E-mail: pranjan@iitp.ac.in; Thakur, Ajay D.; Centre for Energy and Environment, Indian Institute of Technology Patna, Patliputra, Patna 800013 India

2016-05-06

A new modified technique of synthesizing tin oxide nanoparticles with crystallite size of 2 nm to 6 nm has been developed. Surface area of the nanoparticle has been increased as we approached towards the Debye length. Such a techniques for approaching the Debye length is expected to bring remarkable changes in the properties of resistive based gas sensors. The technique used here is less toxic, economical and has high yield. Phase purity, size, shape and composition has been investigated using x-ray diffraction, micro Raman, scanning electron microscopy and energy dispersive x ray spectroscopy. While surface area has been calculated through Brunaur-Emmett-Teller (BET).

Conversion of nuclear waste to molten glass: Formation of porous amorphous alumina in a high-Al melter feed

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

Xu, Kai; Hrma, Pavel; Washton, Nancy

The transition of Al phases in a simulated high-Al high-level nuclear waste melter feed heated at 5 K min-1 to 700°C was investigated with transmission electron microscopy, 27Al nuclear magnetic resonance spectroscopy, the Brunauer-Emmett-Teller method, and X-ray diffraction. At temperatures between 300 and 500°C, porous amorphous alumina formed from the dehydration of gibbsite, resulting in increased specific surface area of the feed (~8 m2 g-1). The high-surface-area amorphous alumina formed in this manner could potentially stop salt migration in the cold cap during nuclear waste vitrification.

Characterization of Nanoencapsulated Centella asiatica and Zingiber officinale Extract Using Combination of Malto Dextrin and Gum Arabic as Matrix

NASA Astrophysics Data System (ADS)

Meliana, Y.; Harmami, S. B.; Restu, W. K.

2017-02-01

This research investigated nanoencapsulation of Centella asiatica and Zingiber officinale extract. The encapsulated extract was used as a complex matrix of multi-layered interfacial membranes between malto dextrin and gum Arabic. Characterization of nanoencapsulation using Transmission Electron Microscope (TEM), Fourier Transform Infrared Spectroscopy (FTIR) and BET surface area (SA) showed the morphology, functional group and cumulative adsorption in the surface area of pores. The TEM image of the nanoencapsulated powders of Centella asiatica and Zingiber officinale extract showed a nearly spherical shape with the particle size of 664 nm from its average radius.

Voxel-based measurement sensitivity of spatially resolved near-infrared spectroscopy in layered tissues

NASA Astrophysics Data System (ADS)

Niwayama, Masatsugu

2018-03-01

We quantitatively investigated the measurement sensitivity of spatially resolved spectroscopy (SRS) across six tissue models: cerebral tissue, a small animal brain, the forehead of a fetus, an adult brain, forearm muscle, and thigh muscle. The optical path length in the voxel of the model was analyzed using Monte Carlo simulations. It was found that the measurement sensitivity can be represented as the product of the change in the absorption coefficient and the difference in optical path length in two states with different source-detector distances. The results clarified the sensitivity ratio between the surface layer and the deep layer at each source-detector distance for each model and identified changes in the deep measurement area when one of the detectors was close to the light source. A comparison was made with the results from continuous-wave spectroscopy. The study also identified measurement challenges that arise when the surface layer is inhomogeneous. Findings on the measurement sensitivity of SRS at each voxel and in each layer can support the correct interpretation of measured values when near-infrared oximetry or functional near-infrared spectroscopy is used to investigate different tissue structures.

Magnetic field controlled graphene oxide-based origami with enhanced surface area and mechanical properties.

PubMed

Park, Ok-Kyung; Tiwary, Chandra Sekhar; Yang, Yang; Bhowmick, Sanjit; Vinod, Soumya; Zhang, Qingbo; Colvin, Vicki L; Asif, S A Syed; Vajtai, Robert; Penev, Evgeni S; Yakobson, Boris I; Ajayan, Pulickel M

2017-06-01

One can utilize the folding of paper to build fascinating 3D origami architectures with extraordinary mechanical properties and surface area. Inspired by the same, the morphology of 2D graphene can be tuned by addition of magnetite (Fe 3 O 4 ) nanoparticles in the presence of a magnetic field. The innovative 3D architecture with enhanced mechanical properties also shows a high surface area (∼2500 m 2 g -1 ) which is utilized for oil absorption. Detailed microscopy and spectroscopy reveal rolling of graphene oxide (GO) sheets due to the magnetic field driven action of magnetite particles, which is further supported by molecular dynamics (MD) simulations. The macroscopic and local deformation resulting from in situ mechanical loading inside a scanning electron microscope reveals a change in the mechanical response due to a change internal morphology, which is further supported by MD simulation.

Structural characteristics of biochar-graphene nanosheet composites and their adsorption performance for phthalic acid esters

NASA Astrophysics Data System (ADS)

Ghaffar, Abdul; Zhu, Xiaoying; Chen, Baoliang

2017-04-01

The nonuniform and unhomogenous structure of biochar including defects could affect the adsorption performance of biochars. Biochar and graphene nanosheet (GNS) composites (BG) were prepared by simple dip coating method following thermal route of bamboo wood biomass at three different temperatures (300, 500, 700°C), in addition to biochars. The morphology and structural composition of biochars and BG composites were examined by scanning electron microscopy, transmission electron microscopy, Brunauer-Emmet-Teller surface area with N2 and CO2, Raman spectroscopy, Fourier Transformed Infrared spectroscopy, X-ray Photoelectron spectroscopy, Thermogravimetric analysis and CHN elemental analysis. It was found that GNS ( 1µm, 0.1% mass) provided higher thermal stability, porous structure, and relatively higher surface area (N2 and CO2), to BG composites. BG composites portrayed the existence of GNS bearing cavities and evidently increased the graphitic structure. The adsorption capabilities of biochars and BG composites towards dimethyl phthalate (DMP), diethyl phthalate (DEP), and dibutyl phthalate (DBP) as model phthalic acid esters (PAEs) were examined by batch sorption technique. The BG composites exhibited the increased adsorption capacity comparatively to biochars. The aromatic sheets of biochars and GNS on biochars dominated the π-π EDA (electron donor-acceptor) interaction for ring structure of DMP molecule in addition to pore-diffusion mechanism, whereas adsorption of DBP was attributed to hydrophobicity. Our results suggest that surface composition and morphology of biochars can be regulated with GNS and may enhance their adsorption capacity, thus could be considered for effective environmental remediation of various organic contaminants.

Fabrication of hollow boron-doped diamond nanostructure via electrochemical corrosion of a tungsten oxide template.

PubMed

Lim, Young-Kyun; Lee, Eung-Seok; Lee, Choong-Hyun; Lim, Dae-Soon

2018-08-10

In the study, a hollow boron-doped diamond (BDD) nanostructure electrode is fabricated to increase the reactive surface area for electrochemical applications. Tungsten oxide nanorods are deposited on the silicon substrate as a template by the hot filament chemical vapor deposition (HFCVD) method. The template is coated with a 100 nm BDD layer deposited by HFCVD to form a core-shell nanostructure. The WO x core is finally electrochemically dissolved to form hollow BDD nanostructure. The fabricated hollow BDD nanostructure electrode is investigated via scanning electron microscopy, transmission electron microscopy, and Raman spectroscopy. The specific surface areas of the electrodes were analyzed and compared by using Brunauer-Emmett-Teller method. Furthermore, cyclic voltammetry and chronocoulometry are used to investigate the electrochemical characteristics and the reactive surface area of the as-prepared hollow BDD nanostructure electrode. A hollow BDD nanostructure electrode exhibits a reactive area that is 15 times that of a planar BDD thin electrode.

Large Area Atomically Flat Surfaces via Exfoliation of Bulk Bi 2Se 3 Single Crystals

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

Melamed, Celeste L.; Ortiz, Brenden R.; Gorai, Prashun

In this paper, we present an exfoliation method that produces cm 2-area atomically flat surfaces from bulk layered single crystals, with broad applications such as for the formation of lateral heterostructures and for use as substrates for van der Waals epitaxy. Single crystals of Bi 2Se 3 were grown using the Bridgman method and examined with X-ray reciprocal space maps, Auger spectroscopy, low-energy electron diffraction, and X-ray photoelectron spectroscopy. An indium-bonding exfoliation technique was developed that produces multiple ~100 um thick atomically flat, macroscopic (>1 cm 2) slabs from each Bi 2Se 3 source crystal. Two-dimensional X-ray diffraction and reciprocalmore » space maps confirm the high crystalline quality of the exfoliated surfaces. Atomic force microscopy reveals that the exfoliated surfaces have an average root-mean-square (RMS) roughness of ~0.04 nm across 400 μm 2 scans and an average terrace width of 70 um between step edges. First-principles calculations reveal exfoliation energies of Bi 2Se 3 and a number of other layered compounds, which demonstrate relevance of our method across the field of 2D materials. While many potential applications exist, excellent lattice matching with the III-V alloy space suggests immediate potential for the use of these exfoliated layered materials as epitaxial substrates for photovoltaic development.« less

La and Al co-doped CaMnO 3 perovskite oxides: From interplay of surface properties to anion exchange membrane fuel cell performance

DOE PAGES

Dzara, Michael J.; Christ, Jason M.; Joghee, Prabhuram; ...

2017-09-01

This work reports the first account of perovskite oxide and carbon composite oxygen reduction reaction (ORR) catalysts integrated into anion exchange membrane fuel cells (AEMFCs). Perovskite oxides with a theoretical stoichiometry of Ca 0.9La 0.1Al 0.1Mn 0.9O 3-δ are synthesized by an aerogel method and calcined at various temperatures, resulting in a set of materials with varied surface chemistry and surface area. Material composition is evaluated by X-ray diffraction, energy dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy. The perovskite oxide calcined at 800 degrees C shows the importance of balance between surface area, purity of the perovskite phase, and surfacemore » composition, resulting in the highest ORR mass activity when evaluated in rotating disk electrodes. Integration of this catalyst into AEMFCs reveals that the best AEMFC performance is obtained when using composites with 30:70 perovskite oxide:carbon composition. Doubling the loading leads to an increase in the power density from 30 to 76 mW cm -2. The AEMFC prepared with a composite based on perovskite oxide and N-carbon achieves a power density of 44 mW cm -2, demonstrating an ~50% increase when compared to the highest performing composite with undoped carbon at the same loading.« less

Large Area Atomically Flat Surfaces via Exfoliation of Bulk Bi 2Se 3 Single Crystals

DOE PAGES

Melamed, Celeste L.; Ortiz, Brenden R.; Gorai, Prashun; ...

2017-09-12

In this paper, we present an exfoliation method that produces cm 2-area atomically flat surfaces from bulk layered single crystals, with broad applications such as for the formation of lateral heterostructures and for use as substrates for van der Waals epitaxy. Single crystals of Bi 2Se 3 were grown using the Bridgman method and examined with X-ray reciprocal space maps, Auger spectroscopy, low-energy electron diffraction, and X-ray photoelectron spectroscopy. An indium-bonding exfoliation technique was developed that produces multiple ~100 um thick atomically flat, macroscopic (>1 cm 2) slabs from each Bi 2Se 3 source crystal. Two-dimensional X-ray diffraction and reciprocalmore » space maps confirm the high crystalline quality of the exfoliated surfaces. Atomic force microscopy reveals that the exfoliated surfaces have an average root-mean-square (RMS) roughness of ~0.04 nm across 400 μm 2 scans and an average terrace width of 70 um between step edges. First-principles calculations reveal exfoliation energies of Bi 2Se 3 and a number of other layered compounds, which demonstrate relevance of our method across the field of 2D materials. While many potential applications exist, excellent lattice matching with the III-V alloy space suggests immediate potential for the use of these exfoliated layered materials as epitaxial substrates for photovoltaic development.« less

Nb2O5 nanowires in-situ grown on carbon fiber: A high-efficiency material for the photocatalytic reduction of Cr(VI).

PubMed

Du, Yucheng; Zhang, Shihao; Wang, Jinshu; Wu, Junshu; Dai, Hongxing

2018-04-01

Niobium oxide nanowire-deposited carbon fiber (CF) samples were prepared using a hydrothermal method with amorphous Nb 2 O 5 ·nH 2 O as precursor. The physical properties of the samples were characterized by means of numerous techniques, including X-ray diffraction (XRD), energy-dispersive spectroscopy (EDS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected-area electron diffraction (SAED), UV-visible spectroscopy (UV-vis), N 2 adsorption-desorption, Fourier transform infrared spectroscopy (FT-IR), and X-ray photoelectron spectroscopy. The efficiency for the removal of Cr(VI) was determined. Parameters such as pH value and initial Cr(VI) concentration could influence the Cr(VI) removal efficiency or adsorption capacity of the Nb 2 O 5 /carbon fiber sample obtained after hydrothermal treatment at 160°C for 14hr. The maximal Cr(VI) adsorption capacity of the Nb 2 O 5 nanowire/CF sample was 115mg/g. This Nb 2 O 5 /CF sample also showed excellent photocatalytic activity and stability for the reduction of Cr(VI) under UV-light irradiation: the Cr(VI) removal efficiency reached 99.9% after UV-light irradiation for 1hr and there was no significant decrease in photocatalytic performance after the use of the sample for 10 repeated cycles. Such excellent Cr(VI) adsorption capacity and photocatalytic performance was related to its high surface area, abundant surface hydroxyl groups, and good UV-light absorption ability. Copyright © 2017. Published by Elsevier B.V.

Electrolyte-induced surface transformation and transition-metal dissolution of fully delithiated LiNi 0.8Co 0.15Al 0.05O 2

DOE PAGES

Faenza, Nicholas V.; Lebens-Higgins, Zachary W.; Mukherjee, Pinaki; ...

2017-06-08

Here, enabling practical utilization of layered Rmore » $$\\bar{3}$$ m positive electrodes near full delithiation requires an enhanced understanding of the complex electrode–electrolyte interactions that often induce failure. Using Li[Ni 0.8Co 0.15Al 0.05]O 2 (NCA) as a model layered compound, the chemical and structural stability in a strenuous thermal and electrochemical environment was explored. Operando microcalorimetry and electrochemical impedance spectroscopy identified a fingerprint for a structural decomposition and transition-metal dissolution reaction that occurs on the positive electrode at full delithiation. Surface-sensitive characterization techniques, including X-ray absorption spectroscopy and high-resolution transmission electron microscopy, measured a structural and morphological transformation of the surface and subsurface regions of NCA. Despite the bulk structural integrity being maintained, NCA surface degradation at a high state of charge induces excessive transition-metal dissolution and significant positive electrode impedance development, resulting in a rapid decrease in electrochemical performance. Additionally, the impact of electrolyte salt, positive electrode surface area, and surface Li 2CO 3 content on the magnitude and character of the dissolution reaction was studied.« less

Electrolyte-Induced Surface Transformation and Transition-Metal Dissolution of Fully Delithiated LiNi0.8Co0.15Al0.05O2.

PubMed

Faenza, Nicholas V; Lebens-Higgins, Zachary W; Mukherjee, Pinaki; Sallis, Shawn; Pereira, Nathalie; Badway, Fadwa; Halajko, Anna; Ceder, Gerbrand; Cosandey, Frederic; Piper, Louis F J; Amatucci, Glenn G

2017-09-19

Enabling practical utilization of layered R3̅m positive electrodes near full delithiation requires an enhanced understanding of the complex electrode-electrolyte interactions that often induce failure. Using Li[Ni 0.8 Co 0.15 Al 0.05 ]O 2 (NCA) as a model layered compound, the chemical and structural stability in a strenuous thermal and electrochemical environment was explored. Operando microcalorimetry and electrochemical impedance spectroscopy identified a fingerprint for a structural decomposition and transition-metal dissolution reaction that occurs on the positive electrode at full delithiation. Surface-sensitive characterization techniques, including X-ray absorption spectroscopy and high-resolution transmission electron microscopy, measured a structural and morphological transformation of the surface and subsurface regions of NCA. Despite the bulk structural integrity being maintained, NCA surface degradation at a high state of charge induces excessive transition-metal dissolution and significant positive electrode impedance development, resulting in a rapid decrease in electrochemical performance. Additionally, the impact of electrolyte salt, positive electrode surface area, and surface Li 2 CO 3 content on the magnitude and character of the dissolution reaction was studied.

The effect of surface charge on photocatalytic degradation of methylene blue dye using chargeable titania nanoparticles.

PubMed

Azeez, Fadhel; Al-Hetlani, Entesar; Arafa, Mona; Abdelmonem, Yasser; Nazeer, Ahmed Abdel; Amin, Mohamed O; Madkour, Metwally

2018-05-08

Herein, a simple approach based on tailoring the surface charge of nanoparticles, NPs, during the preparation to boost the electrostatic attraction between NPs and the organic pollutant was investigated. In this study, chargeable titania nanoparticles (TiΟ 2 NPs) were synthesized via a hydrothermal route under different pH conditions (pH = 1.6, 7.0 and 10). The prepared TiΟ 2 NPs were fully characterized via various techniques including; transmission electron microscopy (TEM), X-ray diffraction (XRD), N 2 adsorption/desorption, X-ray photoelectron spectroscopy (XPS), Ultraviolet-visible spectroscopy (UV-Vis) and dynamic light scattering (DLS). The influence of the preparation pH on the particle size, surface area and band gap was investigated and showed pH-dependent behavior. The results revealed that upon increasing the pH value, the particle size decreases and lead to larger surface area with less particles agglomeration. Additionally, the effect of pH on the surface charge was monitored by XPS to determine the amount of hydroxyl groups on the TiO 2 NPs surface. Furthermore, the photocatalytic activity of the prepared TiΟ 2 NPs towards methylene blue (MB) photodegradation was manifested. The variation in the preparation pH affected the point of zero charge (pH PZC ) of TiO 2 NPs, subsequently, different photocatalytic activities based on electrostatic interactions were observed. The optimum efficiency obtained was 97% at a degradation rate of 0.018 min -1 using TiO 2 NPs prepared at pH 10.

Auger Spectroscopy Analysis of Spalled LEU-10Mo Foils

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

Lawrence, Samantha Kay; Schulze, Roland K.

2017-08-03

Presentation includes slides on Surface Science used to probe LEU-10Mo Spall; Auger highlights graphitic-like inclusions and Mo-deficient oxide on base metal; Higher C concentration detected within spall area Images Courtesy; Depth profiling reveals thick oxide; Mo concentration nears nominal only at depths ~400 nm; and lastly Key Findings.

Large area substrate for surface enhanced Raman spectroscopy (SERS) using glass-drawing technique

DOEpatents

Ivanov, Ilia N; Simpson, John T

2012-06-26

A method of making a large area substrate comprises drawing a plurality of tubes to form a plurality of drawn tubes, and cutting the plurality of drawn tubes into cut drawn tubes. Each cut drawn tube has a first end and a second end along the longitudinal direction of the respective cut drawn tube. The cut drawn tubes collectively have a predetermined periodicity. The method of making a large area substrate also comprises forming a metal layer on the first ends of the cut drawn tubes to provide a large area substrate.

Three-dimensional interconnected porous graphitic carbon derived from rice straw for high performance supercapacitors

NASA Astrophysics Data System (ADS)

Jin, Hong; Hu, Jingpeng; Wu, Shichao; Wang, Xiaolan; Zhang, Hui; Xu, Hui; Lian, Kun

2018-04-01

Three-dimensional interconnected porous graphitic carbon materials are synthesized via a combination of graphitization and activation process with rice straw as the carbon source. The physicochemical properties of the three-dimensional interconnected porous graphitic carbon materials are characterized by Nitrogen adsorption/desorption, Fourier-transform infrared spectroscopy, X-ray diffraction, Raman spectroscopy, Scanning electron microscopy and Transmission electron microscopy. The results demonstrate that the as-prepared carbon is a high surface area carbon material (a specific surface area of 3333 m2 g-1 with abundant mesoporous and microporous structures). And it exhibits superb performance in symmetric double layer capacitors with a high specific capacitance of 400 F g-1 at a current density of 0.1 A g-1, good rate performance with 312 F g-1 under a current density of 5 A g-1 and favorable cycle stability with 6.4% loss after 10000 cycles at a current density of 5 A g-1 in the aqueous electrolyte of 6M KOH. Thus, rice straw is a promising carbon source for fabricating inexpensive, sustainable and high performance supercapacitors' electrode materials.

Synthesis of graphene aerogel for adsorption of bisphenol A

NASA Astrophysics Data System (ADS)

Trinh, Truong Thi Phuong Nguyet Xuan; Long, Nguyen Huynh Bach Son; Quang, Dong Thanh; Hieu, Nguyen Huu

2018-04-01

In this research, graphene aerogel (GA) was synthesized by chemical reduction method using ethylene diamine as a reducing agent. The morphology and properties of GA were characterized by calculating apparent density, Fourier transform infrared spectroscopy, X-ray diffraction, Raman spectroscopy, field emission scanning electron microscopy, and Brunauer-Emmett-Teller (BET) specific surface area. High-performance liquid chromatography (HPLC) was used to quantify the amount of the residual bisphenol A (BPA) concentration. The analysis results showed that GA exhibited low density ranging from 4-8 mg/cm3, hydrophobicity, high porosity, and specific surface area of 1883 m2/g according to BET. The obtained GA was used as an adsorbent for BPA. The effects of pH, contact time, and initial BPA concentration on the adsorption were investigated. The adsorption equilibrium time could be reached within 240 minutes. The adsorption data were well-fitted to pseudo-second-order kinetic equation and Langmuir isotherm model. The maximum adsorption capacity of GA for BPA calculated by the Langmuir model was 185.185 mg/g at pH 7. Accordingly, GA could be considered as promising adsorbents for BPA in water.

Limitations of using Raman microscopy for the analysis of high-content-carbon-filled ethylene propylene diene monomer rubber.

PubMed

Ghanbari-Siahkali, Afshin; Almdal, Kristoffer; Kingshott, Peter

2003-12-01

The effects of laser irradiation on changes to the surface chemistry and structure of a commercially available ethylene propylene diene monomer (EPDM) rubber sample after Raman microscopy analysis was investigated. The Raman measurements were carried out with different levels of laser power on the sample, ranging from 4.55 mW to 0.09 mW. The surface of the EPDM was analyzed before and after laser exposure using X-ray photoelectron spectroscopy (XPS) and attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy. The techniques have surface probe depths of approximately < or = 10 nm and 1 microm, respectively. Both sets of analysis show that ingredients of the blended EPDM rubber "bloom" to the surface as a result of local heating that takes place due to the absorption of laser by carbon black during the Raman analysis. Scanning electron microscopy (SEM) analysis was also performed on the Raman analyzed areas to visually illustrate the effects created due to laser light exposure (i.e., burning marks). The change in surface chemistry also occurs in regions a few millimeters from the exposed sites, indicating that the effect is quite long range. However, this phenomenon has no major influence, as far as XPS or ATR-FTIR results disclose, on the backbone structure of the rubber sample. The results indicate that precautions should be taken when analyzing complex blended polymer samples using Raman spectroscopy.

Infrared Spectroscopy as a Chemical Fingerprinting Tool

NASA Technical Reports Server (NTRS)

Huff, Tim; Munafo, Paul M. (Technical Monitor)

2002-01-01

Infrared (IR) spectroscopy is a powerful analytical tool in the chemical fingerprinting of materials. The technique is rapid, reproducible and usually non-invasive. With the appropriate accessories, the technique can be used to examine samples in either a solid, liquid or gas phase. Solid samples of varying sizes and shapes may be used, and with the addition of microscopic IR (microspectroscopy) capabilities, minute materials such as single fibers and threads may be examined. With the addition of appropriate software, microspectroscopy can be used for automated discrete point or compositional surface area mapping, with the latter providing a means to record changes in the chemical composition of a material surface over a defined area. Both aqueous and non-aqueous free-flowing solutions can be analyzed using appropriate IR techniques, as can viscous liquids such as heavy oils and greases. Due to the ability to characterize gaseous samples, IR spectroscopy can also be coupled with thermal processes such as thermogravimetric (TG) analyses to provide both thermal and chemical data in a single run. In this configuration, solids (or liquids) heated in a TG analyzer undergo decomposition, with the evolving gases directed into the IR spectrometer. Thus, information is provided on the thermal properties of a material and the order in which its chemical constituents are broken down during incremental heating. Specific examples of these varied applications will be cited, with data interpretation and method limitations further discussed.

Ultrasound-assisted facile synthesis of a new tantalum(V) metal-organic framework nanostructure: Design, characterization, systematic study, and CO2 adsorption performance

NASA Astrophysics Data System (ADS)

Sargazi, Ghasem; Afzali, Daryoush; Mostafavi, Ali; Ebrahimipour, S. Yousef

2017-06-01

This work presents a fast route for the preparation of a new Ta(V) metal-organic framework nanostructure with high surface area, significant porosity, and small size distribution. X-ray diffraction (XRD), scanning electron microscopy (SEM), Transition electron microscopy (TEM), energy dispersive spectrometer (EDS), thermo-gravimetric analysis (TGA), differential scanning calorimetry (DSC), fourier transform infrared spectroscopy (FTIR), CHNS/O elemental analyser, and Brunauer-Emmett-Teller (BET) surface area analysis were applied to characterize the synthesized product. Moreover, the influences of ultrasonic irradiation including temperature, time, and power on different features of the final products were systematically studied using 2k-1 factorial design experiments, and the response surface optimization was used for determining the best welding parameter combination. The results obtained from analyses of variances showed that ultrasonic parameters affected the size distribution, thermal behaviour, and surface area of Ta-MOF samples. Based on response surface methodology, Ta-MOF could be obtained with mean diameter of 55 nm, thermal stability of 228 °C, and high surface area of 2100 m2/g. The results revealed that the synthesized products could be utilized in various applications such as a novel candidate for CO2 adsorption.

Toluene and acetaldehyde removal from air on to graphene-based adsorbents with microsized pores.

PubMed

Kim, Ji Min; Kim, Ji Hoon; Lee, Chang Yeon; Jerng, Dong Wook; Ahn, Ho Seon

2018-02-15

Volatile organic compound (VOC) gases can cause harm to the human body with exposure over the long term even at very low concentrations (ppmv levels); thus, effective absorbents for VOC gas removal are an important issue. In this study, accordingly, graphene-based adsorbents with microsized pores were used as adsorbents to remove toluene and acetaldehyde gases at low concentrations (30ppm). Sufficient amounts of the adsorbents were prepared for use on filters and were loaded uniformly at 0.1-0.5g on a 50×50mm 2 area, to evaluate their adsorption features with low gas concentrations. The morphology and chemical composition of the adsorbents were characterized using scanning electron microscopy, N 2 adsorption-desorption isotherms, X-ray photoelectron spectroscopy, and Raman spectroscopy. Microwave irradiation and heat treatment near 800°C under KOH activation resulted in enlargement of the pristine graphene surface and its specific surface area; maximum volume capacities of 3510m 3 /g and 630m 3 /g were observed for toluene and acetaldehyde gas. The high removal efficiency for toluene (98%) versus acetaldehyde (30%) gas was attributed to π-π interactions between the pristine graphene surface and toluene molecules. Copyright © 2017 Elsevier B.V. All rights reserved.

Interrelationship between TiO2 nanoparticle size and kind/size of dyes in the mechanism and conversion efficiency of dye sensitized solar cells.

PubMed

Tahay, Pooya; Babapour Gol Afshani, Meisam; Alavi, Ali; Parsa, Zahra; Safari, Nasser

2017-05-10

In order to provide a comprehensive investigation of TiO 2 nanoparticle size in relation with different dye types in DSSCs, three sizes of TiO 2 nanoparticles and two different dye types including a porphyrin dye (T2) and a ruthenium dye (N3) were synthesized. Steady state current-voltage (J-V) characteristics were investigated for the fabricated DSSCs and the results demonstrated that the optimum TiO 2 nanoparticle size changed with the dye type. The obtained J-V data were interpreted by cyclic voltammetry, UV-visible absorption spectroscopy, BET measurement, DFT calculation, IPCE measurement and impedance spectroscopy. The results for the N3 dye show that the surface area of the TiO 2 nanoparticles is a key factor for the N3 cells, which is restricted by TiO 2 pore diameter and surface state traps. In contrast, the density of localized states of the TiO 2 film under the LUMO state of the porphyrin dyes is the dominating factor for the performance of the solar cells, which is restricted by the surface area of the TiO 2 nanoparticles. These obtained results represent a significant advance in the development of porphyrin, ruthenium and even solid electrolyte DSSCs.

Hydrothermal synthesis of MnO2/CNT nanocomposite with a CNT core/porous MnO2 sheath hierarchy architecture for supercapacitors.

PubMed

Xia, Hui; Wang, Yu; Lin, Jianyi; Lu, Li

2012-01-05

MnO2/carbon nanotube [CNT] nanocomposites with a CNT core/porous MnO2 sheath hierarchy architecture are synthesized by a simple hydrothermal treatment. X-ray diffraction and Raman spectroscopy analyses reveal that birnessite-type MnO2 is produced through the hydrothermal synthesis. Morphological characterization reveals that three-dimensional hierarchy architecture is built with a highly porous layer consisting of interconnected MnO2 nanoflakes uniformly coated on the CNT surface. The nanocomposite with a composition of 72 wt.% (K0.2MnO2·0.33 H2O)/28 wt.% CNT has a large specific surface area of 237.8 m2/g. Electrochemical properties of the CNT, the pure MnO2, and the MnO2/CNT nanocomposite electrodes are investigated by cyclic voltammetry and electrochemical impedance spectroscopy measurements. The MnO2/CNT nanocomposite electrode exhibits much larger specific capacitance compared with both the CNT electrode and the pure MnO2 electrode and significantly improves rate capability compared to the pure MnO2 electrode. The superior supercapacitive performance of the MnO2/CNT nancomposite electrode is due to its high specific surface area and unique hierarchy architecture which facilitate fast electron and ion transport.

Hydrothermal synthesis of MnO2/CNT nanocomposite with a CNT core/porous MnO2 sheath hierarchy architecture for supercapacitors

PubMed Central

2012-01-01

MnO2/carbon nanotube [CNT] nanocomposites with a CNT core/porous MnO2 sheath hierarchy architecture are synthesized by a simple hydrothermal treatment. X-ray diffraction and Raman spectroscopy analyses reveal that birnessite-type MnO2 is produced through the hydrothermal synthesis. Morphological characterization reveals that three-dimensional hierarchy architecture is built with a highly porous layer consisting of interconnected MnO2 nanoflakes uniformly coated on the CNT surface. The nanocomposite with a composition of 72 wt.% (K0.2MnO2·0.33 H2O)/28 wt.% CNT has a large specific surface area of 237.8 m2/g. Electrochemical properties of the CNT, the pure MnO2, and the MnO2/CNT nanocomposite electrodes are investigated by cyclic voltammetry and electrochemical impedance spectroscopy measurements. The MnO2/CNT nanocomposite electrode exhibits much larger specific capacitance compared with both the CNT electrode and the pure MnO2 electrode and significantly improves rate capability compared to the pure MnO2 electrode. The superior supercapacitive performance of the MnO2/CNT nancomposite electrode is due to its high specific surface area and unique hierarchy architecture which facilitate fast electron and ion transport. PMID:24576342

Hydrothermal synthesis of MnO2/CNT nanocomposite with a CNT core/porous MnO2 sheath hierarchy architecture for supercapacitors

NASA Astrophysics Data System (ADS)

Xia, Hui; Wang, Yu; Lin, Jianyi; Lu, Li

2012-01-01

MnO2/carbon nanotube [CNT] nanocomposites with a CNT core/porous MnO2 sheath hierarchy architecture are synthesized by a simple hydrothermal treatment. X-ray diffraction and Raman spectroscopy analyses reveal that birnessite-type MnO2 is produced through the hydrothermal synthesis. Morphological characterization reveals that three-dimensional hierarchy architecture is built with a highly porous layer consisting of interconnected MnO2 nanoflakes uniformly coated on the CNT surface. The nanocomposite with a composition of 72 wt.% (K0.2MnO2·0.33 H2O)/28 wt.% CNT has a large specific surface area of 237.8 m2/g. Electrochemical properties of the CNT, the pure MnO2, and the MnO2/CNT nanocomposite electrodes are investigated by cyclic voltammetry and electrochemical impedance spectroscopy measurements. The MnO2/CNT nanocomposite electrode exhibits much larger specific capacitance compared with both the CNT electrode and the pure MnO2 electrode and significantly improves rate capability compared to the pure MnO2 electrode. The superior supercapacitive performance of the MnO2/CNT nancomposite electrode is due to its high specific surface area and unique hierarchy architecture which facilitate fast electron and ion transport.

Biotemplated Synthesis of Anatase Titanium Dioxide Nanoparticles via Lignocellulosic Waste Material

PubMed Central

Bagheri, Samira; Abd Hamid, Sharifah Bee

2014-01-01

Anatase titanium dioxide nanoparticles (TiO2-NPs) were synthesized by sol-gel method using rice straw as a soft biotemplate. Rice straw, as a lignocellulosic waste material, is a biomass feedstock which is globally produced in high rate and could be utilized in an innovative approach to manufacture a value-added product. Rice straw as a reliable biotemplate has been used in the sol-gel method to synthesize ultrasmall sizes of TiO2-NPs with high potential application in photocatalysis. The physicochemical properties of titanium dioxide nanoparticles were investigated by a number of techniques such as X-ray diffraction analysis (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, thermogravimetric analysis (TGA), ultraviolet visible spectra (UV-Vis), and surface area and pore size analysis. All results consensually confirmed that particle sizes of synthesized titanium dioxide were template-dependent, representing decrease in the nanoparticles sizes with increase of biotemplate concentration. Titanium dioxide nanoparticles as small as 13.0 ± 3.3 nm were obtained under our experimental conditions. Additionally, surface area and porosity of synthesized TiO2-NPs have been enhanced by increasing rice straw amount which results in surface modification of nanoparticles and potential application in photocatalysis. PMID:25126547

Reduction Expansion Synthesis as Strategy to Control Nitrogen Doping Level and Surface Area in Graphene

PubMed Central

Canty, Russell; Gonzalez, Edwin; MacDonald, Caleb; Osswald, Sebastian; Zea, Hugo; Luhrs, Claudia C.

2015-01-01

Graphene sheets doped with nitrogen were produced by the reduction-expansion (RES) method utilizing graphite oxide (GO) and urea as precursor materials. The simultaneous graphene generation and nitrogen insertion reactions are based on the fact that urea decomposes upon heating to release reducing gases. The volatile byproducts perform two primary functions: (i) promoting the reduction of the GO and (ii) providing the nitrogen to be inserted in situ as the graphene structure is created. Samples with diverse urea/GO mass ratios were treated at 800 °C in inert atmosphere to generate graphene with diverse microstructural characteristics and levels of nitrogen doping. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to study the microstructural features of the products. The effects of doping on the samples structure and surface area were studied by X-ray diffraction (XRD), Raman Spectroscopy, and Brunauer Emmet Teller (BET). The GO and urea decomposition-reduction process as well as nitrogen-doped graphene stability were studied by thermogravimetric analysis (TGA) coupled with mass spectroscopy (MS) analysis of the evolved gases. Results show that the proposed method offers a high level of control over the amount of nitrogen inserted in the graphene and may be used alternatively to control its surface area. To demonstrate the practical relevance of these findings, as-produced samples were used as electrodes in supercapacitor and battery devices and compared with conventional, thermally exfoliated graphene. PMID:28793618

Lignin from sugar cane bagasse: extraction, fabrication of nanostructured films, and application.

PubMed

Pereira, A A; Martins, G F; Antunes, P A; Conrrado, R; Pasquini, D; Job, A E; Curvelo, A A S; Ferreira, M; Riul, A; Constantino, C J L

2007-06-05

Four lignin samples were extracted from sugar cane bagasse using four different alcohols (methanol, ethanol, n-propanol, and 1-butanol) via the organosolv-CO2 supercritical pulping process. Langmuir films were characterized by surface pressure vs mean molecular area (Pi-A) isotherms to exploit information at the molecular level carrying out stability tests, cycles of compression/expansion (hysteresis), subphase temperature variations, and metallic ions dissolved into the water subphase at different concentrations. Briefly, it was observed that these lignins are relatively stable on the water surface when compared to those obtained via different extraction processes. Besides, the Pi-A isotherms are shifted to smaller molecular areas at higher subphase temperatures and to larger molecular areas when the metallic ions are dissolved into the subphase. The results are related to the formation of stable aggregates (domains) onto the water subphase by these lignins, as shown in the Pi-A isotherms. It was found as well that the most stable lignin monolayer onto the water subphase is that extracted with 1-butanol. Homogeneous Langmuir-Blodgett (LB) films of this lignin could be produced as confirmed by UV-vis absorption spectroscopy and the cumulative transfer parameter. In addition, FTIR analysis showed that this lignin LB film is structured in a way that the phenyl groups are organized preferentially parallel to the substrate surface. Further, these LB films were deposited onto gold interdigitated electrodes and ITO and applied in studies involving the detection of Cd+2 ions in aqueous solutions at low concentration levels through impedance spectroscopy and electrochemical measurements. FTIR spectroscopy was carried out before and after soaking the thin films into Cd+2 aqueous solutions, revealing a possible physical interaction between the lignin phenyl groups and the heavy metal ions. The importance of using nanostructured systems is demonstrated as well by comparing both LB and cast films.

Adsorption of cadmium by activated carbon cloth: influence of surface oxidation and solution pH.

PubMed

Rangel-Mendez, J R; Streat, M

2002-03-01

The surface of activated carbon cloth (ACC), based on polyacrylonitrile fibre as a precursor, was oxidised using nitric acid, ozone and electrochemical oxidation to enhance cadmium ion exchange capacity. Modified adsorbents were physically and chemically characterised by pH titration, direct titration, X-ray photoelectron spectroscopy, elemental analysis, surface area and porosimetry, and scanning electron microscopy. BET surface area decreased after oxidation, however, the total ion exchange capacity increased by a factor of approximately 3.5 compared to the commercial as-received ACC. A very significant increase in cadmium uptake, by a factor of 13, was observed for the electrochemically oxidised ACC. Equilibrium sorption isotherms were determined at pH 4, 5 and 6 and these showed that cadmium uptake increased with increasing pH. There was clear evidence of physical damage to ozone-oxidised fibre, however, acid and electrochemically oxidised samples were completely stable.

Key factor affecting the structural and textural properties of ZSM-5/MCM-41 composite

NASA Astrophysics Data System (ADS)

Boukoussa, Bouhadjar; Aouad, Nafissa; Hamacha, Rachida; Bengueddach, Abdelkader

2015-03-01

ZSM-5/MCM-41 micro/mesoporous composite materials were synthesized by the hydrothermal technique with alkali-treated ZSM-5 zeolite as source of silica and aluminum and characterized by various physico-chemical techniques such as X-ray diffraction (XRD), nitrogen sorption at 77 K, transmission electronic microscopy (TEM), FTIR spectroscopy and NH3 temperature programmed desorption (TPD) techniques. The effect of concentration of CTAB in the synthesis of these solids has been investigated, the mesopore volume, surface area and surface acidity decrease with increasing the concentration of CTAB. Increasing the CTAB concentration causes the recrystallization of zeolite ZSM-5 and it disadvantage the formation of mesoporous materials MCM-41. The catalytic activity of ZSM-5/MCM-41 materials has been evaluated in the Friedel-Crafts acylation of anisole with benzoyl chloride as alkylating agent. The results revealed the reaction to be influenced by surface area, pore volume and surface acidity.

Speciation of residual carbon contained in UO{sub 2}

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

Ziouane, Yannis; Arab-Chapelet, Bénédicte; Tamain, Christelle

2016-12-15

UO{sub 2} powders were synthesized thanks to oxalic precipitation (platelet morphology) and sol-gel route and completely characterized. A secondary phase was found depending on the calcination atmospheres. This phase has been identified by Raman spectroscopy as graphitic material (i.e. carbon-based secondary compound) and quantified by thermogravimetric analyses. Its amount varies with the calcination atmosphere. The presence of this secondary phase has no significant effect on the lattice parameter and its specific surface area. - Graphical abstract: Figure 2: Raman spectroscopy of the three UO{sub 2} powders and of the dissolution residues.

Spectroscopy of Moses Rock Kimberlite Diatreme

NASA Technical Reports Server (NTRS)

Pieters, C. M.; Mustard, J. F.

1985-01-01

Three types of remote sensing data (Airborne Imaging Spectroscopy (AIS), NS001, Zeiss IR-photographs) were obtained for the Moses Rock kimberlite dike in southern Utah. The goal is to identify and characterize the mantle derived mafic component in such volcanic features. The Zeiss and NS001 images provide information on the regional setting and allow units of the dike to be distinguished from surrounding material. A potential unmapped satellite dike was identified. The AIS data provide characterizing information of the surface composition of the dike. Serpentized olivine-bearing soils are (tentatively) identified from the AIS spectra for a few areas within the dike.

Environmental chemistry at vapor/water interfaces: insights from vibrational sum frequency generation spectroscopy.

PubMed

Jubb, Aaron M; Hua, Wei; Allen, Heather C

2012-01-01

The chemistry that occurs at surfaces has been an intense area of study for many years owing to its complexity and importance in describing a wide range of physical phenomena. The vapor/water interface is particularly interesting from an environmental chemistry perspective as this surface plays host to a wide range of chemistries that influence atmospheric and geochemical interactions. The application of vibrational sum frequency generation (VSFG), an inherently surface-specific, even-order nonlinear optical spectroscopy, enables the direct interrogation of various vapor/aqueous interfaces to elucidate the behavior and reaction of chemical species within the surface regime. In this review we discuss the application of VSFG to the study of a variety of atmospherically important systems at the vapor/aqueous interface. Chemical systems presented include inorganic ionic solutions prevalent in aqueous marine aerosols, small molecular solutes, and long-chain fatty acids relevant to fat-coated aerosols. The ability of VSFG to probe both the organization and reactions that may occur for these systems is highlighted. A future perspective toward the application of VSFG to the study of environmental interfaces is also provided.

Status and Direction of Tribology as a Science in the 80's. Understanding and Prediction

NASA Technical Reports Server (NTRS)

Tabor, D.

1984-01-01

The most challenging research problems in tribology for the next decade or beyond are classified horizontally into two categories: (1) understanding of basic mechanisms and (2) prediction of practical performance. Vertical classifications are in terms of particular themes or fields of interest. Areas where more fundamental work is required are: adhesion and friction of clean and contaminated surfaces; lubrication; new materials; surface characterization at the engineering level (topography) and at the atomic levels (various spectroscopies); and wear.

Fabrication of large area nanoprism arrays and their application for surface enhanced Raman spectroscopy

NASA Astrophysics Data System (ADS)

Cui, B.; Clime, L.; Li, K.; Veres, T.

2008-04-01

This work demonstrates the fabrication of metallic nanoprism (triangular nanostructure) arrays using a low-cost and high-throughput process. In the method, the triangular structure is defined by the shadow of a pyramid during angle evaporation of a metal etching mask. The pyramids were created by nanoimprint lithography in polymethylmethacrylate (PMMA) using a mould having an inverse-pyramid-shaped hole array formed by KOH wet etching of silicon. Silver and gold nanoprism arrays with a period of 200 nm and an edge length of 100 nm have been fabricated and used as effective substrates for surface enhanced Raman spectroscopy (SERS) detection of rhodamine 6G (R6G) molecules. Numerical calculations confirmed the great enhancement of electric field near the sharp nanoprism corners, as well as the detrimental effect of the chromium adhesion layer on localized surface plasmon resonance. The current method can also be used to fabricate non-equilateral nanoprism and three-dimensional (3D) nanopyramid arrays, and it can be readily extended to other metals.

Fabrication of large area nanoprism arrays and their application for surface enhanced Raman spectroscopy.

PubMed

Cui, B; Clime, L; Li, K; Veres, T

2008-04-09

This work demonstrates the fabrication of metallic nanoprism (triangular nanostructure) arrays using a low-cost and high-throughput process. In the method, the triangular structure is defined by the shadow of a pyramid during angle evaporation of a metal etching mask. The pyramids were created by nanoimprint lithography in polymethylmethacrylate (PMMA) using a mould having an inverse-pyramid-shaped hole array formed by KOH wet etching of silicon. Silver and gold nanoprism arrays with a period of 200 nm and an edge length of 100 nm have been fabricated and used as effective substrates for surface enhanced Raman spectroscopy (SERS) detection of rhodamine 6G (R6G) molecules. Numerical calculations confirmed the great enhancement of electric field near the sharp nanoprism corners, as well as the detrimental effect of the chromium adhesion layer on localized surface plasmon resonance. The current method can also be used to fabricate non-equilateral nanoprism and three-dimensional (3D) nanopyramid arrays, and it can be readily extended to other metals.

Tunable Nanoantennas for Surface Enhanced Infrared Absorption Spectroscopy by Colloidal Lithography and Post-Fabrication Etching

NASA Astrophysics Data System (ADS)

Chen, Kai; Duy Dao, Thang; Nagao, Tadaaki

2017-03-01

We fabricated large-area metallic (Al and Au) nanoantenna arrays on Si substrates using cost-effective colloidal lithography with different micrometer-sized polystyrene spheres. Variation of the sphere size leads to tunable plasmon resonances in the middle infrared (MIR) range. The enhanced near-fields allow us to detect the surface phonon polaritons in the natural SiO2 thin layers. We demonstrated further tuning capability of the resonances by employing dry etching of the Si substrates with the nanoantennas acting as the etching masks. The effective refractive index of the nanoantenna surroundings is efficiently decreased giving rise to blueshifts of the resonances. In addition, partial removal of the Si substrates elevates the nanoantennas from the high-refractive-index substrates making more enhanced near-fields accessible for molecular sensing applications as demonstrated here with surface-enhanced infrared absorption (SEIRA) spectroscopy for a thin polymer film. We also directly compared the plasmonic enhancement from the Al and Au nanoantenna arrays.

One-step Melt Synthesis of Water Soluble, Photoluminescent, Surface-Oxidized Silicon Nanoparticles for Cellular Imaging Applications

PubMed Central

Manhat, Beth A.; Brown, Anna L.; Black, Labe A.; Ross, J.B. Alexander; Fichter, Katye; Vu, Tania; Richman, Erik

2012-01-01

We have developed a versatile, one-step melt synthesis of water-soluble, highly emissive silicon nanoparticles using bi-functional, low-melting solids (such as glutaric acid) as reaction media. Characterization through transmission electron microscopy, selected area electron diffraction, X-ray photoelectron spectroscopy, and Raman spectroscopy shows that the one-step melt synthesis produces nanoscale Si cores surrounded by a silicon oxide shell. Analysis of the nanoparticle surface using FT-IR, zeta potential, and gel electrophoresis indicates that the bi-functional ligand used in the one-step synthesis is grafted onto the nanoparticle, which allows for tuning of the particle surface charge, solubility, and functionality. Photoluminescence spectra of the as-prepared glutaric acid-synthesized silicon nanoparticles show an intense blue-green emission with a short (ns) lifetime suitable for biological imaging. These nanoparticles are found to be stable in biological media and have been used to examine cellular uptake and distribution in live N2a cells. PMID:23139440

Development of high-sensitive, reproducible colloidal surface-enhanced Raman spectroscopy active substrate using silver nanocubes for potential biosensing applications

NASA Astrophysics Data System (ADS)

Hasna, Kudilatt; Lakshmi, Kiran; Ezhuthachan Jayaraj, Madambi Kunjukuttan; Kumar, Kumaran Rajeev; Matham, Murukeshan Vadakke

2016-04-01

Surface-enhanced Raman spectroscopy (SERS) has emerged as one of the thrust research areas that could find potential applications in bio and chemical sensing. We developed colloidal SERS active substrate with excellent sensitivity and high reproducibility using silver nanocube (AgNC) synthesized via the solvothermal method. Finite-difference time-domain simulation was carried out in detail to visualize dipole generation in the nanocube during localized surface plasmon resonance and to locate the respective hot spots in AgNC responsible for the huge Raman enhancement. The prediction is verified by the SERS analysis of the synthesized nanocubes using Rhodamine 6G molecule. An excellent sensitivity with a detection limit of 10-17 M and a very high enhancement factor of 1.2×108 confirms the "hot spots" in the nanocube. SERS activity is also carried out for crystal violet and for food adulterant Sudan I molecule. Finally, label-free DNA detection is performed to demonstrate the versatility of SERS as a potential biosensor.

Bromomethane Contamination in the Cathode of Proton Exchange Membrane Fuel Cells.

PubMed

Zhai, Yunfeng; Baturina, Olga; Ramaker, David E; Farquhar, Erik; St-Pierre, Jean; Swider-Lyons, Karen E

2016-09-20

The effects of bromomethane (BrCH 3 ), an airborne contaminant, on the performance of a single PEMFC are compared with that of another halocarbon, chlorobenzene. Under a constant current of 1 A cm -2 and at 45 °C, 20 ppm bromomethane causes approximately 30% cell voltage loss in approximately 30 h, as opposed to much more rapid performance degradation observed with chlorobenzene. Electrochemical impedance spectroscopy, cyclic voltammetry, linear scanning voltammetry, and polarization measurements are applied to characterize the temporary electrochemical reaction effect and permanent performance effects. X-ray absorption spectroscopy is used to confirm that Br is adsorbed on the Pt electrocatalyst surface. We conclude that airborne bromomethane poisons a PEMFC in a different way from chlorobenzene because it is largely hydrolyzed to bromide, Br - , which is then excluded from the Pt catalyst by the negatively charged Nafion ionomer. The little Br - and bromomethane that adsorbs on the Pt surface can be partially removed by cycling but causes some irreversible surface area loss.

Bromomethane Contamination in the Cathode of Proton Exchange Membrane Fuel Cells

PubMed Central

Baturina, Olga; Ramaker, David E.; Farquhar, Erik; St-Pierre, Jean; Swider-Lyons, Karen E.

2016-01-01

The effects of bromomethane (BrCH3), an airborne contaminant, on the performance of a single PEMFC are compared with that of another halocarbon, chlorobenzene. Under a constant current of 1 A cm−2 and at 45 °C, 20 ppm bromomethane causes approximately 30% cell voltage loss in approximately 30 h, as opposed to much more rapid performance degradation observed with chlorobenzene. Electrochemical impedance spectroscopy, cyclic voltammetry, linear scanning voltammetry, and polarization measurements are applied to characterize the temporary electrochemical reaction effect and permanent performance effects. X-ray absorption spectroscopy is used to confirm that Br is adsorbed on the Pt electrocatalyst surface. We conclude that airborne bromomethane poisons a PEMFC in a different way from chlorobenzene because it is largely hydrolyzed to bromide, Br−, which is then excluded from the Pt catalyst by the negatively charged Nafion ionomer. The little Br− and bromomethane that adsorbs on the Pt surface can be partially removed by cycling but causes some irreversible surface area loss. PMID:27695133

Meso-scale defect evaluation of selective laser melting using spatially resolved acoustic spectroscopy

PubMed Central

Hirsch, M.; Catchpole-Smith, S.; Patel, R.; Marrow, P.; Li, Wenqi; Tuck, C.; Sharples, S. D.

2017-01-01

Developments in additive manufacturing technology are serving to expand the potential applications. Critical developments are required in the supporting areas of measurement and in process inspection to achieve this. CM247LC is a nickel superalloy that is of interest for use in aerospace and civil power plants. However, it is difficult to process via selective laser melting (SLM) as it suffers from cracking during rapid cooling and solidification. This limits the viability of CM247LC parts created using SLM. To quantify part integrity, spatially resolved acoustic spectroscopy (SRAS) has been identified as a viable non-destructive evaluation technique. In this study, a combination of optical microscopy and SRAS was used to identify and classify the surface defects present in SLM-produced parts. By analysing the datasets and scan trajectories, it is possible to correlate morphological information with process parameters. Image processing was used to quantify porosity and cracking for bulk density measurement. Analysis of surface acoustic wave data showed that an error in manufacture in the form of an overscan occurred. Comparing areas affected by overscan with a bulk material, a change in defect density from 1.17% in the bulk material to 5.32% in the overscan regions was observed, highlighting the need to reduce overscan areas in manufacture. PMID:28989306

Investigation of a fiber optic surface plasmon spectroscopy in conjunction with conductivity as an in situ method for simultaneously monitoring changes in dissolved organic carbon and salinity in coastal waters.

PubMed

Kim, Yoon-Chang; Cramer, Jeffrey A; Booksh, Karl S

2011-10-21

A combination surface plasmon resonance (SPR) and conductivity sensor array was developed and implemented to demonstrate the ability to differentiate among changes in dissolved organic carbon (DOC) and salinity in coastal water. The array is capable of achieving sufficient spatial and temporal data density to better understand the cycling and fate of terrestrial DOC in coastal areas. DOC is the second largest source of bioreactive carbon in the environment and plays a key role in mediating microbial activity and generation of atmospheric CO(2). In the coastal areas, the salinity is also an important property in many applications, such as leak detection for landfill liners, saltwater intrusion to drinking water, marine environment monitoring, and seasonal climate prediction. Conductivity sensors are the industry standard for determining salinity in ocean systems. However, both conductivity and refractive index sensors, such as SPR spectroscopy based sensors, respond to salinity and DOC levels. To demonstrate the capability of the SPR sensor and a conductivity sensor to collect complimentary data useful in discrimination of salinity and DOC in coastal zone water, conductivity, SPR, and temperature data were collected during passage from the Juan de Fuca ridge area returning to the University of Washington docks.

Meso-scale defect evaluation of selective laser melting using spatially resolved acoustic spectroscopy.

PubMed

Hirsch, M; Catchpole-Smith, S; Patel, R; Marrow, P; Li, Wenqi; Tuck, C; Sharples, S D; Clare, A T

2017-09-01

Developments in additive manufacturing technology are serving to expand the potential applications. Critical developments are required in the supporting areas of measurement and in process inspection to achieve this. CM247LC is a nickel superalloy that is of interest for use in aerospace and civil power plants. However, it is difficult to process via selective laser melting (SLM) as it suffers from cracking during rapid cooling and solidification. This limits the viability of CM247LC parts created using SLM. To quantify part integrity, spatially resolved acoustic spectroscopy (SRAS) has been identified as a viable non-destructive evaluation technique. In this study, a combination of optical microscopy and SRAS was used to identify and classify the surface defects present in SLM-produced parts. By analysing the datasets and scan trajectories, it is possible to correlate morphological information with process parameters. Image processing was used to quantify porosity and cracking for bulk density measurement. Analysis of surface acoustic wave data showed that an error in manufacture in the form of an overscan occurred. Comparing areas affected by overscan with a bulk material, a change in defect density from 1.17% in the bulk material to 5.32% in the overscan regions was observed, highlighting the need to reduce overscan areas in manufacture.

Catalyst free growth of CNTs by CVD on nanoscale rough surfaces of silicon substrates

NASA Astrophysics Data System (ADS)

Damodar, D.; Sahoo, R. K.; Jacob, C.

2013-06-01

Catalyst free growth of carbon nanotubes (CNT) has been achieved using atmospheric pressure chemical vapor deposition (APCVD) on surface modified Si(111) substrates. The effect of the substrate surface has been observed by partially etching with KOH (potassium hydroxide) solution which is an anisotropic etchant. Scanning electron microscopy (SEM) confirmed the formation of CNTs over most of the area of the substrate where substrates were anisotropically etched. Transmission electron microscopy (TEM) was used to observe the internal structure of the CNTs. Raman spectroscopy further confirmed the formation of the carbon nanostructures and also their graphitic crystallinity.

Micro faraday-element array detector for ion mobility spectroscopy

DOEpatents

Gresham, Christopher A [Albuquerque, NM; Rodacy, Phillip J [Albuquerque, NM; Denton, M Bonner [Tucson, AZ; Sperline, Roger [Tucson, AZ

2004-10-26

An ion mobility spectrometer includes a drift tube having a collecting surface covering a collecting area at one end of the tube. The surface comprises a plurality of closely spaced conductive elements on a non-conductive substrate, each conductive element being electrically insulated from each other element. A plurality of capacitive transimpedance amplifiers (CTIA) adjacent the collecting surface are electrically connected to the plurality of elements, so charge from an ion striking an element is transferred to the capacitor of the connected CTIA. A controller counts the charge on the capacitors over a period of time.

Bioengineered silver nanoparticles as potent anti-corrosive inhibitor for mild steel in cooling towers.

PubMed

Narenkumar, Jayaraman; Parthipan, Punniyakotti; Madhavan, Jagannathan; Murugan, Kadarkarai; Marpu, Sreekar Babu; Suresh, Anil Kumar; Rajasekar, Aruliah

2018-02-01

Silver nanoparticle-aided enhancement in the anti-corrosion potential and stability of plant extract as ecologically benign alternative for microbially induced corrosion treatment is demonstrated. Bioengineered silver nanoparticles (AgNPs) surface functionalized with plant extract material (proteinacious) was generated in vitro in a test tube by treating ionic AgNO 3 with the leaf extract of Azadirachta indica that acted as dual reducing as well as stabilizing agent. Purity and crystallinity of the AgNPs, along with physical and surface characterizations, were evaluated by performing transmission electron microscopy, Fourier transform infrared spectroscopy, energy dispersive x-ray spectra, single-area electron diffractions, zeta potential, and dynamic light scattering measurements. Anti-corrosion studies against mild steel (MS1010) by corrosion-inducive bacterium, Bacillus thuringiensis EN2 isolated from cooling towers, were evaluated by performing electrochemical impedance spectroscopy (EIS), weight loss analysis, and surface analysis by infrared spectroscopy. Our studies revealed that AgNPs profoundly inhibited the biofilm on MS1010 surface and reduced the corrosion rates with the CR of 0.5 mm/y and an inhibition efficiency of 77% when compared to plant extract alone with a CR of 2.2 mm/y and an inhibition efficiency of 52%. Further surface analysis by infrared spectra revealed that AgNPs formed a protective layer of self-assembled film on the surface of MS1010. Additionally, EIS and surface analysis revealed that the AgNPs have inhibited the bacterial biofilm and reduced the pit on MS1010. This is the first report disclosing the application of bioengineered AgNP formulations as potent anti-corrosive inhibitor upon forming a protective layer over mild steel in cooling water towers. Graphical Abstract ᅟ.

Structural and Morphological Properties of Carbon Supports: Effect of Catalyst degradation, ECS Transactions 33(1), 425 (2010)

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

A. Patel; K. Artyushkova; P. Atanassov

The object of this work was to identify correlations between performance losses of Pt electrocatalysts on carbon support materials and the chemical and morphological parameters that describe them. Accelerated stress testing, with an upper potential of 1.2 V, was used to monitor changes to cathode properties, including kinetic performance and effective platinum surface area losses. The structure and chemical compositions were studied using X-ray Photoelectron Spectroscopy and Scanning Electron Microscopy coupled with Digital Image Processing. As this is an ongoing study, it is difficult to draw firm conclusions, though a trend between support surface area overall performance loss was foundmore » to exist.« less

Structural and Morphological Properties of Carbon Supports: Effect on Catalyst Degradation

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

Patel, Anant; Artyushkova, Kateryna; Atanassov, Plamen

2010-07-01

The object of this work was to identify correlations between performance losses of Pt electrocatalysts on carbon support materials and the chemical and morphological parameters that describe them. Accelerated stress testing, with an upper potential of 1.2 V, was used to monitor changes to cathode properties, including kinetic performance and effective platinum surface area losses. The structure and chemical compositions were studied using X-ray Photoelectron Spectroscopy and Scanning Electron Microscopy coupled with Digital Image Processing. As this is an ongoing study, it is difficult to draw firm conclusions, though a trend between support surface area overall performance loss was foundmore » to exist.« less

Preparation and recognition of surface molecularly imprinted core-shell microbeads for protein in aqueous solutions

NASA Astrophysics Data System (ADS)

Lu, Yan; Yan, Chang-Ling; Gao, Shu-Yan

2009-04-01

In this paper, a surface molecular imprinting technique was reported for preparing core-shell microbeads of protein imprinting, and bovine hemoglobin or bovine serum albumin were used as model proteins for studying the imprinted core-shell microbeads. 3-Aminophenylboronic acid (APBA) was polymerized onto the surface of polystyrene microbead in the presence of the protein templates to create protein-imprinted core-shell microbeads. The various samples were characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS) and Brunauer-Emmett-Teller (BET) methods. The effect of pH on rebinding of the template hemoglobin, the specific binding and selective recognition were studied for the imprinted microbeads. The results show that the bovine hemoglobin-imprinted core-shell microbeads were successfully created. The shell was a sort of imprinted thin films with porous structure and larger surface areas. The imprinted microbeads have good selectivity for templates and high stability. Due to the recognition sites locating at or closing to the surface, these imprinted microbeads have good property of mass-transport. Unfortunately, the imprint technology was not successfully applied to imprinting bovine serum albumin (BSA).

Grafting of ionic liquids on stainless steel surface for antibacterial application.

PubMed

Pang, Li Qing; Zhong, Li Juan; Zhou, Hui Fang; Wu, Xue E; Chen, Xiao Dong

2015-02-01

Stainless steel (SS) is favored for many uses due to its excellent chemical resistance, thermal stability and mechanical properties. Biofilms can be formed on stainless steel and may lead to serious hygiene problems and economic losses in many areas, e.g. food processing, public infrastructure and healthcare. For the first time, our work endeavored to make SS having antibacterial properties, ionic liquids (ILs) were grafted on SS surface via silane treatment followed by thiol-ene click reaction. The chemical structure and composition of the ILs grafted stainless-steel coupon surfaces were characterized by X-ray photoelectron spectroscopy (XPS) and attenuated total reflection-Fourier transform infrared (ATR-FTIR) spectroscopy. The antibacterial activity has been investigated, and the results showed that the ILs grafted SS surface exhibited significant antibacterial effects against Gram-negative Escherichia coli. Additionally, the results obtained here indicated that the ILs used here having bromide anion showed much better antibacterial activity against E. coli than the corresponding ILs with tetrafluoroborate and hexafluorophosphate as anions. These results obtained here can help to design novel and more efficient stainless steel having antibacterial surface. Copyright © 2014 Elsevier B.V. All rights reserved.

Analytical Chemistry of Surfaces: Part II. Electron Spectroscopy.

ERIC Educational Resources Information Center

Hercules, David M.; Hercules, Shirley H.

1984-01-01

Discusses two surface techniques: X-ray photoelectron spectroscopy (ESCA) and Auger electron spectroscopy (AES). Focuses on fundamental aspects of each technique, important features of instrumentation, and some examples of how ESCA and AES have been applied to analytical surface problems. (JN)

Reflectance and Thermal Infrared Spectroscopy of Mars: Relationship Between ISM and TES for Compositional Determinations

NASA Technical Reports Server (NTRS)

Boyce, Joseph (Technical Monitor); Mustard, John

2004-01-01

Reflectance spectroscopy has demonstrated that high albedo surfaces on Mars contain heavily altered materials with some component of hematite, poorly crystalline ferric oxides, and an undefined silicate matrix. The spectral properties of many low albedo regions indicate crystalline basalts containing both low and high calcium pyroxene, a mineralogy consistent with the basaltic SNC meteorites. The Thermal Emission Spectrometer (TES) experiment on the Mars Geochemical Surveyor has acquired critical new data relevant to surface composition and mineralogy, but in a wavelength region that is complementary to reflectance spectroscopy. The essence of the completed research was to analyze TES data in the context of reflectance data obtained by the French ISM imaging spectrometer experiment in 1989. This approach increased our understanding of the complementary nature of these wavelength regions for mineralogic determinations using actual observations of the martian surface. The research effort focused on three regions of scientific importance: Syrtis Major-Isidis Basin, Oxia Palus-Arabia, and Valles Marineris. In each region distinct spatial variations related to reflectance, and in derived mineralogic information and interpreted compositional units were analyzed. In addition, specific science questions related to the composition of volcanics and crustal evolution, soil compositions and pedogenic processes, and the relationship between pristine lithologies and weathering provided an overall science-driven framework for the work. The detailed work plan involved colocation of TES and ISM data, extraction of reflectance and emissivity spectra from areas of known reflectance variability, and quantitative analysis using factor analysis and statistical techniques to determine the degree of correspondence between these different wavelength regions. Identified coherent variations in TES spectroscopy were assessed against known atmospheric effects to validate that the variations are due to surface properties. With this new understanding of reflectance and emission spectroscopy, mineralogic interpretations were derived and applied to the science objectives of the three regions.

Beryllium surface levels in a military ammunition plant.

PubMed

Sanderson, Wayne T; Leonard, Stephanie; Ott, Darrin; Fuortes, Laurence; Field, William

2008-07-01

This study evaluated the presence of beryllium surface contamination in a U.S. conventional munitions plant as an indicator of possible past beryllium airborne and skin exposure and used these measurements to classify job categories by potential level of exposure. Surface samples were collected from production and nonproduction areas of the plant and at regional industrial reference sites with no known history of beryllium use. Surface samples of premoistened wiping material were analyzed for beryllium mass content using inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and results expressed as micrograms of beryllium per 100 square centimeters (micro g/100 cm(2)). Beryllium was detected in 87% of samples collected at the munitions plant and in 72% of the samples collected at regional reference sites. Two munitions plant samples from areas near sanders and grinders were above 3.0 micro g/100 cm(2) (U.S. Department of Energy surface contamination limit). The highest surface level found at the reference sites was 0.44 micro g/100 cm(2). Workers in areas where beryllium-containing alloy tools were sanded or ground, but not other work areas, may have been exposed to airborne beryllium concentrations above levels encountered in other industries where metal work is conducted. Surface sampling provided information useful for categorizing munitions plant jobs by level of past beryllium airborne and skin exposure and, subsequently, for identifying employees within exposure strata to be screened for beryllium sensitization.

Terahertz emission and spectroscopy on InN epilayer and nanostructure

NASA Astrophysics Data System (ADS)

Ahn, H.; Pan, C.-L.; Gwo, S.

2009-02-01

We report a comprehensive study on THz emission and spectroscopy of indium nitride (InN) films and its nanorod arrays grown by plasma-assisted molecular beam epitaxy technique. For the enhancement of THz emission from InN, we demonstrated two method; firstly using nanorod arrays, which have large surface area for optical absorption and THz emission, and secondly using nonpolar InN film, of which the electric field is along the sample surface. We propose that a "screened" photo-Dember effect due to narrow surface electron accumulation layer of InN is responsible for the nanorod-size-dependent enhancement from InN nanorods. The primary THz radiation mechanism of nonpolar InN is found to be due to the acceleration of photoexcited carriers under the polarization-induced in-plane electric field. THz time-domain spectroscopy has been used to investigate THz conductivity and dielectric response of InN nanorod arrays and epitaxial film. The complex THz conductivity of InN film is well fitted by the Drude model, while the negative imaginary conductivity of the InN nanorods can be described by using a non-Drude model, which includes a preferential backward scattering due to defects in InN nanorods, or a Coulombic restoring force from charged defects.

Hierarchical Co(OH)2 nanostructures/glassy carbon electrode derived from Co(BTC) metal-organic frameworks for glucose sensing

NASA Astrophysics Data System (ADS)

He, Juan; Lu, Xingping; Yu, Jie; Wang, Li; Song, Yonghai

2016-07-01

A novel Co(OH)2/glassy carbon electrode (GCE) has been fabricated via metal-organic framework (MOF)-directed method. In the strategy, the Co(BTC, 1,3,5-benzentricarboxylic acid) MOFs/GCE was firstly prepared by alternately immersing GCE in Co2+ and BTC solution based on a layer-by-layer method. And then, the Co(OH)2 with hierarchical flake nanostructure/GCE was constructed by immersing Co(BTC) MOFs/GCE into 0.1 M NaOH solution at room temperature. Such strategy improves the distribution of hierarchical Co(OH)2 nanostructures on electrode surface greatly, enhances the stability of nanomaterials on the electrode surface, and increases the use efficiency of the Co(OH)2 nanostructures. Scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray powder diffraction, energy dispersive spectroscopy, Fourier transform infrared spectroscopy, and Raman spectra were used to characterize the Co(BTC) MOFs/GCE and Co(OH)2/GCE. Based on the hierarchical Co(OH)2 nanostructures/GCE, a novel and sensitive nonenzymatic glucose sensor was developed. The good performance of the resulted sensor toward the detection of glucose was ascribed to hierarchical flake nanostructures, good mechanical stability, excellent distribution, and large specific surface area of Co(OH)2 nanostructures. The proposed preparation method is simple, efficient, and cheap .

Tip-enhanced Raman spectroscopy and near-field polarization

NASA Astrophysics Data System (ADS)

Saito, Yuika; Mino, Toshihiro; Verma, Prabhat

2015-12-01

Tip-enhanced Raman spectroscopy (TERS) is a powerful tool for High-resolution Raman spectroscopy. In this method, a metal coated nano-tip acts as a plasmonic antenna to enhance the originally weak Raman scattering from a nanometric volume of a sample. The technique enables to detect Raman scattering light from nano-scale area and also enhance the light intensity with combination of near-filed light and localized surface plasmon generated at a metallized tip apex. Nowadays TERS is used to investigate various nano-scale samples, for examples, carbon nanotubes, graphenes DNA and biomaterials. As the TERS developed, there is high demand to investigate the properties of near-field light e.g. polarization properties. We have analyzed the polarization properties of near-field light in TERS and successfully realized the quantitative nano-imaging by visible light.

Synthesis and characterization of hydrogen-bond acidic functionalized graphene

NASA Astrophysics Data System (ADS)

Yang, Liu; Han, Qiang; Pan, Yong; Cao, Shuya; Ding, Mingyu

2014-05-01

Hexafluoroisopropanol phenyl group functionalized materials have great potential in the application of gas-sensitive materials for nerve agent detection, due to the formation of strong hydrogen-bonding interactions between the group and the analytes. In this paper, take full advantage of ultra-large specific surface area and plenty of carbon-carbon double bonds and hexafluoroisopropanol phenyl functionalized graphene was synthesized through in situ diazonium reaction between -C=C- and p-hexafluoroisopropanol aniline. The identity of the as-synthesis material was confirmed by transmission electron microscopy, Raman spectroscopy, ultraviolet visible spectroscopy, X-ray photoelectron spectroscopy and thermo gravimetric analysis. The synthesis method is simply which retained the excellent physical properties of original graphene. In addition, the novel material can be assigned as an potential candidate for gas sensitive materials towards organophosphorus nerve agent detection.

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

Moosakhani, S.; Color and Polymer Research Center; Sabbagh Alvani, A.A., E-mail: sabbagh_alvani@aut.ac.ir

Highlights: • We have demonstrated AgI sensitized solar cell for the first time. • Obtained mesoporous titania powders possessed small crystallite size, high purity and surface area, and developed mesopores with a narrow pore size distribution. • Photovoltaic measurements revealed the electron injection from AgI to TiO{sub 2}. • The assembled AgI-QD solar cells yielded a power conversion efficiency of 0.64% under one sun illumination. • AgI may be a suitable candidate material for use as a non-toxic sensitizer in QDSSC. - Abstract: The present study reports the performance of a new photosensitizer -AgI quantum dots (QDs)- and mesoporous titaniamore » (TiO{sub 2}) nanocrystals synthesized by sol–gel (SG) method for solar cells. Furthermore, the effects of n-heptane on the textural properties of TiO{sub 2} nanocrystals were comprehensively investigated by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), N{sub 2} adsorption–desorption measurements, and UV–vis spectroscopy. TiO{sub 2} powders exhibited an anatase-type mesoporous structure with a high surface area of 89.7 m{sup 2}/g. Afterwards, the QDs were grown on mesoporous TiO{sub 2} surface to fabricate a TiO{sub 2}/AgI electrode by a successive ionic layer adsorption and reaction (SILAR) deposition route. Current–voltage characteristics and electrochemical impedance spectroscopy (EIS) data demonstrated that the injection of photoexcited electrons from AgI QDs into the TiO{sub 2} matrix produces photocurrents. The assembled AgI-QD solar cells yielded a power conversion efficiency of 0.64% and a short-circuit current of 2.13 mA/cm{sup 2} under one sun illumination.« less

Effect of crystal habits on the surface energy and cohesion of crystalline powders.

PubMed

Shah, Umang V; Olusanmi, Dolapo; Narang, Ajit S; Hussain, Munir A; Gamble, John F; Tobyn, Michael J; Heng, Jerry Y Y

2014-09-10

The role of surface properties, influenced by particle processing, in particle-particle interactions (powder cohesion) is investigated in this study. Wetting behaviour of mefenamic acid was found to be anisotropic by sessile drop contact angle measurements on macroscopic (>1cm) single crystals, with variations in contact angle of water from 56.3° to 92.0°. This is attributed to variations in surface chemical functionality at specific facets, and confirmed using X-ray photoelectron spectroscopy (XPS). Using a finite dilution inverse gas chromatography (FD-IGC) approach, the surface energy heterogeneity of powders was determined. The surface energy profile of different mefenamic acid crystal habits was directly related to the relative exposure of different crystal facets. Cohesion, determined by a uniaxial compression test, was also found to relate to surface energy of the powders. By employing a surface modification (silanisation) approach, the contribution from crystal shape from surface area and surface energy was decoupled. By "normalising" contribution from surface energy and surface area, needle shaped crystals were found to be ∼2.5× more cohesive compared to elongated plates or hexagonal cuboid shapes crystals. Copyright © 2014. Published by Elsevier B.V.

Preparation and characterization of Y-Fe alloy nanowires by template-assisted electrodeposition from aqueous solution

NASA Astrophysics Data System (ADS)

Wang, XiaoChao; Han, Li; Zhang, YuanYuan; Xue, ShouHong

2016-03-01

In this study, a method was proposed for the preparation of Y-Fe alloy nanowires by PC membrane template-assisted electrodeposition from aqueous solution. Citric acid acted as complexing agent was used into the solution to fabricate Y-Fe alloy nanowires. The electrolyte solution consisted of 5 g L-1 YCl3, 12.5 g L-1 FeSO·6H2O, different concentrations of citric acid , 25 g L-1 boric acid in deionized water. The energy dispersive spectroscopy (EDS) found that the content of Y in the nanowires can be controlled by citric acid concentration and the current intensity, and the content of Y could reach up to 33.16 wt%. Scanning electron microscopy (SEM), BET specific surface area (BET), and X-ray diffraction (XRD) showed that there was a shift in the structure of nanowires from semicrystalline to amorphous due to the change of Y content, and their shapes were approximately 100 nm in diameter and 6 μm in length; the surface areas of nanowires were about 3.97 m2/g. Fourier transform infrared (FTIR) spectroscopy, UV-Vis diffuse reflectance spectroscopy, and X-ray photoelectron spectroscopy (XPS) indicated the formation of Y-Fe alloy, Y2O3 and Fe2O3 existed in the outer layer of nanowires. The magnetic field applied both parallel and perpendicular to the nanowires by alternating gradient magnetometer (AGM) showed small magnetic anisotropy and low coercivity with easy axis of magnetization perpendicular to the nanowires. In addition, the magneto-optic Kerr effect (MOKE) was investigated, and a Kerr rotation angle of 29 mdeg was obtained.

Many particle spectroscopy of atoms, molecules, clusters and surfaces: international conference MPS-2016

NASA Astrophysics Data System (ADS)

Grum-Grzhimailo, Alexei N.; Popov, Yuri V.; Gryzlova, Elena V.; Solov'yov, Andrey V.

2017-07-01

The conference on Many Particle Spectroscopy of Atoms, Molecules, Clusters and Surfaces (MPS-2016) brought together near to a hundred scientists in the field of electronic, photonic, atomic and molecular collisions, and spectroscopy from around the world. We deliver an Editorial of a topical issue presenting original research results from some of the participants on both experimental and theoretical studies involving many particle spectroscopy of atoms, molecules, clusters and surfaces. Contribution to the Topical Issue "Many Particle Spectroscopy of Atoms, Molecules, Clusters and Surfaces", edited by A.N. Grum-Grzhimailo, E.V. Gryzlova, Yu.V. Popov, and A.V. Solov'yov.

Ultrasonically treated multi-walled carbon nanotubes (MWCNTs) as PtRu catalyst supports for methanol electrooxidation

NASA Astrophysics Data System (ADS)

Yang, Chunwei; Hu, Xinguo; Wang, Dianlong; Dai, Changsong; Zhang, Liang; Jin, Haibo; Agathopoulos, Simeon

In the quest of fabricating supported catalysts, experimental results of transmission electron microscopy, Raman and infrared spectroscopy indicate that ultrasonic treatment effectively functionalizes multi-walled carbon nanotubes (MWCNTs), endowing them with groups that can act as nucleation sites which can favor well-dispersed depositions of PtRu clusters on their surface. Ultrasonic treatment seems to be superior than functionalization via regular refluxing. This is confirmed by the determination of the electrochemistry active surface area (ECA) and the CO-tolerance performance of the PtRu catalysts, measured by adsorbed CO-stripping voltammetry in 0.5 M sulfuric acid solution, and the real surface area of the PtRu catalysts, evaluated by Brunauer-Emmett-Teller (BET) measurements. Finally, the effectiveness for methanol oxidation is assessed by cyclic voltammetry (CV) in a sulfuric acid and methanol electrolyte.

One-Pot synthesis of phosphorylated mesoporous carbon heterogeneous catalysts with tailored surface acidity

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

Fulvio, Pasquale F; Mahurin, Shannon Mark; Mayes, Richard T

2012-01-01

Soft-templated phosphorylated mesoporous carbons with homogeneous distributions of phosphate groups were prepared by a 'one-pot' synthesis method using mixtures of phosphoric acid with hydrochloric, or nitric acids in the presence of Pluronic F127 triblock copolymer. Adjusting the various ratios of phosphoric acid used in these mixtures resulted in carbons with distinct adsorption, structural and surface acidity properties. The pore size distributions (PSDs) from nitrogen adsorption at -196 C showed that mesoporous carbons exhibit specific surface areas as high as 551 m{sup 2}/g and mesopores as large as 13 nm. Both structural ordering of the mesopores and the final phosphate contentsmore » were strongly dependent on the ratios of H{sub 3}PO{sub 4} in the synthesis gels, as shown by transmission electron microscopy (TEM), X-ray photoelectron (XPS) and energy dispersive X-ray spectroscopy (EDS). The number of surface acid sites determined from temperature programmed desorption of ammonia (NH{sub 3}-TPD) were in the range of 0.3-1.5 mmol/g while the active surface areas are estimated to comprise 5-54% of the total surface areas. Finally, the conversion temperatures for the isopropanol dehydration were lowered by as much as 100 C by transitioning from the least acidic to the most acidic catalysts surface.« less

CTAB-assisted ultrasonic synthesis, characterization and photocatalytic properties of WO{sub 3}

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

Sánchez-Martínez, D., E-mail: dansanm@gmail.com; Gomez-Solis, C.; Torres-Martinez, Leticia M.

2015-01-15

Highlights: • WO{sub 3} 2D nanostructures were synthesized by ultrasound method assisted with CTAB. • WO{sub 3} morphology was mainly of rectangular nanoplates with a thickness of ∼50 nm. • The highest surface area value of WO{sub 3} was obtained to lowest concentration of CTAB. • WO{sub 3} activity was attributed to morphology, surface area and the addition of CTAB. • WO{sub 3} nanoplates were able to causing almost complete mineralization of rhB and IC. - Abstract: WO{sub 3} 2D nanostructures have been prepared by ultrasound synthesis method assisted with CTAB using different molar ratios. The formation of monoclinic crystalmore » structure of WO{sub 3} was confirmed by X-ray powder diffraction (XRD). The characterization of the WO{sub 3} samples was complemented by analysis of scanning electron microscopy (SEM), which revealed morphology mainly of rectangular nanoplates with a thickness of around 50 nm and length of 100–500 nm. Infrared spectroscopy (FT-IR) was used to confirm the elimination of the CTAB in the synthesized samples. The specific surface area was determinate by the BET method and by means of diffuse reflectance spectroscopy (DRS) it was determinate the band-gap energy (E{sub g}) of the WO{sub 3} samples. The photocatalytic activity of the WO{sub 3} oxide was evaluated in the degradation reactions of rhodamine B (rhB) and indigo carmine (IC) under Xenon lamp irradiation. The highest photocatalytic activity was observed in the samples containing low concentration of CTAB with morphology of rectangular nanoplates and with higher surface area value than commercial WO{sub 3}. Photodegradation of rhB and IC were followed by means of UV–vis absorption spectra. The mineralization degree of organic dyes by WO{sub 3} photocatalyst was determined by total organic carbon analysis (TOC) reaching percentages of mineralization of 92% for rhB and 50% for IC after 96 h of lamp irradiation.« less

[Influence of surface chemical properties and pore structure characteristics of activated carbon on the adsorption of nitrobenzene from aqueous solution].

PubMed

Liu, Shou-Xin; Chen, Xi; Zhang, Xian-Quan

2008-05-01

Commercial activated carbon was treated by HNO3 oxidation and then subsequently heat treated under N2 atmosphere. Effect of surface chemical properties and pore structure on the adsorption performance of nitrobenzene was investigated. N2/77K adsorption isotherm and scanning electron microscopy (SEM) were used to characterize the pore structure and surface morphology of carbon. Boehm titration, Fourier transform infrared spectroscopy (FTIR), the point of zero charge (pH(PZC)) measurement and elemental analysis were used to characterize the surface properties. The results reveal that HNO3 oxidation can modify the surface chemical properties, increase the number of acidic surface oxygen-containing groups and has trivial effect on the pore structure of carbon. Further heat treatment can cause the decomposition of surface oxygen-containing groups, and increase the external surface area and the number of mesopores. Adsorption capacity of nitrobenzene on AC(NO-T), AC(raw) and AC(NO) was 1011.31, 483.09 and 321.54 mg x g(-1), respectively. Larger external surface area and the number of meso-pores, together with the less acid surface oxygen-containing groups were the main reason for the larger adsorption capacity AC(NO-T).

Sol-gel chemical sensors for surface-enhanced Raman spectroscopy

NASA Astrophysics Data System (ADS)

Lee, Vincent Y.; Farquharson, Stuart; Kwon, Hueong-Chan; Shahriari, Mahmoud R.; Rainey, Petrie M.

1999-02-01

Surface-enhanced Raman spectroscopy (SERS) promises to be one of the most sensitive methods for chemical detection. Unfortunately, the inability of SERS to perform quantitative chemical analysis has slowed its general use in laboratories. This is largely due to the difficulty of manufacturing either active surfaces that yield reproducible enhancements, or surfaces that are capable of reversible chemical adsorption, or both. In an effort to meet this need, we have developed metal-doped sol-gels that provide surface-enhancement of Raman scattering. The porous silica network offers a unique environment for stabilizing SER active metal particles and the high surface area increases the interaction between the analyte and metal particles. This eliminates the need to concentrate the analyte on the surface by evaporating the solvent. The sol-gel is easily coated on a variety of surfaces, such as fiber optics, glass slides, or glass tubing, and can be designed into sample flow systems. Here we present the development of both gold- and silver-doped sol-gels, which have been used to coat the inside walls of glass sample vials for SERS applications. The performance of the metal-doped sol-gels was evaluated using p-aminobenzoic acid, to establish enhancement factors, detection limits, dynamic response range, reversibility, reproducibility, and suitability to commercial spectrometers. Measurements of trace chemicals, such as adenine and cocaine, are also presented.

Degradation of oxygen reduction reaction kinetics in porous La0.6Sr0.4Co0.2Fe0.8O3-δ cathodes due to aging-induced changes in surface chemistry

NASA Astrophysics Data System (ADS)

Baqué, Laura C.; Soldati, Analía L.; Teixeira-Neto, Erico; Troiani, Horacio E.; Schreiber, Anja; Serquis, Adriana C.

2017-01-01

The modification of surface composition after long-term operation is one of the most reported degradation mechanisms of (La,Sr)(Co,Fe)O3-δ (LSCFO) cathodes for Solid Oxide Fuel Cells (SOFCs). Nevertheless, its effect on the oxygen reduction reaction kinetics of porous LSCFO cathodes has not been yet reliably established. In this work, La- and Sr-enrichment at the LSCFO surface of porous cathodes has been induced after 50 h aging at 800 °C under air. Such cation redistribution can extend up to ∼400 nm depth under the LSCFO surface as detected by high resolution Scanning Transmission Electron Microscopy-Energy Dispersive Spectroscopy maps acquired inside the cathode pores. The observed surface chemical changes hamper the oxygen surface exchange reaction at the LSCFO/gas interface. Accordingly, a suitable Electrochemical Impedance Spectroscopy analysis revealed that the oxygen ion conductivity remains practically unaltered during the aging treatment while the oxygen surface exchange resistance increases up to 1.8 times. As a result, the cathode impedance response deteriorates within the 10-0.1 Hz frequency range during the aging treatment, resulting in a total cathode area specific resistance increase of 150%. The methodology adopted has demonstrated to be very valuable for studying the degradation of SOFC cathodes produced by the modification of surface composition.

Natural fiber templated TiO2 microtubes via a double soaking sol-gel route and their photocatalytic performance

NASA Astrophysics Data System (ADS)

Yang, Li; Li, Xu; Wang, Ziru; Shen, Yun; Liu, Ming

2017-10-01

TiO2 microtubes with a yam-like surface were prepared for the first time through a simple and efficient double soaking sol-gel route by utilizing Platanus acerifolia seed fibers as bio-templates. The physicochemical properties of the samples were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDX), Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), Brunauer Emmett Teller (BET) surface analysis and Ultraviolet-visible absorption spectroscopy (UV-vis). The results showed that the obtained TiO2 microtubes had an anatase phase and were composed of a smooth internal wall and a rough yam-like external wall with an average diameter of 24 μm and the wall thickness of 2 μm. The surface area and pore volume of the as-prepared TiO2 microtubes reached 128.271 m2/g and 0.149 cm3/g, respectively. The UV-vis analysis displayed a favorable extension of light absorption capacity of TiO2 microtubes. The synthetic mechanism was preliminarily discussed as well. The moisture in the natural fiber templates facilitated the mild hydrolysis of titanium sol, leaving a prime layer on the surface of the fibers, and subsequently assisted in the successful preparation of TiO2 microtubes with a yam-like surface without requiring specific control of hydrolysis. Photocatalytic experiments indicated that the as-obtained TiO2 microtubes exhibited a higher efficiency than commercial P25 in the degradation of tetracycline hydrochloride.

Fabrication of a Horizontal and a Vertical Large Surface Area Nanogap Electrochemical Sensor

PubMed Central

Hammond, Jules L.; Rosamond, Mark C.; Sivaraya, Siva; Marken, Frank; Estrela, Pedro

2016-01-01

Nanogap sensors have a wide range of applications as they can provide accurate direct detection of biomolecules through impedimetric or amperometric signals. Signal response from nanogap sensors is dependent on both the electrode spacing and surface area. However, creating large surface area nanogap sensors presents several challenges during fabrication. We show two different approaches to achieve both horizontal and vertical coplanar nanogap geometries. In the first method we use electron-beam lithography (EBL) to pattern an 11 mm long serpentine nanogap (215 nm) between two electrodes. For the second method we use inductively-coupled plasma (ICP) reactive ion etching (RIE) to create a channel in a silicon substrate, optically pattern a buried 1.0 mm × 1.5 mm electrode before anodically bonding a second identical electrode, patterned on glass, directly above. The devices have a wide range of applicability in different sensing techniques with the large area nanogaps presenting advantages over other devices of the same family. As a case study we explore the detection of peptide nucleic acid (PNA)−DNA binding events using dielectric spectroscopy with the horizontal coplanar device. PMID:27983655

Ultrasound-assisted facile synthesis of a new tantalum(V) metal-organic framework nanostructure: Design, characterization, systematic study, and CO{sub 2} adsorption performance

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

Sargazi, Ghasem, E-mail: g.sargazi@gmail.com; Young Researchers Society, Shahid Bahonar University of Kerman, Kerman, Iran; Afzali, Daryoush, E-mail: daryoush_afzali@yahoo.com

2017-06-15

This work presents a fast route for the preparation of a new Ta(V) metal-organic framework nanostructure with high surface area, significant porosity, and small size distribution. X-ray diffraction (XRD), scanning electron microscopy (SEM), Transition electron microscopy (TEM), energy dispersive spectrometer (EDS), thermo-gravimetric analysis (TGA), differential scanning calorimetry (DSC), fourier transform infrared spectroscopy (FTIR), CHNS/O elemental analyser, and Brunauer-Emmett-Teller (BET) surface area analysis were applied to characterize the synthesized product. Moreover, the influences of ultrasonic irradiation including temperature, time, and power on different features of the final products were systematically studied using 2{sup k-1} factorial design experiments, and the response surfacemore » optimization was used for determining the best welding parameter combination. The results obtained from analyses of variances showed that ultrasonic parameters affected the size distribution, thermal behaviour, and surface area of Ta-MOF samples. Based on response surface methodology, Ta-MOF could be obtained with mean diameter of 55 nm, thermal stability of 228 °C, and high surface area of 2100 m{sup 2}/g. The results revealed that the synthesized products could be utilized in various applications such as a novel candidate for CO{sub 2} adsorption. - Graphical abstract: A facile route was used for fabrication of a new metal -organic framework based on tantalum nanostructures that have high surface area, considerable porosity, homogenous morphology, and small size distribution.« less

Nanostructured diamond layers enhance the infrared spectroscopy of biomolecules.

PubMed

Kozak, Halyna; Babchenko, Oleg; Artemenko, Anna; Ukraintsev, Egor; Remes, Zdenek; Rezek, Bohuslav; Kromka, Alexander

2014-03-04

We report on the fabrication and practical use of high-quality optical elements based on Au mirrors coated with diamond layers with flat, nanocolumnar, and nanoporous morphologies. Diamond layers (100 nm thickness) are grown at low temperatures (about 300 °C) from a methane, carbon dioxide, and hydrogen gas mixture by a pulsed microwave plasma system with linear antennas. Using grazing angle reflectance (GAR) Fourier transform infrared spectroscopy with p-polarized light, we compare the IR spectra of fetal bovine serum proteins adsorbed on diamond layers with oxidized (hydrophilic) surfaces. We show that the nanoporous diamond layers provide IR spectra with a signal gain of about 600% and a significantly improved sensitivity limit. This is attributed to its enhanced internal surface area. The improved sensitivity enabled us to distinguish weak infrared absorption peaks of <10-nm-thick protein layers and thereby to analyze the intimate diamond-molecule interface.

Surface Evaluation by X-Ray Photoelectron Spectroscopy of High Performance Polyimide Foams After Exposure to Oxygen Plasma

NASA Technical Reports Server (NTRS)

Melendez, Orlando; Hampton, Michael D.; Williams, Martha K.; Brown, Sylvia F.; Nelson, Gordon L.; Weiser, Erik S.

2002-01-01

Aromatic polyimides have been attractive in the aerospace and electronics industries for applications such as cryogenic insulation, flame retardant panels and structural subcomponents. Newer to the arena of polyimides is the synthesis of polyimide foams and their applications. In the present work, three different, closely related, polyimide foams developed by NASA Langley Research Center (LaRC) are studied by X-ray Photoelectron Spectroscopy (XPS) after exposure to radio frequency generated Oxygen Plasma. Although polyimide films exposure to atomic oxygen and plasma have been studied previously and reported, the data relate to films and not foams. Foams have much more surface area and thus present new information to be explored. Understanding degradation mechanisms and properties versus structure, foam versus solid is of interest and fundamental to the application and protection of foams exposed to atomic oxygen in Low Earth Orbit (LEO).

Functionalization of CNTs surface with phosphonuim based deep eutectic solvents for arsenic removal from water

NASA Astrophysics Data System (ADS)

AlOmar, Mohamed Khalid; Alsaadi, Mohammed Abdulhakim; Hayyan, Maan; Akib, Shatirah; Hashim, Mohd Ali

2016-12-01

Herein, we present the use of deep eutectic solvent (DES) as functionalization agents for carbon nanotubes (CNTs) to form novel adsorbents for removal of arsenic ions (As3+) from water. Two DESs systems were prepared using methyltriphenylphosphonium bromide (MTPB) and benzyltriphenylphosphonium chloride (BTPC) as salts, in conjugation with glycerol (Gly) as a hydrogen bond donor. The resulting novel adsorbents were characterized using thermogravimetric analysis (TGA), Zeta potential, Raman spectroscopy, Fourier transform infrared (FTIR) spectroscopy, XRD, EDX, FESEM, and BET surface area. Optimization studies were carried out utilizing RSM-CCD experimental design to estimate the optimum removal conditions for each adsorbent. The adsorption experimental data of both adsorbents were found to fit well with pseudo-second-order kinetics model, as well as with Langmuir and Freundlich adsorption isotherm models. The maximum adsorption capacity of a MTPB-DES-functionalized CNTs adsorbent was 23.4 mg/g.

Hierarchical carbon nanopetal/polypyrrole nanocomposite electrodes with brush-like architecture for supercapacitors.

PubMed

Cherusseri, Jayesh; Kar, Kamal K

2016-03-28

Hierarchical 3D nanocomposite electrodes with tube brush-like morphology are synthesized by electrochemically depositing polypyrrole (PPY) on carbon nanopetal (CNP) coated carbon fibers (CFs). Initially CNPs are synthesized on CF substrate by chemical vapour deposition. The CNPs synthesized on CF (CNPCF) are further used as an electrically conducting large surface area bearing template for the electropolymerization of PPY in order to fabricate CNPCF-PPY nanocomposite electrodes for supercapacitors (SCs). The CF in CNPCF-PPY nanocomposite functions as (i) a mechanical support for the CNPs, (ii) a current collector for the SC cell and also (iii) to prevent the agglomeration of CNPs within the CNPCF-PPY nanocomposite. Transmission electron microscopy and scanning electron microscopy are used to examine the surface morphology of CNPCF-PPY nanocomposites. The chemical structure of the nanocomposites is analysed by Fourier transform infrared spectroscopy. X-Ray photoelectron spectroscopy has been used to understand the chemical bonding states of the hierarchical CNPCF-PPY nanocomposites. The electrochemical properties of symmetric type CNPCF-PPY SC cells are examined by electrochemical impedance spectroscopy, cyclic voltammetry and galvanostatic charge-discharge measurements. The hierarchical CNPCF-PPY SC exhibits a maximum gravimetric capacitance of 280.4 F g(-1) and an area specific capacitance of 210.3 mF cm(-2) at a current density of 0.42 mA cm(-2). The CNPCF-PPY SC cell exhibits good cycling stability of more than 5000 cycles. The present study proclaims the development of a novel lightweight SC with high-performance.

Structure of nanoporous carbon materials for supercapacitors

NASA Astrophysics Data System (ADS)

Volperts, A.; Mironova-Ulmane, N.; Sildos, I.; Vervikishko, D.; Shkolnikov, E.; Dobele, G.

2012-08-01

Activated carbons with highly developed porous structure and nanosized pores (8 - 11 Å) were prepared from alder wood using thermochemical activation method with sodium hydroxide. Properties of the obtained activated carbons were examined by benzene and nitrogen sorption, X-Ray diffraction and Raman spectroscopy. Tests of activated carbons as electrodes in supercapacitors were performed as well. It was found that specific surface area of above mentioned activated carbons was 1800 m2/g (Dubinin - Radushkevich). Raman spectroscopy demonstrated the presence of ordered and disordered structures of graphite origin. The performance of activated carbons as electrodes in supercapacitors have shown superior results in comparison with electrodes made with commercial carbon tissues.

Surface studies on superhydrophobic and oleophobic polydimethylsiloxane-silica nanocomposite coating system

NASA Astrophysics Data System (ADS)

Basu, Bharathibai J.; Dinesh Kumar, V.; Anandan, C.

2012-11-01

Superhydrophobic and oleophobic polydimethylsiloxane (PDMS)-silica nanocomposite double layer coating was fabricated by applying a thin layer of low surface energy fluoroalkyl silane (FAS) as topcoat. The coatings exhibited WCA of 158-160° and stable oleophobic property with oil CA of 79°. The surface morphology was characterized by field emission scanning electron microscopy (FESEM) and surface chemical composition was determined by energy dispersive X-ray spectrometery (EDX) and X-ray photoelectron spectroscopy (XPS). FESEM images of the coatings showed micro-nano binary structure. The improved oleophobicity was attributed to the combined effect of low surface energy of FAS and roughness created by the random distribution of silica aggregates. This is a facile, cost-effective method to obtain superhydrophobic and oleophobic surfaces on larger area of various substrates.

In situ biosensing of the nanomechanical property and electrochemical spectroscopy of Streptococcus mutans-containing biofilms

NASA Astrophysics Data System (ADS)

Haochih Liu, Bernard; Li, Kun-Lin; Kang, Kai-Li; Huang, Wen-Ke; Liao, Jiunn-Der

2013-07-01

This work presents in situ biosensing approaches to study the nanomechanical and electrochemical behaviour of Streptococcus mutans biofilms under different cultivation conditions and microenvironments. The surface characteristics and sub-surface electrochemistry of the cell wall of S. mutans were measured by atomic force microscopy (AFM) based techniques to monitor the in situ biophysical status of biofilms under common anti-pathogenic procedures such as ultraviolet (UV) radiation and alcohol treatment. The AFM nanoindentation suggested a positive correlation between nanomechanical strength and the level of UV radiation of S. mutans; scanning impedance spectroscopy of dehydrated biofilms revealed reduced electrical resistance that is distinctive from that of living biofilms, which can be explained by the discharge of cytoplasm after alcohol treatment. Furthermore, the localized elastic moduli of four regions of the biofilm were studied: septum (Z-ring), cell wall, the interconnecting area between two cells and extracellular polymeric substance (EPS) area. The results indicated that cell walls exhibit the highest elastic modulus, followed by Z-ring, interconnect and EPS. Our approach provides an effective alternative for the characterization of the viability of living cells without the use of biochemical labelling tools such as fluorescence dyeing, and does not rely on surface binding or immobilization for detection. These AFM-based techniques can be very promising approaches when the conventional methods fall short.

Immobilization of Hg(II) in water with polysulfide-rubber (PSR) polymer-coated activated carbon.

PubMed

Kim, Eun-Ah; Seyfferth, Angelia L; Fendorf, Scott; Luthy, Richard G

2011-01-01

An effective mercury removal method using polymer-coated activated carbon was studied for possible use in water treatment. In order to increase the affinity of activated carbon for mercury, a sulfur-rich compound, polysulfide-rubber (PSR) polymer, was effectively coated onto the activated carbon. The polymer was synthesized by condensation polymerization between sodium tetrasulfide and 1,2-dichloroethane in water. PSR-mercury interactions and Hg-S bonding were elucidated from x-ray photoelectron spectroscopy, and Fourier transform infra-red spectroscopy analyses. The sulfur loading levels were controlled by the polymer dose during the coating process and the total surface area of the activated carbon was maintained for the sulfur loading less than 2 wt%. Sorption kinetic studies showed that PSR-coated activated carbon facilitates fast reaction by providing a greater reactive surface area than PSR alone. High sulfur loading on activated carbon enhanced mercury adsorption contributing to a three orders of magnitude reduction in mercury concentration. μ-X-ray absorption near edge spectroscopic analyses of the mercury bound to activated carbon and to PSR on activated carbon suggests the chemical bond with mercury on the surface is a combination of Hg-Cl and Hg-S interaction. The pH effect on mercury removal and adsorption isotherm results indicate competition between protons and mercury for binding to sulfur at low pH. Copyright © 2010. Published by Elsevier Ltd.

Real-time Full-spectral Imaging and Affinity Measurements from 50 Microfluidic Channels using Nanohole Surface Plasmon Resonance†

PubMed Central

Lee, Si Hoon; Lindquist, Nathan C.; Wittenberg, Nathan J.; Jordan, Luke R.; Oh, Sang-Hyun

2012-01-01

With recent advances in high-throughput proteomics and systems biology, there is a growing demand for new instruments that can precisely quantify a wide range of receptor-ligand binding kinetics in a high-throughput fashion. Here we demonstrate a surface plasmon resonance (SPR) imaging spectroscopy instrument capable of extracting binding kinetics and affinities from 50 parallel microfluidic channels simultaneously. The instrument utilizes large-area (~cm2) metallic nanohole arrays as SPR sensing substrates and combines a broadband light source, a high-resolution imaging spectrometer and a low-noise CCD camera to extract spectral information from every channel in real time with a refractive index resolution of 7.7 × 10−6. To demonstrate the utility of our instrument for quantifying a wide range of biomolecular interactions, each parallel microfluidic channel is coated with a biomimetic supported lipid membrane containing ganglioside (GM1) receptors. The binding kinetics of cholera toxin b (CTX-b) to GM1 are then measured in a single experiment from 50 channels. By combining the highly parallel microfluidic device with large-area periodic nanohole array chips, our SPR imaging spectrometer system enables high-throughput, label-free, real-time SPR biosensing, and its full-spectral imaging capability combined with nanohole arrays could enable integration of SPR imaging with concurrent surface-enhanced Raman spectroscopy. PMID:22895607

The effect of nanoparticles size on photocatalytic and antimicrobial properties of Ag-Pt/TiO2 photocatalysts

NASA Astrophysics Data System (ADS)

Zielińska-Jurek, Anna; Wei, Zhishun; Wysocka, Izabela; Szweda, Piotr; Kowalska, Ewa

2015-10-01

Ag-Pt-modified TiO2 nanocomposites were synthesized using the sol-gel method. Bimetallic modified TiO2 nanoparticles exhibited improved photocatalytic activity under visible-light irradiation, better than monometallic Ag/TiO2 and Pt/TiO2 nanoparticles (NPs). All modified powders showed localized surface plasmon resonance (LSPR) in visible region. The photocatalysts' characteristics by X-ray diffractometry (XRD), scanning transmission electron microscopy (STEM), diffuse reflectance spectroscopy (DRS), X-ray photoelectron spectroscopy (XPS), nitrogen adsorption (BET method for specific surface area) showed that sample with the highest photocatalytic activity had anatase structure, about 93 m2/g specific surface area, maximum plasmon absorption at ca. 420 nm and contained small NPs of silver of 6 nm and very fine platinum NPs of 3 nm. The photocatalytic activity was estimated by measuring the decomposition rate of phenol in 0.2 mM aqueous solution under Vis and UV/vis light irradiation. It was found that size of platinum was decisive for the photocatalytic activity under visible light irradiation, i.e., the smaller Pt NPs were, the higher was photocatalytic activity. While, antimicrobial activities, estimated for bacteria Escherichia coli and Staphylococcus aureus, and pathogenic fungi belonging to Candida family, were only observed for photocatalysts containing silver, i.e., Ag/TiO2 and Ag-Pt/TiO2 nanocomposites.

Surface active gold nanoparticles biosynthesis by new approach for bionanocatalytic activity.

PubMed

Vasantharaj, S; Sripriya, N; Shanmugavel, M; Manikandan, E; Gnanamani, A; Senthilkumar, P

2018-02-01

In the present day, nanotechnology is one of the most promising leading scientific and potentials areas in modern key technology development toward to the humankind. The synthesis of noble metal nanoparticles (NPs) is an expanding research area due to the possible applications for the development of bio-medical applications. Eco-friendly approach for the biosynthesis of gold nanoparticles (AuNPs) using the aqueous extract from Ruellia tuberosa and Phyllanthus acidus (leaf and twig) for the first time. Surface active AuNPs were characterized by UV-Vis spectroscopy, FTIR (Fourier transform infrared) spectroscopy, DSC (differential scanning colorimetry), DLS (dynamic light scattering) and environmental SEM (scanning electron microscope) analysis at room temperature (RT). Enhanced surface plasmon resonance (SPR) absorbance UV visible optical spectra were detected in the range of 552, 548, 558 and 536 nm. SEM and DLS (transmission mode) analysis confirmed the morphology of the nanoparticles to be spherical with the average size in the range of 88.37, 94.31, 82.23 and 81.36 nm. Further they have enhanced the enzyme activity on α-amylase, cellulase, and xylanase. The results suggest that the phyto-fabricated AuNPs from R. tuberosa and P. acidus is simple, less expensive, eco-friendly, green synthesis and also can be exploited for the potential future industrial and bio-medical applications. Copyright © 2018 Elsevier B.V. All rights reserved.

Facile fabrication of superhydrophobic hybrid nanotip and nanopore arrays as surface-enhanced Raman spectroscopy substrates

NASA Astrophysics Data System (ADS)

Li, Yuxin; Li, Juan; Wang, Tiankun; Zhang, Zhongyue; Bai, Yu; Hao, Changchun; Feng, Chenchen; Ma, Yingjun; Sun, Runguang

2018-06-01

We demonstrate the fabrication of superhydrophobic hybrid nanotip and nanopore arrays (NTNPAs) that can act as sensitive surface-enhanced Raman spectroscopy (SERS) substrates. The large-area substrates were fabricated by following a facile, low-cost process consisting of the one-step voltage-variation anodization of Al foil, followed by Ag nanoparticle deposition and fluorosilane (FS) modification. Uniformly distributed, large-area (5 × 5 cm2) NTNPAs can be obtained rapidly by anodizing Al foil for 1560 s followed by Ag deposition for 400 s, which showed good SERS reproducibility as using1 μM Rhodamine 6G (R6G) as analyte. SERS performances of superhydrophobic NTNPAs with different FS modification and Ag nanoparticle deposition orders were also studied. The nanosamples with FS modification followed by Ag nanoparticle deposition (FS-Ag) showed better SERS sensitivity than the nanosamples with Ag nanoparticle deposition followed by FS modification (Ag-FS). The detection limit of a directly dried R6G droplet can reach 10-8 M on the FS-Ag nanosamples. The results can help create practical high sensitive SERS substrates, which can be used in developing advanced bio- and chemical sensors.

Influence of bases on hydrothermal synthesis of titanate nanostructures

NASA Astrophysics Data System (ADS)

Sikhwivhilu, Lucky M.; Sinha Ray, Suprakas; Coville, Neil J.

2009-03-01

A hydrothermal treatment of titanium dioxide (TiO2) with various bases (i.e., LiOH, NaOH, KOH, and NH4OH) was used to prepare materials with unique morphologies, relatively small crystallite sizes, and large specific surface areas. The experimental results show that the formation of TiO2 is largely dependent on the type, strength and concentration of a base. The effect of the nature of the base used and the concentration of the base on the formation of nanostructures were investigated using X-ray diffraction, Raman spectroscopy, transmission and scanning electron microscopy, as well as surface area measurements. Sodium hydroxide (NaOH) and potassium hydroxide (KOH) were both used to transform the morphology of starting TiO2 material.

Characterization of the adsorption of water vapor and chlorine on microcrystalline silica

NASA Technical Reports Server (NTRS)

Skiles, J. A.; Wightman, J. P.

1979-01-01

The characterization of water adsorption on silica is necessary to an understanding of how hydrogen chloride interacts with silica. The adsorption as a function of outgas temperatures of silica and as a function of the isotherm temperature was studied. Characterization of the silica structure by infrared analysis, X-ray diffraction and differential scanning calorimetry, surface area determinations, characterization of the sample surface by electron spectroscopy for chemical analysis (ESCA), and determinations of the heat of immersion in water of silica were investigated. The silica with a scanning electron microscope was examined.

Diamond heteroepitaxial lateral overgrowth

DOE PAGES

Tang, Y. -H.; Bi, B.; Golding, B.

2015-02-24

A method of diamond heteroepitaxial lateral overgrowth is demonstrated which utilizes a photolithographic metal mask to pattern a thin (001) epitaxial diamond surface. Significant structural improvement was found, with a threading dislocation density reduced by two orders of magnitude at the top surface of a thick overgrown diamond layer. In the initial stage of overgrowth, a reduction of diamond Raman linewidth in the overgrown area was also realized. Thermally-induced stress and internal stress were determined by Raman spectroscopy of adhering and delaminated diamond films. As a result, the internal stress is found to decrease as sample thickness increases.

Use of different rapid mixing devices for controlling the properties of magnetite nanoparticles produced by precipitation

NASA Astrophysics Data System (ADS)

Wei, Li; Hervé, Muhr; Edouard, Plasari

2012-03-01

Magnetite nanoparticles were precipitated by the classic Massart's method in a 2.5 L stirred tank reactor where the injection of reagent solutions was effectuated by different micro-mixers (T-tube and Hartridge-Roughton rapid mixing devices). The specific surface area, the average particle size and the particle size distribution were highly influenced by changing operating parameters. Laser Diffraction, BET adsorption, Energy-Dispersive X-ray Spectroscopy (EDX), Raman spectroscopy and Transmission Electron Microscopy (TEM) were used for characterizing magnetite nanoparticles. Especially, Hartridge-Roughton micromixer appears to be the most efficient mixing device for producing magnetite nanoparticles. The average particle size of magnetite nanoparticles prepared by Hartridge-Roughton rapid mixing device was less than 10 nm and the EDX and Raman spectroscopy shows that the particle purity is quite high.

Facile preparation of dendritic Ag-Pd bimetallic nanostructures on the surface of Cu foil for application as a SERS-substrate

NASA Astrophysics Data System (ADS)

Yi, Zao; Tan, Xiulan; Niu, Gao; Xu, Xibin; Li, Xibo; Ye, Xin; Luo, Jiangshan; Luo, Binchi; Wu, Weidong; Tang, Yongjian; Yi, Yougen

2012-05-01

Dendritic Ag-Pd bimetallic nanostructures have been synthesized on the surface of Cu foil via a multi-stage galvanic replacement reaction (MGRR) of Ag dendrites in a Na2PdCl4 solution. After five stages of replacement reaction, one obtained structures with protruding Ag-Pd flakes; these will mature into many porous structures with a few Ag atoms that are left over dendrites. The dendritic Ag-Pd bimetallic nanostructures were characterized by transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray (EDX), selected area electron diffraction (SAED) and X-ray photoelectron spectroscopy (XPS). The morphology of the products strongly depended on the stage of galvanic replacement reaction and reaction temperature. The morphology and composition-dependent surface-enhanced Raman scattering (SERS) of the as-synthesized Ag-Pd bimetallic nanostructures were investigated. The effectiveness of these dendritic Ag-Pd bimetallic nanostructures on the surface of Cu foil as substrates toward SERS detection was evaluated by using rhodamine 6G (R6G) as a probe molecule. The results indicate that as-synthesized dendritic Ag-Pd bimetallic nanostructures are good candidates for SERS spectroscopy.

Magnetic and interface properties of the core-shell Fe3O4/Au nanocomposites

NASA Astrophysics Data System (ADS)

Baskakov, A. O.; Solov'eva, A. Yu.; Ioni, Yu. V.; Starchikov, S. S.; Lyubutin, I. S.; Khodos, I. I.; Avilov, A. S.; Gubin, S. P.

2017-11-01

Core-shell Fe3O4/Au nanostructures were obtained with an advanced method of two step synthesis and several complementary methodics were applied for investigation structural and magnetic properties of the samples. Along with X-ray diffraction and transmission electron microscopy, electron diffraction, optical, Raman and Mössbauer spectroscopy were used for nanoparticle characterization. It was established that the physical and structural properties Fe3O4/Au nanocomposites are specific of intrinsic properties of gold and magnetite. Mössbauer and Raman spectroscopy data indicated that magnetite was in a nonstoichiometric state with an excess of trivalent iron both in the initial Fe3O4 nanoparticles and in the Fe3O4/Au nanocomposites. As follows from the Mössbauer data, magnetic properties of iron ions in the internal area (in core) and in the surface layer of magnetite nanoparticles are different due to the rupture of exchange bonds at the particles surface. This leads to decrease in an effective magnetic moment at the surface. Gold atoms at the interface of the composites interact with dangling bonds of magnetite and stabilize the magnetic properties of the surface layers of magnetite.

Electro and Magneto-Electropolished Surface Micro-Patterning on Binary and Ternary Nitinol

PubMed Central

Munroe, Norman; McGoron, Anthony

2012-01-01

In this study, an Atomic Force Microscopy (AFM) roughness analysis was performed on non-commercial Nitinol alloys with Electropolished (EP) and Magneto-Electropolished (MEP) surface treatments and commercially available stents by measuring Root-Mean-Square (RMS), Average Roughness (Ra), and Surface Area (SA) values at various dimensional areas on the alloy surfaces, ranging from (800 × 800 nm) to (115 × 115μm), and (800 × 800 nm) to (40 × 40 μm) on the commercial stents. Results showed that NiTi-Ta 10 wt% with an EP surface treatment yielded the highest overall roughness, while the NiTi-Cu 10 wt% alloy had the lowest roughness when analyzed over (115 × 115 μm). Scanning Electron Microscopy (SEM) and Energy Dispersive Spectroscopy (EDS) analysis revealed unique surface morphologies for surface treated alloys, as well as an aggregation of ternary elements Cr and Cu at grain boundaries in MEP and EP surface treated alloys, and non-surface treated alloys. Such surface micro-patterning on ternary Nitinol alloys could increase cellular adhesion and accelerate surface endothelialization of endovascular stents, thus reducing the likelihood of in-stent restenosis and provide insight into hemodynamic flow regimes and the corrosion behavior of an implantable device influenced from such surface micro-patterns. PMID:22754200

A hybrid MBE-based growth method for large-area synthesis of stacked hexagonal boron nitride/graphene heterostructures

NASA Astrophysics Data System (ADS)

Wofford, Joseph M.; Nakhaie, Siamak; Krause, Thilo; Liu, Xianjie; Ramsteiner, Manfred; Hanke, Michael; Riechert, Henning; J. Lopes, J. Marcelo

2017-02-01

Van der Waals heterostructures combining hexagonal boron nitride (h-BN) and graphene offer many potential advantages, but remain difficult to produce as continuous films over large areas. In particular, the growth of h-BN on graphene has proven to be challenging due to the inertness of the graphene surface. Here we exploit a scalable molecular beam epitaxy based method to allow both the h-BN and graphene to form in a stacked heterostructure in the favorable growth environment provided by a Ni(111) substrate. This involves first saturating a Ni film on MgO(111) with C, growing h-BN on the exposed metal surface, and precipitating the C back to the h-BN/Ni interface to form graphene. The resulting laterally continuous heterostructure is composed of a top layer of few-layer thick h-BN on an intermediate few-layer thick graphene, lying on top of Ni/MgO(111). Examinations by synchrotron-based grazing incidence diffraction, X-ray photoemission spectroscopy, and UV-Raman spectroscopy reveal that while the h-BN is relaxed, the lattice constant of graphene is significantly reduced, likely due to nitrogen doping. These results illustrate a different pathway for the production of h-BN/graphene heterostructures, and open a new perspective for the large-area preparation of heterosystems combining graphene and other 2D or 3D materials.

Gold-Gilded Zinc Oxide Nanodiamonds: Plasmonic and Morphological Effects

NASA Astrophysics Data System (ADS)

Khan, G. R.; Khan, R. A.

The novel properties, diverse applications and device performance of nanocomposites can be greatly modulated through astute combination of plasmonic and morphological effects. The biosensing sensitivity, semiconducting capability, photocatalytic efficiency and antibacterial efficacy of ZnO nanostructures can be enhanced by a diamond-like morphology of ZnO via incorporation of plasmonic gold owing to their exceptional specific surface area, outstanding photoluminescence and excellent biocompatibility. Toward the realization of this goal, Au-Zno nanodiamonds have been successfully synthesized by a microwave assisted solution phase route without use of any costly solvents, surfactants, substrates, post-synthesis treatment or hazardous ingredients. It shows the ability to control the concentration of Au nanoparticles in ZnO and the evolution of its growth in diamond shape. The synthesized nanocomposites were characterized by high-resolution measurements such as transmission electron microscopy (TEM), diffused reflectance spectroscopy (DRS), energy dispersive X-ray spectroscopy (EDX), X-ray diffractometory (XRD), Raman spectroscopy and Fourier transform infrared spectroscopy (FT-IR), and the results discussed in detail.

Synthesis of ZnO nanopencils using wet chemical method and its investigation as LPG sensor

NASA Astrophysics Data System (ADS)

Shimpi, Navinchandra G.; Jain, Shilpa; Karmakar, Narayan; Shah, Akshara; Kothari, D. C.; Mishra, Satyendra

2016-12-01

ZnO nanopencils (NPCs) were prepared by a novel wet chemical process, using triethanolamine (TEA) as a mild base, which is relatively simple and cost effective method as compared to hydrothermal method. ZnO NPCs were characterized using powder X-ray diffraction (XRD), Fourier Transform Infra-Red (FTIR) spectroscopy in mid-IR and far-IR regions, X-ray Photoelectron Spectroscopy (XPS), UV-vis (UV-vis) absorption spectroscopy, room temperature Photoluminescence (PL) spectroscopy and Field Emission Scanning Electron Microscopy (FESEM). ZnO NPCs obtained, were highly pure, uniform and monodispersed.XRD pattern indicated hexagonal unit cell structure with preferred orientation along the c-axis. Sensing behaviour of ZnO NPCs was studied towards Liquefied Petroleum Gas (LPG) at different operating temperatures. The study shows that ZnO NPCs were most sensitive and promising candidate for detection of LPG at 250 °C with gas sensitivity > 60%. The high response towards LPG is due to high surface area of ZnO NPCs and their parallel alignment.

Browning phenomenon of medieval stained glass windows.

PubMed

Ferrand, Jessica; Rossano, Stéphanie; Loisel, Claudine; Trcera, Nicolas; van Hullebusch, Eric D; Bousta, Faisl; Pallot-Frossard, Isabelle

2015-04-07

In this work, three pieces of historical on-site glass windows dated from the 13th to 16th century and one archeological sample (8th century) showing Mn-rich brown spots at their surface or subsurface have been characterized by optical microscopy and Scanning Electron Microscopy coupled with Energy Dispersive X-ray spectroscopy. The oxidation state of Mn as well as the Mn environment in the alteration phase have been characterized by X-ray absorption spectroscopy at the Mn K-edge. Results show that the oxidation state of Mn and therefore the nature of the alteration phase varies according to the sample considered and is correlated with the extent of the brown alteration. The larger the brown areas the more oxidized the Mn. However, by contrast with literature, the samples presenting the more extended brown areas are not similar to pyrolusite and contain Mn mainly under a (+III) oxidation state.

Conformational changes of a calix[8]arene derivative at the air-water interface.

PubMed

de Miguel, Gustavo; Pedrosa, José M; Martín-Romero, María T; Muñoz, Eulogia; Richardson, Tim H; Camacho, Luis

2005-03-10

The particular behavior of a p-tert-butyl calix[8]arene derivative (C8A) has been studied at the air-water interface using surface pressure-area isotherms, surface potential-area isotherms, film relaxation measurements, Brewster angle microscopy (BAM), and infrared spectroscopy for Langmuir-Blodgett films. Thus, it is observed that the properties of the film, for example, isotherms, domain formation, and FTIR spectra, recorded during the first compression cycle differ appreciably from those during the second compression and following cycles. The results obtained are interpreted on the basis of the conformational changes of the C8A molecules by surface pressure, allowing us to inquire into the inter- and intramolecular interactions (hydrogen bonds) of those molecules. Thus, the compression induces changes in the kind of hydrogen bonds from intra- and intermolecular with other C8A molecules to hydrogen bonds with water molecules.

Enhanced methane emissions from oil and gas exploration areas to the atmosphere--the central Bohai Sea.

PubMed

Zhang, Yong; Zhao, Hua-de; Zhai, Wei-dong; Zang, Kun-peng; Wang, Ju-ying

2014-04-15

The distributions of dissolved methane in the central Bohai Sea were investigated in November 2011, May 2012, July 2012, and August 2012. Methane concentration in surface seawater, determined using an underway measurement system combined with wavelength-scanned cavity ring-down spectroscopy, showed marked spatiotemporal variations with saturation ratio from 107% to 1193%. The central Bohai Sea was thus a source of atmospheric methane during the survey periods. Several episodic oil and gas spill events increased surface methane concentration by up to 4.7 times and raised the local methane outgassing rate by up to 14.6 times. This study demonstrated a method to detect seafloor CH4 leakages at the sea surface, which may have applicability in many shallow sea areas with oil and gas exploration activities around the world. Copyright © 2014 Elsevier Ltd. All rights reserved.

Three-dimensional scanning force/tunneling spectroscopy at room temperature.

PubMed

Sugimoto, Yoshiaki; Ueda, Keiichi; Abe, Masayuki; Morita, Seizo

2012-02-29

We simultaneously measured the force and tunneling current in three-dimensional (3D) space on the Si(111)-(7 × 7) surface using scanning force/tunneling microscopy at room temperature. The observables, the frequency shift and the time-averaged tunneling current were converted to the physical quantities of interest, i.e. the interaction force and the instantaneous tunneling current. Using the same tip, the local density of states (LDOS) was mapped on the same surface area at constant height by measuring the time-averaged tunneling current as a function of the bias voltage at every lateral position. LDOS images at negative sample voltages indicate that the tip apex is covered with Si atoms, which is consistent with the Si-Si covalent bonding mechanism for AFM imaging. A measurement technique for 3D force/current mapping and LDOS imaging on the equivalent surface area using the same tip was thus demonstrated.

Note: A novel technique for analysis of aqueous solutions by laser-induced breakdown spectroscopy

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

Rusak, D. A.; Bell, Z. T.; Anthony, T. P.

2015-11-15

Surface-enhanced Raman spectroscopy (SERS) substrates typically consist of gold or silver nanoparticles deposited on a non-conductive substrate. In Raman spectroscopy, the nanoparticles produce an enhancement of the electromagnetic field which, in turn, leads to greater electronic excitation of molecules in the local environment. Here, we show that these same surfaces can be used to enhance the signal-to-noise ratio obtained in laser-induced breakdown spectroscopy of aqueous solutions. In this case, the SERS substrates not only lower breakdown thresholds and lead to more efficient plasma initiation but also provide an appropriately wettable surface for the deposition of the liquid. We refer tomore » this technique as surface-enhanced laser-induced breakdown spectroscopy.« less

NMR imaging and spectroscopy of the mammalian central nervous system after heavy ion radiation

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

Richards, T.

NMR imaging, NMR spectroscopic, and histopathologic techniques were used to study the proton relaxation time and related biochemical changes in the central nervous system after helium beam in vivo irradiation of the rodent brain. The spectroscopic observations reported in this dissertation were made possible by development of methods for measuring the NMR parameters of the rodent brain in vivo and in vitro. The methods include (1) depth selective spectroscopy using an optimization of rf pulse energy based on a priori knowledge of N-acetyl aspartate and lipid spectra of the normal brain, (2) phase-encoded proton spectroscopy of the living rodent usingmore » a surface coil, and (3) dual aqueous and organic tissue extraction technique for spectroscopy. Radiation induced increases were observed in lipid and p-choline peaks of the proton spectrum, in vivo. Proton NMR spectroscopy measurements on brain extracts (aqueous and organic solvents) were made to observe chemical changes that could not be seen in vivo. Radiation-induced changes were observed in lactate, GABA, glutamate, and p-choline peak areas of the aqueous fraction spectra. In the organic fraction, decreases were observed in peak area ratios of the terminal-methyl peaks, the N-methyl groups of choline, and at a peak at 2.84 ppM (phosphatidyl ethanolamine and phosphatidyl serine resonances) relative to TMS. With histology and Evans blue injections, blood-brain barrier alternations were seen as early as 4 days after irradiation. 83 references, 53 figures.« less

Conformal atomic layer deposition of alumina on millimeter tall, vertically-aligned carbon nanotube arrays.

PubMed

Stano, Kelly L; Carroll, Murphy; Padbury, Richard; McCord, Marian; Jur, Jesse S; Bradford, Philip D

2014-11-12

Atomic layer deposition (ALD) can be used to coat high aspect ratio and high surface area substrates with conformal and precisely controlled thin films. Vertically aligned arrays of multiwalled carbon nanotubes (MWCNTs) with lengths up to 1.5 mm were conformally coated with alumina from base to tip. The nucleation and growth behaviors of Al2O3 ALD precursors on the MWCNTs were studied as a function of CNT surface chemistry. CNT surfaces were modified through a series of post-treatments including pyrolytic carbon deposition, high temperature thermal annealing, and oxygen plasma functionalization. Conformal coatings were achieved where post-treatments resulted in increased defect density as well as the extent of functionalization, as characterized by X-ray photoelectron spectroscopy and Raman spectroscopy. Using thermogravimetric analysis, it was determined that MWCNTs treated with pyrolytic carbon and plasma functionalization prior to ALD coating were more stable to thermal oxidation than pristine ALD coated samples. Functionalized and ALD coated arrays had a compressive modulus more than two times higher than a pristine array coated for the same number of cycles. Cross-sectional energy dispersive X-ray spectroscopy confirmed that Al2O3 could be uniformly deposited through the entire thickness of the vertically aligned MWCNT array by manipulating sample orientation and mounting techniques. Following the ALD coating, the MWCNT arrays demonstrated hydrophilic wetting behavior and also exhibited foam-like recovery following compressive strain.

Influence of Surface Modification on the Microstructure and Thermo-Mechanical Properties of Bamboo Fibers

PubMed Central

Zhang, Xiaoping; Wang, Fang; Keer, Leon M.

2015-01-01

The objective of this study is to investigate the effect of surface treatment on the morphology and thermo-mechanical properties of bamboo fibers. The fibers are subjected to an alkali treatment using 4 wt % sodium hydroxide (NaOH) for 1 h. Mechanical measurements show that the present concentration has an insignificant effect on the fiber tensile strength. In addition, systematic experimental results characterizing the morphological aspects and thermal properties of the bamboo fibers are analyzed by scanning electron microscopy, Fourier transform infrared spectroscopy, thermogravimetric analysis, and differential scanning calorimetry. It is found that an alkali treatment may increase the effective surface area, which is in turn available for superior bonding with the matrix. Fourier transform infrared spectroscopy analysis reveals that the alkali treatment leads to a gradual removal of binding materials, such as hemicellulose and lignin from the bamboo fiber. A comparison of the curve of thermogravimetric analysis and differential scanning calorimetry for the treated and untreated samples is presented to demonstrate that the presence of treatment contributes to a better thermal stability for bamboo fibers. PMID:28793585

Point contact tunneling spectroscopy apparatus for large scale mapping of surface superconducting properties

DOE PAGES

Groll, Nickolas; Pellin, Michael J.; Zasadzinksi, John F.; ...

2015-09-18

In this paper, we describe the design and testing of a point contact tunneling spectroscopy device that can measure material surface superconducting properties (i.e., the superconducting gap Δ and the critical temperature T C) and density of states over large surface areas with size up to mm 2. The tip lateral (X,Y) motion, mounted on a (X,Y,Z) piezo-stage, was calibrated on a patterned substrate consisting of Nb lines sputtered on a gold film using both normal (Al) and superconducting (PbSn) tips at 1.5 K. The tip vertical (Z) motion control enables some adjustment of the tip-sample junction resistance that canmore » be measured over 7 orders of magnitudes from a quasi-ohmic regime (few hundred Ω) to the tunnel regime (from tens of kΩ up to few GΩ). The low noise electronic and LabVIEW program interface are also presented. Finally, the point contact regime and the large-scale motion capabilities are of particular interest for mapping and testing the superconducting properties of macroscopic scale superconductor-based devices.« less

Hierarchical NiO-SiO2 composite hollow microspheres with enhanced adsorption affinity towards Congo red in water.

PubMed

Lei, Chunsheng; Zhu, Xiaofeng; Zhu, Bicheng; Yu, Jiaguo; Ho, Wingkei

2016-03-15

Hollow microspheres and hierarchical porous nanostructured materials with desired morphologies have gained remarkable attention for their potential applications in environmental technology. In this study, NiO-SiO2 hollow microspheres were prepared by co-precipitation with SiO2 and nickel salt as precursors, followed by dipping in alkaline solution and calcination. The samples were characterized by X-ray diffraction, field-emission scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, nitrogen adsorption, and X-ray photoelectron spectroscopy. The synthesized hollow spheres were composed of a SiO2 shell and hierarchical porous NiO nanosheets on the surface. Adsorption experiments suggested that NiO-SiO2 composite particles were powerful adsorbents for removal of Congo red from water, with a maximum adsorption capacity of 204.1 mg/g. The high specific surface areas, hollow structures, and hierarchical porous surfaces of the hollow composite particles are suitable for various applications, including adsorption of pollutants, chemical separation, and water purification. Copyright © 2015 Elsevier Inc. All rights reserved.

Effects of surface preparation on quality of aluminum alloy weldments

NASA Technical Reports Server (NTRS)

Kizer, D.; Saperstein, Z.

1968-01-01

Study of surface preparations and surface contamination effects on the welding of 2014 aluminum involves several methods of surface analysis to identify surface properties conducive to weld defects. These methods are radioactive evaporation, spectral reflectance mass spectroscopy, gas chromatography and spark emission spectroscopy.

Facile fabrication of Ag3VO4/attapulgite composites for highly efficient visible light-driven photodegradation towards organic dyes and tetracycline hydrochloride

NASA Astrophysics Data System (ADS)

Luo, Yuting; Luo, Jie; Duan, Guorong; Liu, Xiaoheng

2017-12-01

An efficient one-dimensional attapulgite (ATP)-based photocatalyst, Ag3VO4/ATP nanocomposite, was fabricated by a facile deposition precipitation method with well-dispersed Ag3VO4 nanoparticles anchored on the surface of natural ATP fibers. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), and UV-visible diffused reflectance spectroscopy (UV-vis DRS) were employed to investigate the morphologies, structure, and optical property of the prepared photocatalysts. The photocatalytic experiments indicated that the Ag3VO4/ATP nanocomposites exhibited enhanced visible light-driven photocatalytic activity towards the degradation of rhodamine B (RhB), methyl orange (MO), and tetracycline hydrochloride (TCH), of which the 20 wt% Ag3VO4/ATP sample showed superb photocatalytic performance. As demonstrated by N2 adsorption-desorption, photocurrent measurements, electrochemical impedance spectroscopy (EIS), and photoluminescence (PL) spectra analyses, the improved photocatalytic activity arose from the enlarged surface area, the facilitated charge transfer, and the suppressed recombination of photogenerated charge carriers in Ag3VO4/ATP system. Furthermore, radical scavengers trapping experiments and recycling tests were also conducted. This work gives a new insight into fabrication of highly efficient, stable, and cost-effective visible light-driven photocatalyst for practical application in wastewater treatment and environmental remediation.

Ionic liquid-assisted sonochemical preparation of CeO 2 nanoparticles for CO oxidation

DOE PAGES

Alammar, Tarek; Noei, Heshmat; Wang, Yuemin; ...

2014-10-10

CeO 2 nanoparticles were synthesized via a one-step ultrasound synthesis in different kinds of ionic liquids based on bis(trifluoromethanesulfonylamide, [Tf 2N] –, in combination with various cations including 1-butyl-3-methylimidazolium ([C 4mim] +), 1-ethyl-2,3-dimethylimidazolium ([Edimim] +), butyl-pyridinium([Py 4] +), 1-butyl-1-methyl-pyrrolidinium ([Pyrr 14] +), and 2-hydroxyethyl-trimethylammonium ([N 1112OH] +). Depending on synthetic parameters, such as ionic liquid, Ce(IV) precursor, heating method, and precipitator, formed ceria exhibits different morphologies, varying from nanospheres, nanorods, nanoribbons, and nanoflowers. The morphology, crystallinity, and chemical composition of the obtained materials were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), energy dispersive X-raymore » spectroscopy (EDX), Raman spectroscopy, and N2 adsorption. The structural and electronic properties of the as-prepared CeO 2 samples were probed by CO adsorption using IR spectroscopy under ultrahigh vacuum conditions. The catalytic activities of CeO 2 nanoparticles were investigated in the oxidation of CO. CeO 2 nanospheres obtained sonochemically in [C 4mim][Tf 2N] exhibit the best performance for low-temperature CO oxidation. As a result, the superior catalytic performance of this material can be related to its mesoporous structure, small particle size, large surface area, and high number of surface oxygen vacancy sites.« less

Scalable and reusable micro-bubble removal method to flatten large-area 2D materials

NASA Astrophysics Data System (ADS)

Pham, Phi H. Q.; Quach, Nhi V.; Li, Jinfeng; Burke, Peter J.

2018-04-01

Bubbles generated during electro-delamination and chemical etch during large-area two-dimensional (2D) material transfer has been shown to cause rippling, and consequently, results in tears and wrinkles in the transferred film. Here, we demonstrate a scalable and reusable method to remove surface adhered micro-bubbles by using hydrophobic surfaces modified by self-assembled monolayers (SAMs). Bubble removal allows the 2D film to flatten out and prevents the formation of defects. Electrical characterization was used to verify improved transfer quality and was confirmed by increased field-effect mobility and decreased sheet resistance. Raman spectroscopy was also used to validate enhanced electrical quality following transfer. The bubble removal method can be applied to an assortment of 2D materials using diverse hydrophobic SAM variants. Our studies can be integrated into large scale applications and will lead to improved large-area 2D electronics in general.

Indirect photopatterning of functionalized organic monolayers via copper-catalyzed "click chemistry"

NASA Astrophysics Data System (ADS)

Williams, Mackenzie G.; Teplyakov, Andrew V.

2018-07-01

Solution-based lithographic surface modification of an organic monolayer on a solid substrate is attained based on selective area photo-reduction of copper (II) to copper (I) to catalyze the azide-alkyne dipolar cycloaddition "click" reaction. X-ray photoelectron spectroscopy is used to confirm patterning, and spectroscopic results are analyzed and supplemented with computational models to confirm the surface chemistry. It is determined that this surface modification approach requires irradiation of the solid substrate with all necessary components present in solution. This method requires only minutes of irradiation to result in spatial and temporal control of the covalent surface functionalization of a monolayer and offers the potential for wavelength tunability that may be desirable in many applications utilizing organic monolayers.

Molecular beam epitaxy of graphene on ultra-smooth nickel: growth mode and substrate interactions

NASA Astrophysics Data System (ADS)

Wofford, J. M.; Oliveira, M. H., Jr.; Schumann, T.; Jenichen, B.; Ramsteiner, M.; Jahn, U.; Fölsch, S.; Lopes, J. M. J.; Riechert, H.

2014-09-01

Graphene is grown by molecular beam epitaxy using epitaxial Ni films on MgO(111) as substrates. Raman spectroscopy and scanning tunneling microscopy reveal the graphene films to have few crystalline defects. While the layers are ultra-smooth over large areas, we find that Ni surface features lead to local non-uniformly thick graphene inclusions. The influence of the Ni surface structure on the position and morphology of these inclusions strongly suggests that multilayer graphene on Ni forms at the interface of the first complete layer and metal substrate in a growth-from-below mechanism. The interplay between Ni surface features and graphene growth behavior may facilitate the production of films with spatially resolved multilayer inclusions through engineered substrate surface morphology.

Simultaneous determination of CRP and D-dimer in human blood plasma samples with White Light Reflectance Spectroscopy.

PubMed

Koukouvinos, Georgios; Petrou, Panagiota; Misiakos, Konstantinos; Drygiannakis, Dimitris; Raptis, Ioannis; Stefanitsis, Gerasimos; Martini, Spyridoula; Nikita, Dimitra; Goustouridis, Dimitrios; Moser, Isabella; Jobst, Gerhard; Kakabakos, Sotirios

2016-10-15

A dual-analyte assay for the simultaneous determination of C-reactive protein (CRP) and D-dimer in human blood plasma based on a white light interference spectroscopy sensing platform is presented. Measurement is accomplished in real-time by scanning the sensing surface, on which distinct antibody areas have been created, with a reflection probe used both for illumination of the surface and collection of the reflected interference spectrum. The composition of the transducer, the sensing surface chemical activation and biofunctionalization procedures were optimized with respect to signal magnitude and repeatability. The assay format involved direct detection of CRP whereas for D-dimer a two-site immunoassay employing a biotinylated reporter antibody and reaction with streptavidin was selected. The assays were sensitive with detection limits of 25ng/mL for both analytes, precise with intra- and inter-assay CV values ranging from 3.6% to 7.7%, and from 4.8% to 9.5%, respectively, for both assays, and accurate with recovery values ranging from 88.5% to 108% for both analytes. Moreover, the values determined for the two analytes in 35 human plasma samples were in excellent agreement with those received for the same samples by standard diagnostic laboratory instrumentation employing commercial kits. The excellent agreement of the results supported the validity of the proposed system for clinical application for the detection of multiple analytes since it was demonstrated that up to seven antibody areas can be created on the sensing surface and successfully interrogated with the developed optical set-up. Copyright © 2015. Published by Elsevier B.V.

Tailoring surface and photocatalytic properties of ZnO and nitrogen-doped ZnO nanostructures using microwave-assisted facile hydrothermal synthesis

NASA Astrophysics Data System (ADS)

Rangel, R.; Cedeño, V.; Ramos-Corona, A.; Gutiérrez, R.; Alvarado-Gil, J. J.; Ares, O.; Bartolo-Pérez, P.; Quintana, P.

2017-08-01

Microwave hydrothermal synthesis, using an experimental 23 factorial design, was used to produce tunable ZnO nano- and microstructures, and their potential as photocatalysts was explored. Photocatalytic reactions were conducted in a microreactor batch system under UV and visible light irradiation, while monitoring methylene blue degradation, as a model system. The variables considered in the microwave reactor to produce ZnO nano- or microstructures, were time, NaOH concentration and synthesis temperature. It was found that, specific surface area and volume/surface area ratio were affected as a consequence of the synthesis conditions. In the second stage, the samples were plasma treated in a nitrogen atmosphere, with the purpose of introducing nitrogen into the ZnO crystalline structure. The central idea is to induce changes in the material structure as well as in its optical absorption, to make the plasma-treated material useful as photocatalyst in the visible region of the electromagnetic spectrum. Pristine ZnO and nitrogen-doped ZnO compounds were characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), specific surface area (BET), XPS, and UV-Vis diffuse reflectance spectroscopy. The results show that the methodology presented in this work is effective in tailoring the specific surface area of the ZnO compounds and incorporation of nitrogen into their structure, factors which in turn, affect its photocatalytic behavior.

Spectroscopic Methodologies for Characterizing the Adsorption Behavior and Distribution of Silver Nanoparticles to Hydrated Mineral Surfaces

NASA Astrophysics Data System (ADS)

Brittle, S. W.; O'Neil, K. A.; Foose, D. P.; Stahler, A. C.; Johnson, J. K.; Higgins, S. R.; Sizemore, I. E.; Sikon, J.

2016-12-01

The expansive incorporation of silver nanoparticles (AgNPs) into over 400 consumer products has raised considerable concern about their eventual release into the environment. Although minerals make up a large component of soils, there has been limited research on their interactions with AgNPs. In this study, a representative nonsilicate mineral, corundum (α-Al2O3), was used in fused beaded form (specific surface area of 6-8 m2 g-1) as a model to study the interaction between minerals and negatively-charged, Creighton AgNPs. A concentration of 1 mg L-1 of AgNPs was selected in order to ensure sub-monolayer surface coverage and to surpass the maximum contaminant level (MCL) set by the U.S. Environmental Agency (EPA) for Ag+ in drinking water (0.1 mg L-1). Raman maps collected on the corundum particles exposed to AgNPs at environmentally relevant pH values (6-11) demonstrated AgNP adsorption onto the hydrated mineral surface through OH- moieties regardless of surface charge (i.e. no pH dependence). In addition, two other well-established analytical techniques were employed for supportive purposes. Namely, the AgNP-corundum interaction was also confirmed by inductively coupled plasma optical emission spectroscopy (ICP-OES) through the quantification of the total amount of AgNPs adsorbed onto α-Al2O3. It was found that approximately 75% of the available AgNPs had adsorbed to the mineral surface at all pH values. Atomic force microscopy (AFM), in intermittent contact mode, was also performed to map AgNPs surface distribution on polished and annealed flatter corundum windows. To further demonstrate the Raman analysis, the corundum were also imaged to observe AgNPs adsorption with less surface area and onto other minerals through the occurrence of molecular Ag- vibrations and/or the enhancement of a tracer compound dispensed on mineral surfaces with adsorbed AgNPs (i.e., Surface Enhanced Raman Spectroscopy hot-spots). Overall, this spectroscopic-based analysis promotes extrapolation to other studies as an effective way to observe the interactions between mineral surfaces and nanomaterials.

Complex interaction of subsequent surface streamers via deposited charge: a high-resolution experimental study

NASA Astrophysics Data System (ADS)

Hoder, T.; Synek, P.; Chorvát, D.; Ráhel', J.; Brandenburg, R.; Černák, M.

2017-07-01

The coplanar barrier discharge in synthetic air at 30 kPa pressure was studied by time-correlated single photon counting enhanced optical emission spectroscopy, far-field microscopy enhanced intensified CCD camera and sensitive current measurements. The discharge operated in a regime where two subsequent microdischarges appeared within the same voltage half-period. The electrical analysis of the barrier discharge setup enabled us to quantify charge transfer and the effective electric field development. During the second microdischarge the positive surface streamers follow the interface (triple-line) between the area of deposited charge from the previous one and the area of uncharged dielectric surface. It is shown that additional branching and flashes of surface streamers are responsible for the increased spatial complexity of the deposited surface charges at high overvoltage. A suppressed streamer propagating over the area of deposited surface charge was tracked and the evidence of surface streamer reconnection is presented. A spatiotemporal distribution (resolution of 120 ps and 100 μm) of the reduced electric field strength was obtained for both microdischarges from the recorded luminosities of the molecular nitrogen. The reduced electric field of positive streamers in the first microdischarge reached 1200 Td. For the second one, the electric field values for the streamer at the triple-line are slightly lower than that, while for the suppressed streamers are even higher.

Synthetic coprecipitates of exopolysaccharides and ferrihydrite. Part I: Characterization

NASA Astrophysics Data System (ADS)

Mikutta, Christian; Mikutta, Robert; Bonneville, Steeve; Wagner, Friedrich; Voegelin, Andreas; Christl, Iso; Kretzschmar, Ruben

2008-02-01

Iron(III) (hydr)oxides formed at extracellular biosurfaces or in the presence of exopolymeric substances of microbes and plants may significantly differ in their structural and physical properties from their inorganic counterparts. We synthesized ferrihydrite (Fh) in solutions containing acid polysaccharides [polygalacturonic acid (PGA), alginate, xanthan] and compared its properties with that of an abiotic reference by means of X-ray diffraction, transmission electron microscopy, gas adsorption (N 2, CO 2), X-ray absorption spectroscopy, 57Fe Mössbauer spectroscopy, and electrophoretic mobility measurements. The coprecipitates formed contained up to 37 wt% polymer. Two-line Fh was the dominant mineral phase in all precipitates. The efficacy of polymers to precipitate Fh at neutral pH was higher for polymers with more carboxyl C (PGA ˜ alginate > xanthan). Pure Fh had a specific surface area of 300 m 2/g; coprecipitation of Fh with polymers reduced the detectable mineral surface area by up to 87%. Likewise, mineral micro- (<2 nm) and mesoporosity (2-10 nm) decreased by up to 85% with respect to pure Fh, indicative of a strong aggregation of Fh particles by polymers in freeze-dried state. C-1s STXM images showed the embedding of Fh particles in polymer matrices on the micrometer scale. Iron EXAFS spectroscopy revealed no significant changes in the local coordination of Fe(III) between pure Fh and Fh contained in PGA coprecipitates. 57Fe Mössbauer spectra of coprecipitates confirmed Fh as dominant mineral phase with a slightly reduced particle size and crystallinity of coprecipitate-Fh compared to pure Fh and/or a limited magnetic super-exchange between Fh particles in the coprecipitates due to magnetic dilution by the polysaccharides. The pH iep of pure Fh in 0.01 M NaClO 4 was 7.1. In contrast, coprecipitates of PGA and alginate had a pH iep < 2. Considering the differences in specific surface area, porosity, and net charge between the coprecipitates and pure Fh, composites of exopolysaccharides and Fe(III) (hydr)oxides are expected to differ in their geochemical reactivity from pure Fe(III) (hydr)oxides, even if the minerals have a similar crystallinity.

Biofilm formation on nanostructured titanium oxide surfaces and a micro/nanofabrication-based preventive strategy using colloidal lithography.

PubMed

Singh, Ajay Vikram; Vyas, Varun; Salve, Tushar S; Cortelli, Daniele; Dellasega, David; Podestà, Alessandro; Milani, Paolo; Gade, W N

2012-06-01

The contamination of implant devices as a result of biofilm formation through bacterial infection has instigated major research in this area, particularly to understand the mechanism of bacterial cell/implant surface interactions and their preventions. In this paper, we demonstrate a controlled method of nanostructured titanium oxide surface synthesis using supersonic cluster beam depositions. The nanoscale surface characterization using atomic force microscopy and a profilometer display a regulated evolution in nanomorphology and physical properties. X-ray photoelectron spectroscopy analyses display a stoichiometric nanostructured TiO(2) film. Measurement of the water contact angle shows a nominal increase in the hydrophilic nature of ns-TiO(2) films, whereas the surface energy increases with decreasing contact angle. Bacterial species Staphylococcus aureus and Escherichia coli interaction with nanostructured surfaces shows an increase in adhesion and biofilm formation with increasing nanoscale morphological properties. Conversely, limiting ns-TiO(2) film distribution to micro/nanopatterned designed substrates integrated with bovine serum albumin functionalization leads to a reduction in biofilm formations due to a globally decreased bacterial cell-surface interaction area. The results have potential implications in inhibiting bacterial colonization and promoting mammalian cell-implant interactions.

Preparation of activated carbon from cherry stones by chemical activation with ZnCl 2

NASA Astrophysics Data System (ADS)

Olivares-Marín, M.; Fernández-González, C.; Macías-García, A.; Gómez-Serrano, V.

2006-06-01

Cherry stones (CS), an industrial product generated abundantly in the Valle del Jerte (Cáceres province, Spain), were used as precursor in the preparation of activated carbon by chemical activation with ZnCl 2. The influence of process variables such as the carbonisation temperature and the ZnCl 2:CS ratio (impregnation ratio) on textural and chemical-surface properties of the products obtained was studied. Such products were characterised texturally by adsorption of N 2 at -196 °C, mercury porosimetry and density measurements. Information on the surface functional groups and structures of the carbons was provided by FT-IR spectroscopy. Activated carbon with a high development of surface area and porosity is prepared. When using the 4:1 impregnation ratio, the specific surface area (BET) of the resultant carbon is as high as 1971 m 2 g -1. The effect of the increase in the impregnation ratio on the porous structure of activated carbon is stronger than that of the rise in the carbonisation temperature, whereas the opposite applies to the effect on the surface functional groups and structures.

AFM AND XPS Characterization of Zinc-Aluminum Alloy Coatings with Attention to Surface Dross and Flow Lines

NASA Astrophysics Data System (ADS)

Harding, Felipe A.; Alarcon, Nelson A.; Toledo, Pedro G.

Surfaces of various zinc-aluminum alloy (Zn-Al) coated steel samples are studied with attention to foreign surface dross by atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS/ESCA). AFM topographic maps of zinc-aluminum alloy surfaces free of dross reveal the perfect nanoscale details of two kinds of dendrites: branched and globular. In all magnifications the dendrites appear smooth and, in general, very clean. XPS analysis of the extreme surface of a Zn-Al sample reveals Al, Zn, Si and O as the main components. The XPS results show no segregation or separation of phases other than those indicated by the ternary Al-Zn-Si diagram. For surfaces of Zn-Al plagued with impurities, high resolution AFM topographic maps reveal three situations: (1) areas with well-defined dendrites, relatively free of dross; (2) areas with small, millimeter-sized black spots known as dross; and (3) areas with large black stains, known as flow lines. Dendrite deformation and dross accumulation increase notably in the neighborhood, apparently clean to the naked eye, of dross or flow lines. XPS results of areas with dross and flow lines indicate unacceptable high concentration of Si and important Si phase separation. These results, in the light of AFM work, reveal that dross and flow lines are a consequence of a high local concentration of Si from high melting point silica and silicate impurities in the Zn-Al alloy source.

High surface area mesoporous activated carbon-alginate beads for efficient removal of methylene blue.

PubMed

Nasrullah, Asma; Bhat, A H; Naeem, Abdul; Isa, Mohamed Hasnain; Danish, Mohammed

2018-02-01

High surface area mesoporous activated carbon-alginate (AC-alginate) beads were successfully synthesized by entrapping activated carbon powder derived from Mangosteen fruit peel into calcium-alginate beads for methylene blue (MB) removal from aqueous solution. The structure and surface characteristics of AC-alginate beads were analyzed using Fourier transform infra-red (FTIR) spectroscopy, scanning electron microscopy (SEM) and surface area analysis (S BET ), while thermal properties were tested using thermogravimetric analysis (TGA). The effect of AC-alginate dose, pH of solution, contact time, initial concentration of MB solution and temperature on MB removal was elucidated. The results showed that the maximum adsorption capacity of 230mg/g was achieved for 100mg/L of MB solution at pH 9.5 and temperature 25°C. Furthermore, the adsorption of MB on AC-alginate beads followed well pseudo-second order equation and equilibrium adsorption data were better fitted by the Freundlich isotherm model. The findings reveal the feasibility of AC-alginate beads composite to be used as a potential and low cost adsorbent for removal of cationic dyes. Copyright © 2017 Elsevier B.V. All rights reserved.

Sulfur-carbon nanocomposite cathodes improved by an amphiphilic block copolymer for high-rate lithium-sulfur batteries.

PubMed

Fu, Yongzhu; Su, Yu-Sheng; Manthiram, Arumugam

2012-11-01

A sulfur-carbon nanocomposite consisting of a commercial high-surface-area carbon (i.e., Black Pearls 2000, BET surface area >1000 m² g⁻¹) and sulfur has been synthesized by an in situ deposition method. The nanocomposite is in the form of agglomerated nanoparticles, with the micropores within the carbon filled with sulfur and the mesopores on the carbon surface almost completely covered by sulfur. The BET surface area of the nanocomposite containing a sulfur content of 63.5 wt % is significantly reduced to only 40 m² g⁻¹. Cathodes containing the nanocomposite and Pluronic F-127 block copolymer, which partially replaces the polyvinylidene fluoride binder, were prepared and evaluated in lithium cells by cyclic voltammetry and galvanostatic cycling. The nanocomposite cathodes with the copolymer show improved electrochemical stability and cyclability. The Pluronic copolymer helps retain a uniform nanocomposite structure within the electrodes, improving the electrochemical contact, which was manifested by scanning electron microscopy and electrochemical impedance spectroscopy. The sulfur-Black Pearls nanocomposite with the Pluronic copolymer as an additive in the electrodes is promising for high-rate rechargeable lithium-sulfur batteries.

Effective adsorption and collection of cesium from aqueous solution using graphene oxide grown on porous alumina

NASA Astrophysics Data System (ADS)

Entani, Shiro; Honda, Mitsunori; Shimoyama, Iwao; Li, Songtian; Naramoto, Hiroshi; Yaita, Tsuyoshi; Sakai, Seiji

2018-04-01

Graphene oxide (GO) with a large surface area was synthesized by the direct growth of GO on porous alumina using chemical vapor deposition to study the Cs adsorption mechanism in aqueous solutions. Electronic structure analysis employing in situ near-edge X-ray absorption fine structure spectroscopy and X-ray photoelectron spectroscopy measurements clarifies the Cs atoms bond via oxygen functional groups on GO in the aqueous solution. The Cs adsorption capacity was found to be as high as 650-850 mg g-1, which indicates that the GO/porous alumina acts as an effective adsorbent with high adsorption efficiency for radioactive nuclides in aqueous solutions.

Porous glasses as a matrix for incorporation of photonic materials. Pore determination by positron annihilation lifetime spectroscopy

NASA Astrophysics Data System (ADS)

Reisfeld, Pore determination by positron annihilation lifetime spectroscopy R.; Saraidarov, T.; Jasinska, B.

2004-07-01

Porous glasses prepared by the sol-gel technique have a variety of applications when incorporated by photonic materials: tunable lasers, sensors, luminescence solar concentrators, semiconductor quantum dots, biological markers. The known methods of pore size determinations, the nitrogen adsorption and mercury porosimetry allow to determine the sizes of open pores. Positron annihilation lifetime spectroscopy (PALS) allows to determine pore sizes also of closed pores. As an example we have performed measurements of non-doped zirconia-silica-polyurethane (ZSUR) ormocer glasses and the same glasses doped with lead sulfide quantum dots. The pore radii range between 0.25-0.38 nm, total surface area 15.5-23.8 m 2/g.

Detecting salt deposition on a wind turbine blade using laser induced breakdown spectroscopy technique

NASA Astrophysics Data System (ADS)

Sathiesh Kumar, V.; Vasa, Nilesh J.; Sarathi, R.

2013-07-01

The study of pollution performance on a wind turbine blade due to lightning is important, as it can cause major damage to wind turbine blades. In the present work, optical emission spectroscopy (OES) technique is used to understand the influence of pollutant deposited on a wind turbine blade in an off-shore environment. A methodical experimental study was carried out by adopting IEC 60507 standards, and it was observed that the lightning discharge propagates at the interface between the pollutant and the glass fiber reinforced plastic (Material used in manufacturing of wind turbine blades). In addition, as a diagnostic condition monitoring technique, laser-induced breakdown spectroscopy (LIBS) is proposed and demonstrated to rank the severity of pollutant on the wind turbine blades from a remote area. Optical emission spectra observed during surface discharge process induced by lightning impulse voltage is in agreement with the spectra observed during LIBS.

Improved Optical and Morphological Properties of Vinyl-Substituted Hybrid Silica Materials Incorporating a Zn-Metalloporphyrin.

PubMed

Dudás, Zoltán; Fagadar-Cosma, Eugenia; Len, Adél; Románszki, Loránd; Almásy, László; Vlad-Oros, Beatrice; Dascălu, Daniela; Krajnc, Andraž; Kriechbaum, Manfred; Kuncser, Andrei

2018-04-06

This work is focused on a novel class of hybrid materials exhibiting enhanced optical properties and high surface areas that combine the morphology offered by the vinyl substituted silica host, and the excellent absorption and emission properties of 5,10,15,20-tetrakis( N -methyl-4-pyridyl)porphyrin-Zn(II) tetrachloride as a water soluble guest molecule. In order to optimize the synthesis procedure and the performance of the immobilized porphyrin, silica precursor mixtures of different compositions were used. To achieve the requirements regarding the hydrophobicity and the porous structure of the gels for the successful incorporation of porphyrin, the content of vinyltriacetoxysilane was systematically changed and thoroughly investigated. Substitution of the silica gels with organic groups is a viable way to provide new properties to the support. An exhaustive characterization of the synthesized silica samples was realised by complementary physicochemical methods, such as infrared spectroscopy (FT-IR), absorption spectroscopy (UV-Vis) and photoluminescence, nuclear magnetic resonance spectroscopy ( 29 Si-MAS-NMR) transmission and scanning electron microscopy (TEM and SEM), nitrogen absorption (BET), contact angle (CA), small angle X ray and neutron scattering (SAXS and SANS). All hybrids showed an increase in emission intensity in the wide region from 575 to 725 nm (Q bands) in comparison with bare porphyrin. By simply tuning the vinyltriacetoxysilane content, the hydrophilic/hydrophobic profile of the hybrid materials was changed, while maintaining a high surface area. Good control of hydrophobicity is important to enhance properties such as dispersion, stability behaviour, and resistance to water, in order to achieve highly dispersible systems in water for biomedical applications.

The role of CO 2 as a soft oxidant for dehydrogenation of ethylbenzene to styrene over a high-surface-area ceria catalyst

DOE PAGES

Zhang, Li; Wu, Zili; Nelson, Nicholas; ...

2015-09-22

Catalytic performance and the nature of surface adsorbates were investigated for high-surface-area ceria during ethylbenzene oxidative dehydrogenation (ODH) reaction using CO2 as a soft oxidant. A template assisted method was used to synthesize the high-surface-area ceria. The interactions between ethylbenzene, styrene and CO2 on the surface of ceria and the role of CO2 for the ethylbenzene ODH reaction have been investigated in detail by using activity test, in situ Diffuse Reflectance Infrared and Raman spectroscopy. Not only did CO2 as an oxidant favor the higher yield of styrene, but it also inhibited the deposition of coke during the ethylbenzene ODHmore » reaction. Ethylbenzene ODH reaction over ceria followed a two-step pathway: Ethylbenzene is first dehydrogenated to styrene with H2 formed simultaneously, and then CO2 reacts with H2 via the reverse water gas shift. The styrene produced can easily polymerize to form polystyrene, a key intermediate for coke formation. In the absence of CO2, the polystyrene transforms into graphite-like coke at temperatures above 500 °C, which leads to catalyst deactivation. While in the presence of CO2, the coke deposition can be effectively removed via oxidation with CO2.« less

Sorption of agrochemical model compounds by sorbent materials containing beta-cyclodextrin.

PubMed

Wilson, Lee D; Mohamed, Mohamed H; Guo, Rui; Pratt, Dawn Y; Kwon, Jae Hyuck; Mahmud, Sarker T

2010-04-01

Polymeric sorbent materials that incorporate beta-cyclodextrin (CD) have been prepared and their sorption behavior toward two model agrochemical contaminant compounds, p-nitrophenol (PNP) and methyl chloride examined. The sorption of PNP was studied in aqueous solution using ultraviolet-visible (UV-Vis) spectroscopy, whereas the sorption of methyl chloride from the gas phase was studied using a Langmuir adsorption method. The sorption results for PNP in solution were compared between granular activated carbon (GAC), modified GAC, CD copolymers, and CD-based mesoporous silica hybrid materials. Nitrogen porosimetry at 77 K was used to estimate the surface area and pore structure properties of the sorbent materials. The sorbents displayed variable surface areas as follows: copolymers (36.2-157 m(2)/g), CD-silica materials (307-906 m(2)/g), surface modified GAC (657 m(2)/g), and granular activated carbon (approximately 10(3) m(2)/g). The sorption capacities for PNP and methyl chloride with the different sorbents are listed in descending order as follows: GAC > copolymers > surface modified GAC > CD-silica hybrid materials. In general, the differences in the sorption properties of the sorbents were related to the following: (i) surface area of the sorbent, (ii) CD content and accessibility, (iii) and the chemical nature of the sorbent material.

Effects of Thickness and Amount of Carbon Nanofiber Coated Carbon Fiber on Improving the Mechanical Properties of Nanocomposites

PubMed Central

Ghaemi, Ferial; Ahmadian, Ali; Yunus, Robiah; Ismail, Fudziah; Rahmanian, Saeed

2016-01-01

In the current study, carbon nanofibers (CNFs) were grown on a carbon fiber (CF) surface by using the chemical vapor deposition method (CVD) and the influences of some parameters of the CVD method on improving the mechanical properties of a polypropylene (PP) composite were investigated. To obtain an optimum surface area, thickness, and yield of the CNFs, the parameters of the chemical vapor deposition (CVD) method, such as catalyst concentration, reaction temperature, reaction time, and hydrocarbon flow rate, were optimized. It was observed that the optimal surface area, thickness, and yield of the CNFs caused more adhesion of the fibers with the PP matrix, which enhanced the composite properties. Besides this, the effectiveness of reinforcement of fillers was fitted with a mathematical model obtaining good agreement between the experimental result and the theoretical prediction. By applying scanning electronic microscope (SEM), transmission electron microscope (TEM), and Raman spectroscopy, the surface morphology and structural information of the resultant CF-CNF were analyzed. Additionally, SEM images and a mechanical test of the composite with a proper layer of CNFs on the CF revealed not only a compactness effect but also the thickness and surface area roles of the CNF layers in improving the mechanical properties of the composites. PMID:28344263

Tailoring magnetic nanoparticle for transformers application.

PubMed

Morais, P C; Silva, A S; Leite, E S; Garg, V K; Oliveira, A C; Viali, W R; Sartoratto, P P C

2010-02-01

In this study photoacoustic spectroscopy was used to investigate the effect of dilution of an oil-based magnetic fluid sample on the magnetic nanoparticle surface-coating. Changes of the photoacoustic signal intensity on the band-L region (640 to 830 nm) upon dilution of the stock magnetic fluid sample were discussed in terms of molecular surface desorption. The model proposed here assumes that the driving force taking the molecules out from the nanoparticle surface into the bulk solvent is the gradient of osmotic pressure. This gradient of osmotic pressure is established between the nanoparticle surface and the bulk suspension. It is further assumed that the photoacoustic signal intensity (area under the photoacoustic spectra) scales linearly with the number of coating molecules (surface grafting) at the nanoparticle surface. This model picture provides a non-linear analytical description for the reduction of the surface grafting coefficient upon dilution, which was successfully-used to curve-fit the photoacoustic experimental data.

Ion scattering and electron spectroscopy of the chemical species at a HF-prepared Si(211) surface

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

Jaime-Vasquez, M.; Martinka, M.; Groenert, M.

2006-01-16

The species and the nature of their chemical bonds at the surface of a hydrogen-terminated Si(211) wafer were characterized using temperature desorption spectroscopy, ion scattering spectroscopy, and electron spectroscopy. The surface region is dominated by monohydride species with dihydrides present in small amounts. Fluorine is distributed across the top layer as largely a physisorbed species to the Si substrate. Low-energy {sup 3}He{sup +} ions remove the H and F species with only minimal damage to the underlying region.

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

Lucia, M., E-mail: mlucia@pppl.gov; Kaita, R.; Majeski, R.

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.

Synthesis of D-mannose capped silicon nanoparticles and their interactions with MCF-7 human breast cancerous cells.

PubMed

Ahire, Jayshree H; Chambrier, Isabelle; Mueller, Anja; Bao, Yongping; Chao, Yimin

2013-08-14

Silicon nanoparticles (SiNPs) hold prominent interest in various aspects of biomedical applications. For this purpose, surface functionalization of the NPs is essential to stabilize them, target them to specific disease area, and allow them to selectively bind to the cells or the bio-molecules present on the surface of the cells. However, no such functionalization has been explored with Si nanoparticles. Carbohydrates play a critical role in cell recognition. Here, we report the first synthesis of silicon nanoparticles functionalized with carbohydrates. In this study, stable and brightly luminescent d-Mannose (Man) capped SiNPs have been synthesized from amine terminated SiNPs and d-mannopyranoside acid. The surface functionalization is confirmed by Fourier transform infrared spectroscopy (FTIR), nuclear magnetic resonance spectroscopy (NMR), and energy dispersive X-ray spectroscopy (EDX) studies. The mean diameter of the crystal core is 5.5 nm, as measured by transmission electron microscopy (TEM), while the hydrodynamic diameter obtained by dynamic light scattering (DLS) is 16 nm. The quantum yield (QY) of photoluminescence emission is found to be 11.5%, and the nanoparticles exhibit an exceptional stability over two weeks. The Man-capped SiNPs may prove to be valuable tools for further investigating glycobiological, biomedical, and material science fields. Experiments are carried out using Concanavalin A (ConA) as a target protein in order to prove the hypothesis. When Man functionalized SiNPs are treated with ConA, cross-linked aggregates are formed, as shown in TEM images as well as monitored by photoluminescence spectroscopy (PL). Man functionalized SiNPs can target cancerous cells. Visualization imaging of SiNPs in MCF-7 human breast cancer cells shows the fluorescence is distributed throughout the cytoplasm of these cells.

Dealloying, Microstructure and the Corrosion/Protection of Cast Magnesium Alloys

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

Sieradzki, Karl; Aiello, Ashlee; McCue, Ian

The purpose of this project was to develop a greater understanding of micro-galvanic corrosion effects in cast magnesium alloys using both experimental and computational methods. Experimental accomplishments have been made in the following areas of interest: characterization, aqueous free-corrosion, atmospheric corrosion, ionic liquid dissolution, rate kinetics of oxide dissolution, and coating investigation. Commercial alloys (AZ91D, AM60, and AZ31B), binary-phase alloys (αMg-2at.%Al, αMg-5at.%Al, and Mg-8at.%Al), and component phases (Mg, Al, β-Mg, β-1%Zn, MnAl3) were obtained and characterized using energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), and scanning electron microscopy (SEM). Full immersion in aqueous chloride was used to characterize the corrosionmore » behavior of alloys. Rotating disc electrodes (RDEs) were used to observe accelerated long-term corrosion behavior. Al surface redistribution for freely corroded samples was analyzed using SEM, EDS, and lithium underpotential deposition (Li UPD). Atmospheric corrosion was observed using contact angle evolution, overnight pH monitoring, and surface pH evolution studies. Ionic liquid corrosion characterization was performed using linear sweep voltammetry and potentiostatic dissolution in 150° choline chloride-urea (cc-urea). Two surface coatings were investigated: (1) Li-carbonate and (2) cc-urea. Li-carbonate coatings were characterized using X-ray photoelectron spectroscopy (XPS), SEM, and aqueous free corrosion potential monitoring. Hydrophobic cc-urea coatings were characterized using contact angle measurements and electrochemical impedance spectroscopy. Oxide dissolution rate kinetics were studied using inductively coupled plasma mass spectroscopy (ICP-MS). Computational accomplishments have been made through the development of Kinetic Monte Carlo (KMC) simulations which model time- and composition-dependent effects on the microstructure due to spatial redistribution of alloying elements during corrosion.« less

Evidence of alloy formation during reduction of platinized tin oxide surfaces

NASA Technical Reports Server (NTRS)

Gardner, Steven D.; Hoflund, Gar B.; Davidson, Mark R.; Schryer, David R.

1989-01-01

Ion scattering spectroscopy, Auger electron spectroscopy, and electron spectroscopy for chemical analysis have been used to examine a platinized tin oxide catalyst surface before, during, and after reduction by annealing under vacuum at 250 to 450 C. These techniques were then used to examine the reduced surface after a room-temperature, low-pressure oxygen exposure. The spectral results and the behavior of the reduced surface toward oxygen exposure both indicate that a Pt/Sn alloy is produced during reduction.

Analysis of surface scale on the Ni-based superalloy CMSX-10N and proposed mechanism of formation

NASA Astrophysics Data System (ADS)

Simmonds, S.; D'Souza, N.; Ryder, K. S.; Dong, H.

2012-01-01

There is a continuing demand to raise the operating temperature of jet engine turbine blades to meet the need for higher turbine entry temperatures (TET) in order to increase thermal efficiency and thrust. Modern, high-pressure turbine blades are made from Ni-based superalloys in single-crystal form via the investment casting process. One important post-cast surface defect, known as 'surface scale', has been investigated on the alloy CMSX-10N. This is an area of distinct discolouration of the aerofoil seen after casting. Auger electron and X-ray photoelectron spectroscopy analysis were carried out on both scaled and un-scaled areas. In the scaled region, a thin layer (~800nm) of Ni oxide is evident. In the un-scaled regions there is a thicker Al2O3 layer. It is shown that, as the blade cools during casting, differential thermal contraction of mould and alloy causes the solid blade to 'detach' from the mould in these scaled areas. The formation of Ni Oxides is facilitated by this separation.

Periodic silver nanocluster arrays over large-area silica nanosphere template as highly sensitive SERS substrate

NASA Astrophysics Data System (ADS)

Hou, Xu; Wang, Qi; Mao, Guoming; Liu, Hao; Yu, Rongdi; Ren, Xiaomin

2018-04-01

Periodic Ag nanocluster arrays for surface enhanced Raman spectroscopy (SERS) were fabricated through magnetron sputtering Ag over a large-area monolayer template which is based on silica (SiO2) nanospheres. High-density nanogaps between the adjacent Ag nanoclusters acted as "hot-spots", making a dominant contribution to the high-performance SERS detection. Moreover, the nanospheres and Ag nanoclusters effectively increased the surface roughness and also enlarged the surface area of as-obtained SERS substrate, which resulted in a further enhancement in Raman signals. As-prepared SERS substrates showed very high sensitivity with the enhancement factor (EF) value of 4.1 × 1012 for Rhodamine 6G (R6G), allowing the corresponding detection limit as low as 10-16 M. Additionally, SERS signal of melamine was still strong even though its concentration was lowered to 10-7 M. Our results show that preparing highly sensitive SERS substrate with periodic Ag nanoclusters over SiO2 nanosphere template is a convenient and promising pathway for chemical and biologic sensing.

Stabilization and Amorphization of Lovastatin Using Different Types of Silica.

PubMed

Khanfar, Mai; Al-Nimry, Suhair

2017-08-01

Lovastatin (LOV), an antihyperlipidimic agent, is characterized by low solubility/poor dissolution and, thus, low bioavailability (<5%). A beneficial effect on its bioavailability could result from improving its dissolution. One of the most common methods used to enhance dissolution is the preparation of solid dispersions. Solid dispersions of LOV and silica with different surface areas were prepared. The effects of the type of silica, ratio of drug/silica, incubation period with silica, and the effect of surface area were all studied. Characterization of the prepared formulae for possible interaction between drug and polymer was carried out using differential scanning calorimetery, Fourier transform infrared spectroscopy, powder X-ray diffraction, surface area determination, and scanning electron microscopy. The dissolution profiles of all prepared formulae were constructed and evaluated. It was found that the formula made of LOV and Sylysia 350 FCP in a ratio of 1:5 after an incubation period of 48 h resulted in the best release, and it was stable after 3 months storage at 75% RH and 40°C.

High-surface-area nitrogen-doped reduced graphene oxide for electric double-layer capacitors

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

Youn, Hee-Chang; Bak, Seong-Min; Kim, Myeong-Seong

A two-step method consisting of solid-state microwave irradiation and heat treatment under NH₃ gas was used to prepare nitrogen-doped reduced graphene oxide (N-RGO) with a high specific surface area (1007m²g⁻¹), high electrical conductivity (1532S m⁻¹), and low oxygen content (1.5 wt%) for electric double-layer capacitor applications. The specific capacitance of N-RGO was 291 Fg⁻¹ at a current density of 1 A g⁻¹, and a capacitance of 261 F g⁻¹ was retained at 50 A g⁻¹, indicating a very good rate capability. N-RGO also showed excellent cycling stability, preserving 96% of the initial specific capacitance after 100,000 cycles. Near-edge X-ray absorptionmore » fine-structure spectroscopy evidenced the recover of π-conjugation in the carbon networks with the removal of oxygenated groups and revealed the chemical bonding of the nitrogen atoms in N-RGO. The good electrochemical performance of N-RGO is attributed to its high surface area, high electrical conductivity, and low oxygen content.« less

High-surface-area nitrogen-doped reduced graphene oxide for electric double-layer capacitors

DOE PAGES

Youn, Hee-Chang; Bak, Seong-Min; Kim, Myeong-Seong; ...

2015-06-08

A two-step method consisting of solid-state microwave irradiation and heat treatment under NH₃ gas was used to prepare nitrogen-doped reduced graphene oxide (N-RGO) with a high specific surface area (1007m²g⁻¹), high electrical conductivity (1532S m⁻¹), and low oxygen content (1.5 wt%) for electric double-layer capacitor applications. The specific capacitance of N-RGO was 291 Fg⁻¹ at a current density of 1 A g⁻¹, and a capacitance of 261 F g⁻¹ was retained at 50 A g⁻¹, indicating a very good rate capability. N-RGO also showed excellent cycling stability, preserving 96% of the initial specific capacitance after 100,000 cycles. Near-edge X-ray absorptionmore » fine-structure spectroscopy evidenced the recover of π-conjugation in the carbon networks with the removal of oxygenated groups and revealed the chemical bonding of the nitrogen atoms in N-RGO. The good electrochemical performance of N-RGO is attributed to its high surface area, high electrical conductivity, and low oxygen content.« less

Mapping potentialy asbestos-bearing rocks using imaging spectroscopy

USGS Publications Warehouse

Swayze, G.A.; Kokaly, R.F.; Higgins, C.T.; Clinkenbeard, J.P.; Clark, R.N.; Lowers, H.A.; Sutley, S.J.

2009-01-01

Rock and soil that may contain naturally occurring asbestos (NOA), a known human carcinogen, were mapped in the Sierra Nevada, California, using the Airborne Visible/Infrared Imaging Spectrometer (AVIRIS) to determine if these materials could be uniquely identified with spectroscopy. Such information can be used to prepare or refine maps of areas that may contain minerals that can be asbestiform, such as serpentine and tremolite-actinolite, which were the focus of this study. Although thick vegetation can conceal underlying rock and soil, use of linear-mixture spectra calculated from spectra of dry grass and serpentine allowed detection of serpentine in some parts of the study area with up to ~80% dry-grass cover. Chaparral vegetation, which was dominantly, but not exclusively, found in areas underlain by serpentinized ultramafic rocks, was also mapped. Overall, field checking at 201 sites indicated highly accurate identification by AVIRIS of mineral (94%) and vegetation (89%) categories. Practical applications of AVIRIS to mapping areas that may contain NOA include locating roads that are surfaced with serpentine aggregate, identifying sites that may require enhanced dust control or other safety measures, and filling gaps in geologic mapping where field access is limited.

Surface Acidity and Properties of TiO2/SiO2 Catalysts Prepared by Atomic Layer Deposition: UV-visible Diffuse Reflectance, DRIFTS, and Visible Raman Spectroscopy Studies

DTIC Science & Technology

2009-06-15

titanium isopropoxide (TTIP) as metal precursors. The deposition rate of titania films from TiCl4 was found to be stable in the 150-300 °C...tetrachloride (TiCl4) and titanium isopropoxide (TTIP) are widely used as metal precursors and water or hydrogen peroxide are used as oxygen precursors.29-36... titanium dioxide supported on high surface area silica gel have been synthesized by atomic layer deposition (ALD) using titanium tetrachloride (TiCl4) and

Proceedings 5th International Conference on Optics of Surfaces and Interfaces (OSI-V), Léon, México 26-30 May 2003: physica status solidi (c) - conferences and critical reviews

NASA Astrophysics Data System (ADS)

Mendoza, Bernardo S.

2003-05-01

physica status solidi (c) conferences and critical reviews publishes conference proceedings, ranging from large international meetings to specialized topical workshops as well as collections of topical reviews on various areas of current solid state physics research. The objective of "Optics of Surfaces and Interfaces" (OSI-V) is to bridge the gap between basic and applied science. Apart from recent advances in theoretical modeling and experimental research, special attention is given to novel techniques of optical spectroscopy at interfaces.

Simple sol-gel process to obtain silica-coated anatase particles with enhanced TiO2-SiO2 interfacial area.

PubMed

Resende, S F; Nunes, E H M; Houmard, M; Vasconcelos, W L

2014-11-01

In this study we prepared silica-titania composites with a low SiO2:TiO2 molar ratio. These materials were prepared using a simple sol-gel route in which a hydrothermal treatment was used to obtain mesoporous anatase particles. Pure titania was also synthetized for comparison purposes. These materials were examined by scanning and transmission electron microscopy (SEM and TEM, respectively), energy dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), and nitrogen sorption tests. A thin silica coating was formed on the anatase particles. It was observed that the presence of this coating led to samples with an enhanced thermal stability. Indeed, the composites prepared in this work showed an anatase structure and a high specific surface area (SSA), even after their calcination at 800°C. Thus, we believe that the synthetized material present an outstanding SiO2-TiO2 interfacial area associated with a high amount of anatase particles which could improve its photoactive properties. Copyright © 2014 Elsevier Inc. All rights reserved.

Excellent capacitive performance of a three-dimensional hierarchical porous graphene/carbon composite with a superhigh surface area.

PubMed

Li, Xue Jin; Xing, Wei; Zhou, Jin; Wang, Gui Qiang; Zhuo, Shu Ping; Yan, Zi Feng; Xue, Qing Zhong; Qiao, Shi Zhang

2014-10-06

Three-dimensional hierarchical porous graphene/carbon composite was successfully synthesized from a solution of graphene oxide and a phenolic resin by using a facile and efficient method. The morphology, structure, and surface property of the composite were investigated intensively by a variety of means such as scanning electron microscopy (SEM), transmission electron microscopy (TEM), N2 adsorption, Raman spectroscopy, and Fourier transform infrared spectroscopy (FTIR). It is found that graphene serves as a scaffold to form a hierarchical pore texture in the composite, resulting in its superhigh surface area of 2034 m(2) g(-1), thin macropore wall, and high conductivity (152 S m(-1)). As evidenced by electrochemical measurements in both EMImBF4 ionic liquid and KOH electrolyte, the composite exhibits ideal capacitive behavior, high capacitance, and excellent rate performance due to its unique structure. In EMImBF4 , the composite has a high energy density of up to 50.1 Wh kg(-1) and also possesses quite stable cycling stability at 100 °C, suggesting its promising application in high-temperature supercapacitors. In KOH electrolyte, the specific capacitance of this composite can reach up to an unprecedented value of 186.5 F g(-1), even at a very high current density of 50 A g(-1), suggesting its prosperous application in high-power applications. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Mesoporous anatase TiO{sub 2}/reduced graphene oxide nanocomposites: A simple template-free synthesis and their high photocatalytic performance

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

Zhou, Qi; Zhong, Yong-Hui; Laboratory of Nanomaterials and Environmental Detection, Hefei Institute of Physical Sciences, Chinese Academy of Sciences, Hefei 230031

2014-03-01

Graphical abstract: - Highlights: • Mesoporous TiO{sub 2} nanoparticles with anatase phase were assembled on reduced graphene oxide via a template-free one-step hydrothermal method. • The TiO{sub 2}/rGO nanocomposites have better adsorption capacity and photocatalytic degradation efficiency for dyes removal. • Improved dye adsorption and photogenerated charge separation are responsible for enhanced activity. - Abstract: Mesoporous anatase phase TiO{sub 2} was assembled on reduced graphene oxide (rGO) using a template-free one-step hydrothermal process. The nanocomposites were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and Brunauer–Emmett–Teller (BET) surface area.more » Morphology of TiO{sub 2} was related to the content of graphene oxide. TiO{sub 2}/rGO nanocomposites exhibited excellent photocatalytic activity for the photo-degradation of methyl orange. The degradation rate was 4.5 times greater than that of pure TiO{sub 2} nanoparticles. This difference was attributed to the thin two-dimensional graphene sheet. The graphene sheet had a large surface area, high adsorption capacity, and acted as a good electron acceptor for the transfer of photo-generated electrons from the conduction band of TiO{sub 2}. The enhanced surface adsorption characteristics and excellent charge transport separation were independent properties of the photocatalytic degradation process.« less

Mechanisms and efficiency of the simultaneous removal of metals and cyanides by using ferrate(VI): crucial roles of nanocrystalline iron(III) oxyhydroxides and metal carbonates.

PubMed

Filip, Jan; Yngard, Ria A; Siskova, Karolina; Marusak, Zdenek; Ettler, Vojtech; Sajdl, Petr; Sharma, Virender K; Zboril, Radek

2011-08-29

The reaction of potassium ferrate(VI), K(2)FeO(4), with weak-acid dissociable cyanides--namely, K(2)[Zn(CN)(4)], K(2)[Cd(CN)(4)], K(2)[Ni(CN)(4)], and K(3)[Cu(CN)(4)]--results in the formation of iron(III) oxyhydroxide nanoparticles that differ in size, crystal structure, and surface area. During cyanide oxidation and the simultaneous reduction of iron(VI), zinc(II), copper(II), and cadmium(II), metallic ions are almost completely removed from solution due to their coprecipitation with the iron(III) oxyhydroxides including 2-line ferrihydrite, 7-line ferrihydrite, and/or goethite. Based on the results of XRD, Mössbauer and IR spectroscopies, as well as TEM, X-ray photoelectron emission spectroscopy, and Brunauer-Emmett-Teller measurements, we suggest three scavenging mechanisms for the removal of metals including their incorporation into the ferrihydrite crystal structure, the formation of a separate phase, and their adsorption onto the precipitate surface. Zn and Cu are preferentially and almost completely incorporated into the crystal structure of the iron(III) oxyhydroxides; the formation of the Cd-bearing, X-ray amorphous phase, together with Cd carbonate is the principal mechanism of Cd removal. Interestingly, Ni remains predominantly in solution due to the key role of nickel(II) carbonate, which exhibits a solubility product constant several orders of magnitude higher than the carbonates of the other metals. Traces of Ni, identified in the iron(III) precipitate, are exclusively adsorbed onto the large surface area of nanoparticles. We discuss the relationship between the crystal structure of iron(III) oxyhydroxides and the mechanism of metal removal, as well as the linear relationship observed between the rate constant and the surface area of precipitates. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Electron spectroscopy of the diamond surface

NASA Technical Reports Server (NTRS)

Pepper, S. V.

1981-01-01

The diamond surface is studied by ionization loss spectroscopy and Auger electron spectroscopy. For surfaces heated to temperatures not exceeding 900 C, the band gap was found to be devoid of empty states in the absence of electron beam effects. The incident electron beam generates empty states in the band gap and loss of structure in the valence band for these surfaces. A cross section of 1.4 x 10 to the -19th sq cm was obtained for this effect. For surfaces heated to temperatures exceeding 900 C the spectra were identical to those from surfaces modified by the electron beam. The diamond surface undergoes a thermal conversion in its electronic structure at about 900 C.

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

PubMed

Wang, Congzhou; Yadavalli, Vamsi K

2014-05-01

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

Fluorescence-correlation spectroscopy study of molecular transport within reversed-phase chromatographic particles compared to planar model surfaces.

PubMed

Cooper, Justin; Harris, Joel M

2014-12-02

Reversed-phase liquid chromatography (RPLC) is a widely used technique for molecular separations. Stationary-phase materials for RPLC generally consist of porous silica-gel particles functionalized with n-alkane ligands. Understanding motions of molecules within the interior of these particles is important for developing efficient chromatographic materials and separations. To characterize these dynamics, time-resolved spectroscopic methods (photobleach recovery, fluorescence correlation, single-molecule imaging) have been adapted to measure molecular diffusion rates, typically at n-alkane-modified planar silica surfaces, which serve as models of chromatographic interfaces. A question arising from these studies is how dynamics of molecules on a planar surface relate to motions of molecules within the interior of a porous chromatographic particle. In this paper, imaging-fluorescence-correlation spectroscopy is used to measure diffusion rates of a fluorescent probe molecule 1,1'-dioctadecyl-3,3,3'3'-tetramethylindocarbocyanine perchlorate (DiI) within authentic RPLC porous silica particles and compared with its diffusion at a planar C18-modified surface. The results show that surface diffusion on the planar C18 substrate is much faster than the diffusion rate of the probe molecule through a chromatographic particle. Surface diffusion within porous particles, however, is governed by molecular trajectories along the tortuous contours of the interior surface of the particles. By accounting for the greater surface area that a molecule must explore to diffuse macroscopic distances through the particle, the molecular-scale diffusion rates on the two surfaces can be compared, and they are virtually identical. These results provide support for the relevance of surface-diffusion measurements made on planar model surfaces to the dynamic behavior of molecules on the internal surfaces of porous chromatographic particles.

Nanostructure-based plasmon-enhanced Raman spectroscopy for surface analysis of materials

NASA Astrophysics Data System (ADS)

Ding, Song-Yuan; Yi, Jun; Li, Jian-Feng; Ren, Bin; Wu, De-Yin; Panneerselvam, Rajapandiyan; Tian, Zhong-Qun

2016-06-01

Since 2000, there has been an explosion of activity in the field of plasmon-enhanced Raman spectroscopy (PERS), including surface-enhanced Raman spectroscopy (SERS), tip-enhanced Raman spectroscopy (TERS) and shell-isolated nanoparticle-enhanced Raman spectroscopy (SHINERS). In this Review, we explore the mechanism of PERS and discuss PERS hotspots — nanoscale regions with a strongly enhanced local electromagnetic field — that allow trace-molecule detection, biomolecule analysis and surface characterization of various materials. In particular, we discuss a new generation of hotspots that are generated from hybrid structures combining PERS-active nanostructures and probe materials, which feature a strong local electromagnetic field on the surface of the probe material. Enhancement of surface Raman signals up to five orders of magnitude can be obtained from materials that are weakly SERS active or SERS inactive. We provide a detailed overview of future research directions in the field of PERS, focusing on new PERS-active nanomaterials and nanostructures and the broad application prospect for materials science and technology.

Two-dimensional correlation spectroscopy — Biannual survey 2007-2009

NASA Astrophysics Data System (ADS)

Noda, Isao

2010-06-01

The publication activities in the field of 2D correlation spectroscopy are surveyed with the emphasis on papers published during the last two years. Pertinent review articles and conference proceedings are discussed first, followed by the examination of noteworthy developments in the theory and applications of 2D correlation spectroscopy. Specific topics of interest include Pareto scaling, analysis of randomly sampled spectra, 2D analysis of data obtained under multiple perturbations, evolution of 2D spectra along additional variables, comparison and quantitative analysis of multiple 2D spectra, orthogonal sample design to eliminate interfering cross peaks, quadrature orthogonal signal correction and other data transformation techniques, data pretreatment methods, moving window analysis, extension of kernel and global phase angle analysis, covariance and correlation coefficient mapping, variant forms of sample-sample correlation, and different display methods. Various static and dynamic perturbation methods used in 2D correlation spectroscopy, e.g., temperature, composition, chemical reactions, H/D exchange, physical phenomena like sorption, diffusion and phase transitions, optical and biological processes, are reviewed. Analytical probes used in 2D correlation spectroscopy include IR, Raman, NIR, NMR, X-ray, mass spectrometry, chromatography, and others. Application areas of 2D correlation spectroscopy are diverse, encompassing synthetic and natural polymers, liquid crystals, proteins and peptides, biomaterials, pharmaceuticals, food and agricultural products, solutions, colloids, surfaces, and the like.

Surface enhanced Raman spectroscopy: A review of recent applications in forensic science

NASA Astrophysics Data System (ADS)

Fikiet, Marisia A.; Khandasammy, Shelby R.; Mistek, Ewelina; Ahmed, Yasmine; Halámková, Lenka; Bueno, Justin; Lednev, Igor K.

2018-05-01

Surface enhanced Raman spectroscopy has many advantages over its parent technique of Raman spectroscopy. Some of these advantages such as increased sensitivity and selectivity and therefore the possibility of small sample sizes and detection of small concentrations are invaluable in the field of forensics. A variety of new SERS surfaces and novel approaches are presented here on a wide range of forensically relevant topics.

Reflectance spectroscopy of palagonite and iron-rich montmorillonite clay mixtures: Implications for the surface composition of Mars

NASA Technical Reports Server (NTRS)

Orenberg, J. B.; Handy, J.

1991-01-01

Because of the power of remote sensing reflectance spectroscopy in determining mineralogy, it was used as the major method of identifying possible mineral analogs of the Martian surface. A summary of proposed Martian surface compositions from reflectance spectroscopy before 1979 was presented. Since that time, iron-rich montmorillonite clay, nanocrystalline or nanophase hematite, and palagonite were suggested as Mars soil analog materials.

Impedance spectroscopy of reduced monoclinic zirconia.

PubMed

Eder, Dominik; Kramer, Reinhard

2006-10-14

Zirconia doped with low-valent cations (e.g. Y3+ or Ca2+) exhibits an exceptionally high ionic conductivity, making them ideal candidates for various electrochemical applications including solid oxide fuel cells (SOFC) and oxygen sensors. It is nevertheless important to study the undoped, monoclinic ZrO2 as a model system to construct a comprehensive picture of the electrical behaviour. In pure zirconia a residual number of anion vacancies remains because of contaminants in the material as well as the thermodynamic disorder equilibrium, but electronic conduction may also contribute to the observed conductivity. Reduction of zirconia in hydrogen leads to the adsorption of hydrogen and to the formation of oxygen vacancies, with their concentration affected by various parameters (e.g. reduction temperature and time, surface area, and water vapour pressure). However, there is still little known about the reactivities of defect species and their effect on the ionic and electronic conduction. Thus, we applied electrochemical impedance spectroscopy to investigate the electric performance of pure monoclinic zirconia with different surface areas in both oxidizing and reducing atmospheres. A novel equivalent circuit model including parallel ionic and electronic conduction has previously been developed for titania and is used herein to decouple the conduction processes. The concentration of defects and their formation energies were measured using volumetric oxygen titration and temperature programmed oxidation/desorption.

Double-shell Fe2O3 hollow box-like structure for enhanced photo-Fenton degradation of malachite green dye

NASA Astrophysics Data System (ADS)

Jiang, De Bin; Liu, Xiaoying; Xu, Xuan; Zhang, Yu Xin

2018-01-01

In this work we demonstrate the synthesis of novel Fe2O3 nanosheets with double-shell hollow morphology by replica molding from diatomite framework. The nanostructures of Fe2O3 nanosheets were examined by focused-ion-beam scanning electron microscopy (FIB/SEM), X-ray diffraction spectroscopy (XRD), Brunauer-Emmett-Teller (BET) specific surface area measurements and Fourier transform infrared (FT-IR) spectroscopy. The results reveal that (1) Pure Fe2O3 nanosheets were successfully obtained; (2) The double-shell Fe2O3 hollow structure achieved via the NaOH etching silica method was observed; (3) Fe2O3 nanosheets possessed uniformly distributed porous nanosheets. Such structural features enlarged the specific surface area of Fe2O3 nanosheets and led to more catalytic active sites. In the heterogeneous photo-Fenton reaction, the double-shell Fe2O3 hollow morphology exhibited excellent catalytic capability for the degradation of malachite green (MG) at circumneutral pH condition. Under optimum condition, MG solution was almost completely decolorized in 60 min (99.9%). The Fe2O3 nanosheets also showed good stability and recyclability, demonstrating great potential as a promising photo-Fenton catalyst for the effective degradation of MG dye in wastewater.

A controlled release of ibuprofen by systematically tailoring the morphology of mesoporous silica materials

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

Qu Fengyu; Chemistry and Pharmaceutical College, Jiamusi University, Jiamusi 154007; Zhu Guangshan

2006-07-15

A series of mesoporous silica materials with similar pore sizes, different morphologies and variable pore geometries were prepared systematically. In order to control drug release, ibuprofen was employed as a model drug and the influence of morphology and pore geometry of mesoporous silica on drug release profiles was extensively studied. The mesoporous silica and drug-loaded samples were characterized by X-ray diffraction, Fourier transform IR spectroscopy, N{sub 2} adsorption and desorption, scanning electron microscopy, and transmission electron microscopy. It was found that the drug-loading amount was directly correlated to the Brunauer-Emmett-Teller surface area, pore geometry, and pore volume; while the drugmore » release profiles could be controlled by tailoring the morphologies of mesoporous silica carriers. - Graphical abstract: The release of ibuprofen is controlled by tailoring the morphologies of mesoporous silica. The mesoporous silica and drug-loaded samples are characterized by powder X-ray diffraction, Fourier transform IR spectroscopy, N{sub 2} adsorption and desorption, scanning electron microscopy, and transmission electron microscopy. The drug-loading amount is directly correlated to the Brunauer-Emmett-Teller surface area, pore geometry, and pore volume; while the drug release profiles can be controlled by tailoring the morphologies of mesoporous silica carriers.« less

Photocatalytic activity enhancement of anatase-graphene nanocomposite for methylene removal: Degradation and kinetics

NASA Astrophysics Data System (ADS)

Rezaei, Mostafa; Salem, Shiva

2016-10-01

In the present research, the TiO2-graphene nanocomposite was synthesized by an eco-friendly method. The blackberry juice was introduced to graphene oxide (GO) as a reducing agent to produce the graphene nano-sheets. The nanocomposite of anatase-graphene was developed as a photocatalyst for the degradation of methylene blue, owing to the larger specific surface area and synergistic effect of reduced graphene oxide (RGO). The UV spectroscopy measurements showed that the prepared nanocomposite exhibited an excellent photocatalytic activity toward the methylene blue degradation. The rate of electron transfer of redox sheets is much higher than that observed on GO, indicating the applicability of proposed method for the production of anatase-RGO nanocomposite for treatment of water contaminated by cationic dye. The prepared materials were characterized with Fourier transform infrared spectroscopy, X-ray diffraction, Brunauer-Emmett-Teller surface area measurement, scanning electron microscopy and transmission electron microscopy. A facile and rapid route was applied for the uniform deposition of anatase nanoparticles on the sheets. The resulting nanocomposite contained nanoparticles with a mean diameter of 10 nm. A mechanism for the photocatalytic activity of nanocomposite was suggested and the degradation reaction obeyed the second-order kinetics. It was concluded that the degradation kinetics is changed due to the reduction of GO in the presence of blackberry juice.

Microwave-Assisted Synthesis of Perovskite SrSnO 3 Nanocrystals in Ionic Liquids for Photocatalytic Applications

DOE PAGES

Alammar, Tarek; Hamm, Ines; Grasmik, Viktoria; ...

2017-06-05

Nanosized SrSnO 3 photocatalysts have been successfully synthesized by microwave synthesis in various ionic liquids (ILs) followed by a heat treatment process to optimize the materials’ crystallinity. The influence of the ILs with various cations such as 1-butyl-3-methylimidazolium ([C 4mim] +), 6-bis(3-methylimidazolium-1-yl)hexane ([C 6(mim) 2] 2+), butylpyridinium ([C 4Py] +), and tetradecyltrihexylphosphonium ([P 66614] +) and bis(trifluoromethanesulfonyl)amide ([Tf 2N] -) as the anion on the structure, crystallization, and morphology of the products was investigated. The samples were characterized by X-ray diffraction (XRD), thermogravimetry (TG), scanning electron microscopy (SEM), surface area analysis by gas adsorption, X-ray photoelectron spectroscopy (XPS), diffuse reflectancemore » UV–vis spectroscopy, and Raman and IR spectroscopy. According to structure characterization by XRD and Raman spectroscopy all samples crystallized phase-pure in the orthorhombic GdFeO 3 perovskite structure type. SEM reveals that, on the basis of the IL, the obtained SrSnO 3 nanoparticles exhibit different morphologies and sizes. Rod-shaped particles are formed in [C 4mim][Tf 2N], [C 6(mim) 2][Tf 2N] 2, and [P 66614][Tf 2N]. However, the particle dimensions and size distribution vary depending on the IL and range from quite thin and long needlelike particles with a narrow size distribution obtained in [P 66614][Tf 2N] to relatively larger particles with a broader size distribution obtained in [C 6(mim) 2][Tf 2N] 2. In contrast, in [C 4Py][Tf 2N] nanospheres with a diameter of about 50 nm form. For these particles the highest photocatalytic activity was observed. Our investigations indicate that the improved photocatalytic activity of this material results from the synergistic effect of the relatively large surface area associated with nanosize and an appropriate energy band structure.« less

Superstrong encapsulated monolayer graphene by the modified anodic bonding

NASA Astrophysics Data System (ADS)

Jung, Wonsuk; Yoon, Taeshik; Choi, Jongho; Kim, Soohyun; Kim, Yong Hyup; Kim, Taek-Soo; Han, Chang-Soo

2013-12-01

We report a superstrong adhesive of monolayer graphene by modified anodic bonding. In this bonding, graphene plays the role of a superstrong and ultra-thin adhesive between SiO2 and glass substrates. As a result, monolayer graphene presented a strong adhesion energy of 1.4 J m-2 about 310% that of van der Waals bonding (0.45 J m-2) to SiO2 and glass substrates. This flexible solid state graphene adhesive can tremendously decrease the adhesive thickness from about several tens of μm to 0.34 nm for epoxy or glue at the desired bonding area. As plausible causes of this superstrong adhesion, we suggest conformal contact with the rough surface of substrates and generation of C-O chemical bonding between graphene and the substrate due to the bonding process, and characterized these properties using optical microscopy, atomic force microscopy, Raman spectroscopy, and X-ray photoelectron spectroscopy.We report a superstrong adhesive of monolayer graphene by modified anodic bonding. In this bonding, graphene plays the role of a superstrong and ultra-thin adhesive between SiO2 and glass substrates. As a result, monolayer graphene presented a strong adhesion energy of 1.4 J m-2 about 310% that of van der Waals bonding (0.45 J m-2) to SiO2 and glass substrates. This flexible solid state graphene adhesive can tremendously decrease the adhesive thickness from about several tens of μm to 0.34 nm for epoxy or glue at the desired bonding area. As plausible causes of this superstrong adhesion, we suggest conformal contact with the rough surface of substrates and generation of C-O chemical bonding between graphene and the substrate due to the bonding process, and characterized these properties using optical microscopy, atomic force microscopy, Raman spectroscopy, and X-ray photoelectron spectroscopy. Electronic supplementary information (ESI) available. See DOI: 10.1039/c3nr03822j

Ultrasonic spray pyrolysis synthesis of reduced graphene oxide/anatase TiO2 composite and its application in the photocatalytic degradation of methylene blue in water.

PubMed

Park, Jeong-Ann; Yang, Boram; Lee, Joongki; Kim, In Gyeom; Kim, Jae-Hyun; Choi, Jae-Woo; Park, Hee-Deung; Nah, In Wook; Lee, Sang-Hyup

2018-01-01

Reduced graphene oxide (RGO)/anatase TiO 2 composite was prepared using a simple one-step technique-ultrasonic spray pyrolysis-in order to inhibit the aggregation of TiO 2 nanoparticles and to improve the photocatalytic performance for degradation of methylene blue (MB). Different proportions (0-5 wt%) of RGO/TiO 2 composites were characterized by scanning electronic microscopy (SEM), dispersive X-ray spectrometry (EDS), transmission electron microscopy (TEM), Brunauer-Emmett-Teller (BET) surface area, X-ray photoelectron spectroscopy (XPS), X-ray diffractometry (XRD), Raman spectroscopy, UV-vis spectroscopy, and electrochemical impedance spectroscopy (EIS) to verify mechanism. From these analysis, TiO 2 nanoparticles are distributed uniformly on the RGO sheets with crumpled shape during ultrasonic spray pyrolysis and surface area is increasing by increasing portion of RGO. Band gap of RGO 5 /TiO 2 (5 wt% of RGO) composite is 2.72 eV and band gap was reduced by increasing portion of RGO in RGO/TiO 2 composites. The RGO 5 /TiO 2 composite was superior to other lower content of RGO/TiO 2 composites with a rapid transport of charge carriers and an effective charge separation. The highest removal efficiency of MB was obtained at the RGO 5 /TiO 2 composite under UVC irradiation, which coincided with the EIS, and the optimal dose of the composite was determined to be 0.5 g/L. The RGO 5 /TiO 2 composite improve the photocatalytic degradation rate of MB over the TiO 2 due to a retardation of electron-hole recombination. The MB adsorption capacity and photocatalytic degradation efficiency were greatly affected by pH changes and increased with increasing pH due to electrostatic interactions and generation of more hydroxyl radicals. The reusability of RGO 5 /TiO 2 composite was examined during 3 cycles. Copyright © 2017 Elsevier Ltd. All rights reserved.

A non-destructive spectroscopic study of the decoration of archaeological pottery: from matt-painted bichrome ceramic sherds (southern Italy, VIII-VII B.C.) to an intact Etruscan cinerary urn

NASA Astrophysics Data System (ADS)

Bruni, Silvia; Guglielmi, Vittoria; Della Foglia, Elena; Castoldi, Marina; Bagnasco Gianni, Giovanna

2018-02-01

A study is presented based on the use of entirely non-destructive spectroscopic techniques to analyze the chemical composition of the painted surface layer of archaeological pottery. This study aims to define both the raw materials and the working technology of ancient potters. Energy-dispersive X-ray analysis, micro-Raman spectroscopy, visible and near infrared (NIR) diffuse reflection spectroscopy and external reflection Fourier-transform infrared (FTIR) spectroscopy were applied to matt-painted bichrome pottery sherds (VIII-VII century B.C.) from the site of Incoronata near Metaponto in southern Italy. Two different raw materials, ochre and iron-rich clay, were recognized for the red decoration, while the dark areas resulted to have been obtained by the so-called manganese black technique. In any case, it was demonstrated that the decoration was applied before firing, in spite of its sometimes grainy aspect that could suggest a post-firing application. For the samples with a more sophisticated decorative pattern a red/black/white polychromy was recognized, as the lighter areas correspond to an ;intentional white; obtained by the firing of a calcium-rich clay. Reflection spectroscopy in the visible-NIR and mid-IR as well as micro-Raman spectroscopy were then employed to characterize the decoration of an intact ceramic urn from the Etruscan town of Chiusi, evidencing a post-firing painting based on the use of red ochre, carbon black and lime, possibly imitating the ;fresco; technique used in wall paintings.

Self-assembly of a triangle-shaped, hexaplatinum-incorporated, supramolecular amphiphile in solution and at interfaces.

PubMed

Maran, Umamageswaran; Britt, David; Fox, Christopher B; Harris, Joel M; Orendt, Anita M; Conley, Hiram; Davis, Robert; Hlady, Vladamir; Stang, Peter J

2009-08-24

The self-assembly and characterization of a novel supramolecular amphiphile built from a new 60 degree amphiphilic precursor that incorporates hydrophilic platinum(II) metals and hydrophobic dioctadecyloxy chains is reported. The amphiphilic macrocycle and its precursor compound have been characterized by multinuclear NMR spectroscopy, ESI-MS, and other standard techniques. The coacervate morphology of the amphiphile at the liquid-liquid interface has been studied by using confocal optical microscopy and in situ Raman spectroscopy. The self-assembly of the amphiphilic macrocycle at the air-water interface has been investigated through Langmuir-trough techniques. The study indicates the possible formation of surface micelle-like aggregates. The disparity between the experimental molecular areas and those derived from molecular models support the idea of aggregation. AFM images of the surface aggregates show the formation of a flat topology with arbitrary ridgelike patterns. Reasonable molecular-packing arrangements are proposed to explain the molecular organization within the observed structures.

Conformal and highly luminescent monolayers of Alq3 prepared by gas-phase molecular layer deposition.

PubMed

Räupke, André; Albrecht, Fabian; Maibach, Julia; Behrendt, Andreas; Polywka, Andreas; Heiderhoff, Ralf; Helzel, Jonatan; Rabe, Torsten; Johannes, Hans-Hermann; Kowalsky, Wolfgang; Mankel, Eric; Mayer, Thomas; Görrn, Patrick; Riedl, Thomas

2014-01-22

The gas-phase molecular layer deposition (MLD) of conformal and highly luminescent monolayers of tris(8-hydroxyquinolinato)aluminum (Alq3) is reported. The controlled formation of Alq3 monolayers is achieved for the first time by functionalization of the substrate with amino groups, which serve as initial docking sites for trimethyl aluminum (TMA) molecules binding datively to the amine. Thereby, upon exposure to 8-hydroxyquinoline (8-HQ), the self-limiting formation of highly luminescent Alq3 monolayers is afforded. The growth process and monolayer formation were studied and verified by in situ quartz crystal monitoring, optical emission and absorption spectroscopy, and X-ray photoelectron spectroscopy. The nature of the MLD process provides an avenue to coat arbitrarily shaped 3D surfaces and porous structures with high surface areas, as demonstrated in this work for silica aerogels. The concept presented here paves the way to highly sensitive luminescent sensors and dye-sensitized metal oxides for future applications (e.g., in photocatalysis and solar cells).

Engineering and characterization of mesoporous silica-coated magnetic particles for mercury removal from industrial effluents

NASA Astrophysics Data System (ADS)

Dong, Jie; Xu, Zhenghe; Wang, Feng

2008-03-01

Mesoporous silica coatings were synthesized on dense liquid silica-coated magnetite particles using cetyl-trimethyl-ammonium chloride (CTAC) as molecular templates, followed by sol-gel process. A specific surface area of the synthesized particles as high as 150 m 2/g was obtained. After functionalization with mercapto-propyl-trimethoxy-silane (MPTS) through silanation reaction, the particles exhibited high affinity of mercury in aqueous solutions. Atomic force microscopy (AFM), zeta potential measurement, thermal gravimetric analysis (TGA), analytical transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and atomic absorption spectroscopy (AAS) were used to characterize the synthesis processes, surface functionalization, and mercury adsorption on the synthesized magnetite particles. The loading capacity of the particles for mercury was determined to be as high as 14 mg/g at pH 2. A unique feature of strong magnetism of the synthesized nanocomposite particles makes the subsequent separation of the magnetic sorbents from complex multiphase suspensions convenient and effective.

Mercury removal in wastewater by iron oxide nanoparticles

NASA Astrophysics Data System (ADS)

Vélez, E.; Campillo, G. E.; Morales, G.; Hincapié, C.; Osorio, J.; Arnache, O.; Uribe, J. I.; Jaramillo, F.

2016-02-01

Mercury is one of the persistent pollutants in wastewater; it is becoming a severe environmental and public health problem, this is why nowadays its removal is an obligation. Iron oxide nanoparticles are receiving much attention due to their properties, such as: great biocompatibility, ease of separation, high relation of surface-area to volume, surface modifiability, reusability, excellent magnetic properties and relative low cost. In this experiment, Fe3O4 and γ-Fe2O3 nanoparticles were synthesized using iron salts and NaOH as precipitation agents, and Aloe Vera as stabilizing agent; then these nanoparticles were characterized by three different measurements: first, using a Zetasizer Nano ZS for their size estimation, secondly UV-visible spectroscopy which showed the existence of resonance of plasmon at λmax∼360 nm, and lastly by Scanning Electron Microscopy (SEM) to determine nanoparticles form. The results of this characterization showed that the obtained Iron oxides nanoparticles have a narrow size distribution (∼100nm). Mercury removal of 70% approximately was confirmed by atomic absorption spectroscopy measurements.

Enhanced photocatalytic activity of Fe-doped TiO2 coated on N-doped activated carbon composites for photocatalytic degradation of dyeing wastewater

NASA Astrophysics Data System (ADS)

Zhou, Jie; Zhu, Beibei; Wang, Lu; Li, Ya; Qiao, Qichen

2017-10-01

Fe-doped TiO2 coated on N-doped activated carbon (Fe-TiO2/N-AC, FTNA) composites were synthesized simply by a straightforward two-step procedure. The obtained materials were characterized by X-ray diffractometry (XRD), N2 adsorption-desorption, scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and FT-IR spectroscopies. Through the degradation of dyeing wastewater, the photocatalytic activity of FTNA was investigated under ultraviolet light irradiation. The results showed that containing N functional groups were successfully introduced onto the surface of the activated carbon. Compared with Fe-TiO2/AC (FTA), FTNA with average particle size of TiO2 13.6 nm and surface area 1007.89 m2/g showed a higher photoactivity. Additionally, for the photocatalytic degradation of dyeing wastewater, the optimum N content and catalyst content were 0.8% and 5g/L, respectively. Moreover, the photoactivity and photo stability of the catalyst after many runs was also evaluated.

Facile green synthesis of fluorescent N-doped carbon dots from Actinidia deliciosa and their catalytic activity and cytotoxicity applications

NASA Astrophysics Data System (ADS)

Arul, Velusamy; Sethuraman, Mathur Gopalakrishnan

2018-04-01

Green synthesis of fluorescent nitrogen doped carbon dots (N-CDs) using Actinidia deliciosa (A. deliciosa) fruit extract as a carbon precursor and aqueous ammonia as a nitrogen dopant is reported here. The synthesized N-CDs were characterized by high resolution transmission electron microscopy (HR-TEM), energy dispersive spectroscopy (EDS), selected area electron diffraction (SAED), UV-Visible spectroscopy (UV-Vis), fluorescence spectroscopy, Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). The average size of the N-CDs was approximately 3.59 nm and the calculated inter layer distance was found to be 0.21 nm. Raman spectroscopy and SAED pattern revealed the graphitic nature of the synthesized N-CDs. The N-CDs were found to emit intense blue color at 405 nm under the excitation of 315 nm. The doping of nitrogen over the surface of the N-CDs was confirmed by EDS, FT-IR and XPS studies. The synthesized N-CDs were found to exhibit excellent catalytic activity in the reduction of Rhodamine-B using sodium borohydrate. The MTT assay was used to evaluate the cytotoxicity and biocompatibility of N-CDs towards L-929 and MCF-7 cells. From the results obtained, it was found that the N-CDs exhibit low cytotoxicity and superior biocompatibility on both L-929 and MCF-7 cells.

Biopolymer protected silver nanoparticles on the support of carbon nanotube as interface for electrocatalytic applications

NASA Astrophysics Data System (ADS)

Satyanarayana, M.; Kumar, V. Sunil; Gobi, K. Vengatajalabathy

2016-04-01

In this research, silver nanoparticles (SNPs) are prepared on the surface of carbon nanotubes via chitosan, a biopolymer linkage. Here chitosan act as stabilizing agent for nanoparticles and forms a network on the surface of carbon nanotubes. Synthesized silver nanoparticles-MWCNT hybrid composite is characterized by UV-Visible spectroscopy, XRD analysis, and FESEM with EDS to evaluate the structural and chemical properties of the nanocomposite. The electrocatalytic activity of the fabricated SNP-MWCNT hybrid modified glassy carbon electrode has been evaluated by cyclic voltammetry and electrochemical impedance analysis. The silver nanoparticles are of size ˜35 nm and are well distributed on the surface of carbon nanotubes with chitosan linkage. The prepared nanocomposite shows efficient electrocatalytic properties with high active surface area and excellent electron transfer behaviour.

STM/STS Study of LixCoO2 Single Crystals

NASA Astrophysics Data System (ADS)

Iwaya, Katsuya; Minato, Taketoshi; Miyoshi, Kiyotaka; Takeuchi, Jun; Kim, Yousoo; Hitosugi, Taro

2012-02-01

We have performed low temperature scanning tunneling microscopy/spectroscopy (STM/STS) measurements on LixCoO2 (x=0.66) single crystal surfaces. A (1x1) hexagonal lattice was clearly observed and found to be moved by changing bias-voltage polarity, indicating that this could be associated with Li ions on the surface. Under the (1x1) hexagonal lattice, we imaged almost randomly distributed bright dots that were strongly dependent on bias-voltage, with insulating spectroscopic features. Different area on the surface showed a (2x2) hexagonal lattice that could be related to an ordering of Co^3+ and Co^4+ ions. These results suggest the electronic structure of LixCoO2 surface is inhomogeneous possibly due to segregation of Li ions.

Effect of Porosity Parameters and Surface Chemistry on Carbon Dioxide Adsorption in Sulfur-Doped Porous Carbons.

PubMed

Wang, En-Jie; Sui, Zhu-Yin; Sun, Ya-Nan; Ma, Zhuang; Han, Bao-Hang

2018-05-22

In this work, a series of highly porous sulfur-doped carbons are prepared through physical activation methods by using polythiophene as a precursor. The morphology, structure, and physicochemical properties are revealed by a variety of characterization methods, such as scanning electron microscopy, Raman spectroscopy, X-ray photoelectron spectroscopy, and nitrogen sorption measurement. Their porosity parameters and chemical compositions can be well-tuned by changing the activating agents (steam and carbon dioxide) and reaction temperature. These sulfur-doped porous carbons possess specific surface area of 670-2210 m 2 g -1 , total pore volume of 0.31-1.26 cm 3 g -1 , and sulfur content of 0.6-4.9 atom %. The effect of porosity parameters and surface chemistry on carbon dioxide adsorption in sulfur-doped porous carbons is studied in detail. After a careful analysis of carbon dioxide uptake at different temperatures (273 and 293 K), pore volumes from small pore size (less than 1 nm) play an important role in carbon dioxide adsorption at 273 K, whereas surface chemistry is the key factor at a higher adsorption temperature or lower relative pressure. Furthermore, sulfur-doped porous carbons also possess good gas adsorption selectivity and excellent recyclability for regeneration.

Sensitive and fast detection of fructose in complex media via symmetry breaking and signal amplification using surface-enhanced Raman spectroscopy.

PubMed

Sun, Fang; Bai, Tao; Zhang, Lei; Ella-Menye, Jean-Rene; Liu, Sijun; Nowinski, Ann K; Jiang, Shaoyi; Yu, Qiuming

2014-03-04

A new strategy is proposed to sensitively and rapidly detect analytes with weak Raman signals in complex media using surface-enhanced Raman spectroscopy (SERS) via detecting the SERS signal changes of the immobilized probe molecules on SERS-active substrates upon binding of the analytes. In this work, 4-mercaptophenylboronic acid (4-MPBA) was selected as the probe molecule which was immobilized on the gold surface of a quasi-three-dimensional plasmonic nanostructure array (Q3D-PNA) SERS substrate to detect fructose. The molecule of 4-MPBA possesses three key functions: molecule recognition and reversible binding of the analyte via the boronic acid group, amplification of SERS signals by the phenyl group and thus shielding of the background noise of complex media, and immobilization on the surface of SERS-active substrates via the thiol group. Most importantly, the symmetry breaking of the 4-MPBA molecule upon fructose binding leads to the change of area ratio between totally symmetric 8a ring mode and nontotally symmetric 8b ring mode, which enables the detection. The detection curves were obtained in phosphate-buffered saline (PBS) and in undiluted artificial urine at clinically relevant concentrations, and the limit of detection of 0.05 mM was achieved.

TiO2/bone composite materials for the separation of heavy metal impurities from waste water solutions

NASA Astrophysics Data System (ADS)

Dakroury, G.; Labib, Sh.; Abou El-Nour, F. H.

2012-09-01

Pure bone material obtained from cow meat, as apatite-rich material, and TiO2-bone composite materials are prepared and studied to be used for heavy metal ions separation from waste water solutions. Meat wastes are chemically and thermally treated to control their microstructure in order to prepare the composite materials that fulfill all the requirements to be used as selective membranes with high performance, stability and mechanical strength. The prepared materials are analyzed using Hg-porosimetry for surface characterization, energy dispersive X-ray spectroscopy (EDAX) for elemental analysis and Fourier transform infrared spectroscopy (FTIR) for chemical composition investigation. Structural studies are performed using X-ray diffraction (XRD). Microstructural properties are studied using scanning electron microscopy (SEM) and specific surface area studies are performed using Brunauer-Emmet-Teller (BET) method. XRD studies show that multiphase structures are obtained as a result of 1h sintering at 700-1200 °C for both pure bone and TiO2-bone composite materials. The factors affecting the transport of different heavy metal ions through the selected membranes are determined from permeation flux measurements. It is found that membrane pore size, membrane surface roughness and membrane surface charge are the key parameters that control the transport or rejection of heavy metal ions through the selected membranes.

[Current views on surface enhanced Raman spectroscopy in microbiology].

PubMed

Jia, Xiaoxiao; Li, Jing; Qin, Tian; Deng, Aihua; Liu, Wenjun

2015-05-01

Raman spectroscopy has generated many branches during the development for more than 90 years. Surface enhanced Raman spectroscopy (SERS) improves SNR by using the interaction between tested materials and the surface of rough metal, as to quickly get higher sensitivity and precision spectroscopy without sample pretreatment. This article describes the characteristic and classification of SERS, and updates the theory and clinical application of SERS. It also summarizes the present status and progress of SERS in various disciplines and illustrates the necessity and urgency of its research, which provides rationale for the application for SERS in microbiology.

Surface characterization and chemical analysis of bamboo substrates pretreated by alkali hydrogen peroxide.

PubMed

Song, Xueping; Jiang, Yan; Rong, Xianjian; Wei, Wei; Wang, Shuangfei; Nie, Shuangxi

2016-09-01

The surface characterization and chemical analysis of bamboo substrates by alkali hydrogen peroxide pretreatment (AHPP) were investigated in this study. The results tended to manifest that AHPP prior to enzymatic and chemical treatment was potential for improving accessibility and reactivity of bamboo substrates. The inorganic components, organic solvent extractives and acid-soluble lignin were effectively removed by AHPP. X-ray photoelectron spectroscopy (XPS) analysis indicated that the surface of bamboo chips had less lignin but more carbohydrate after pre-treatment. Fiber surfaces became etched and collapsed, and more pores and debris on the substrate surface were observed with Scanning Electron Microscopy (SEM). Brenauer-Emmett-Teller (BET) results showed that both of pore volume and surface area were increased after AHPP. Although XRD analysis showed that AHPP led to relatively higher crystallinity, pre-extraction could overall enhance the accessibility of enzymes and chemicals into the bamboo structure. Copyright © 2016. Published by Elsevier Ltd.

Catalytic Activity and Impedance Behavior of Screen-Printed Nickel Oxide as Efficient Water Oxidation Catalysts.

PubMed

Singh, Archana; Fekete, Monika; Gengenbach, Thomas; Simonov, Alexandr N; Hocking, Rosalie K; Chang, Shery L Y; Rothmann, Mathias; Powar, Satvasheel; Fu, Dongchuan; Hu, Zheng; Wu, Qiang; Cheng, Yi-Bing; Bach, Udo; Spiccia, Leone

2015-12-21

We report that films screen printed from nickel oxide (NiO) nanoparticles and microballs are efficient electrocatalysts for water oxidation under near-neutral and alkaline conditions. Investigations of the composition and structure of the screen-printed films by X-ray diffraction, X-ray absorption spectroscopy, and scanning electron microscopy confirmed that the material was present as the cubic NiO phase. Comparison of the catalytic activity of the microball films to that of films fabricated by using NiO nanoparticles, under similar experimental conditions, revealed that the microball films outperform nanoparticle films of similar thickness owing to a more porous structure and higher surface area. A thinner, less-resistive NiO nanoparticle film, however, was found to have higher activity per Ni atom. Anodization in borate buffer significantly improved the activity of all three films. X-ray photoelectron spectroscopy showed that during anodization, a mixed nickel oxyhydroxide phase formed on the surface of all films, which could account for the improved activity. Impedance spectroscopy revealed that surface traps contribute significantly to the resistance of the NiO films. On anodization, the trap state resistance of all films was reduced, which led to significant improvements in activity. In 1.00 m NaOH, both the microball and nanoparticle films exhibit high long-term stability and produce a stable current density of approximately 30 mA cm(-2) at 600 mV overpotential. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Broad-Bandwidth Chiral Sum Frequency Generation Spectroscopy for Probing the Kinetics of Proteins at Interfaces

PubMed Central

2016-01-01

The kinetics of proteins at interfaces plays an important role in biological functions and inspires solutions to fundamental problems in biomedical sciences and engineering. Nonetheless, due to the lack of surface-specific and structural-sensitive biophysical techniques, it still remains challenging to probe protein kinetics in situ and in real time without the use of spectroscopic labels at interfaces. Broad-bandwidth chiral sum frequency generation (SFG) spectroscopy has been recently developed for protein kinetic studies at interfaces by tracking the chiral vibrational signals of proteins. In this article, we review our recent progress in kinetic studies of proteins at interfaces using broad-bandwidth chiral SFG spectroscopy. We illustrate the use of chiral SFG signals of protein side chains in the C–H stretch region to monitor self-assembly processes of proteins at interfaces. We also present the use of chiral SFG signals from the protein backbone in the N–H stretch region to probe the real-time kinetics of proton exchange between protein and water at interfaces. In addition, we demonstrate the applications of spectral features of chiral SFG that are typical of protein secondary structures in both the amide I and the N–H stretch regions for monitoring the kinetics of aggregation of amyloid proteins at membrane surfaces. These studies exhibit the power of broad-bandwidth chiral SFG to study protein kinetics at interfaces and the promise of this technique in research areas of surface science to address fundamental problems in biomedical and material sciences. PMID:26196215

Detection of surface carbon and hydrocarbons in hot spot regions of niobium superconducting rf cavities by Raman spectroscopy

DOE PAGES

Cao, C.; Argonne National Lab.; Ford, D.; ...

2013-06-26

Raman microscopy/spectroscopy measurements are presented on high purity niobium (Nb) samples, including pieces from hot spot regions of a tested superconducting rf cavity that exhibit a high density of etch pits. Measured spectra are compared with density functional theory calculations of Raman-active, vibrational modes of possible surface Nb-O and Nb-H complexes. The Raman spectra inside particularly rough pits in all Nb samples show clear differences from surrounding areas, exhibiting enhanced intensity and sharp peaks. While some of the sharp peaks are consistent with calculated NbH and NbH 2 modes, there is better overall agreement with C-H modes in chain-type hydrocarbons.more » Other spectra reveal two broader peaks attributed to amorphous carbon. Niobium foils annealed to >2000°C in high vacuum develop identical Raman peaks when subjected to cold working. Regions with enhanced C and O have also been found by SEM/EDX spectroscopy in the hot spot samples and cold-worked foils, corroborating the Raman results. Such regions with high concentrations of impurities are expected to suppress the local superconductivity and this may explain the correlation between hot spots in superconducting rf (SRF) cavities and the observation of a high density of surface pits. Finally, the origin of localized high carbon and hydrocarbon regions is unclear at present but it is suggested that particular processing steps in SRF cavity fabrication may be responsible.« less

Detection of surface carbon and hydrocarbons in hot spot regions of niobium superconducting rf cavities by Raman spectroscopy

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

Cao, C.; Argonne National Lab.; Ford, D.

Raman microscopy/spectroscopy measurements are presented on high purity niobium (Nb) samples, including pieces from hot spot regions of a tested superconducting rf cavity that exhibit a high density of etch pits. Measured spectra are compared with density functional theory calculations of Raman-active, vibrational modes of possible surface Nb-O and Nb-H complexes. The Raman spectra inside particularly rough pits in all Nb samples show clear differences from surrounding areas, exhibiting enhanced intensity and sharp peaks. While some of the sharp peaks are consistent with calculated NbH and NbH 2 modes, there is better overall agreement with C-H modes in chain-type hydrocarbons.more » Other spectra reveal two broader peaks attributed to amorphous carbon. Niobium foils annealed to >2000°C in high vacuum develop identical Raman peaks when subjected to cold working. Regions with enhanced C and O have also been found by SEM/EDX spectroscopy in the hot spot samples and cold-worked foils, corroborating the Raman results. Such regions with high concentrations of impurities are expected to suppress the local superconductivity and this may explain the correlation between hot spots in superconducting rf (SRF) cavities and the observation of a high density of surface pits. Finally, the origin of localized high carbon and hydrocarbon regions is unclear at present but it is suggested that particular processing steps in SRF cavity fabrication may be responsible.« less

In situ FTIR spectroscopic assessment of methylbutynol catalytic conversion products in relation to the surface acid-base properties of systematically modified aluminas

NASA Astrophysics Data System (ADS)

Mekhemer, Gamal A. H.; Zaki, Mohamed I.

2016-10-01

The present investigation was designed to assess the credibility of methylbutynol (MBOH) as an infrared (IR) reactive probe molecule for surface acid-base properties of metal oxides. Accordingly, pure alumina was systematically modified with varied amounts (0.5-10 wt.%) of K+ or SO42 - additives. Then, the influence of nature and amount of the additive on the following alumina properties were examined: (i) bulk composition and structure by X-ray powder diffractometry and ex-situ IR spectroscopy, (ii) surface area and net charge by N2 sorptiometry and pH-metry, respectively, and (iii) nature and strength of exposed surface acid sites by in-situ IR spectroscopy of adsorbed pyridine at ambient and higher temperatures. Results obtained were correlated with IR-identified product distribution of MBOH catalytic decomposition/conversion at 200 °C. It is thereby concluded that MBOH is superior to conventional IR inactive probe molecules in gauging sensitively the prevailing acid or base character, availability of base sites, relative population of Bronsted to Lewis acid sites, and strength and reactivity of the sites exposed on metal oxide surfaces. Hence, all that is needed to get this information is to handle IR spectra taken from the gas phase, a task that is experimentally much more accessible than taking spectra from adsorbed species of irreactive probe molecules.

Periodic nanostructural materials for nanoplasmonics

NASA Astrophysics Data System (ADS)

Choi, Dukhyun

2017-02-01

Nanoscale periodic material design and fabrication are essentially fundamental requirement for basic scientific researches and industrial applications of nanoscience and engineering. Innovative, effective, reproducible, large-area uniform, tunable and robust nanostructure/material syntheses are still challenging. Here, I would like to introduce the novel periodic nanostructural materials particularly with uniformly ordered nanoporous or nanoflower structures, which are fabricated by simple, cost-effective, and high-throughput wet chemical methods. I also report large-area periodic plasmonic nanostructures based on template-based nanolithography. The surface morphology and optical properties are characterized by SEM and UV-vis. spectroscopy. Furthermore, their enhancement factor is evaluated by using SERS signals.

Characterization study of polycrystalline tin oxide surfaces before and after reduction in CO

NASA Technical Reports Server (NTRS)

Drawdy, Jean E.; Hoflund, Gar B.; Davidson, Mark R.; Schryer, David R.

1990-01-01

Polycrystalline tin oxide surfaces have been examined before and after reduction in 40 Torr of CO at 100 and 175 C using Auger electron spectroscopy (AES), electron spectroscopy for chemical analysis (ESCA), ion scattering spectroscopy (ISS) and electron stimulated desorption (ESD). The changes in the surface composition and chemical states of the surface species generally are subtle for the reductive conditions used. However, significant changes do occur with regard to the amounts and the chemical forms of the hydrogen-containing species remaining after both the 100 and 175 C reductions.

Development and Optical Testing of the Camera, Hand Lens, and Microscope Probe with Scannable Laser Spectroscopy (CHAMP-SLS)

NASA Technical Reports Server (NTRS)

Mungas, Greg S.; Gursel, Yekta; Sepulveda, Cesar A.; Anderson, Mark; La Baw, Clayton; Johnson, Kenneth R.; Deans, Matthew; Beegle, Luther; Boynton, John

2008-01-01

Conducting high resolution field microscopy with coupled laser spectroscopy that can be used to selectively analyze the surface chemistry of individual pixels in a scene is an enabling capability for next generation robotic and manned spaceflight missions, civil, and military applications. In the laboratory, we use a range of imaging and surface preparation tools that provide us with in-focus images, context imaging for identifying features that we want to investigate at high magnification, and surface-optical coupling that allows us to apply optical spectroscopic analysis techniques for analyzing surface chemistry particularly at high magnifications. The camera, hand lens, and microscope probe with scannable laser spectroscopy (CHAMP-SLS) is an imaging/spectroscopy instrument capable of imaging continuously from infinity down to high resolution microscopy (resolution of approx. 1 micron/pixel in a final camera format), the closer CHAMP-SLS is placed to a feature, the higher the resultant magnification. At hand lens to microscopic magnifications, the imaged scene can be selectively interrogated with point spectroscopic techniques such as Raman spectroscopy, microscopic Laser Induced Breakdown Spectroscopy (micro-LIBS), laser ablation mass-spectrometry, Fluorescence spectroscopy, and/or Reflectance spectroscopy. This paper summarizes the optical design, development, and testing of the CHAMP-SLS optics.

Bimodal porous TiO2 structures templated by graft copolymer/homopolymer blend for dye-sensitized solar cells with polymer electrolyte

NASA Astrophysics Data System (ADS)

Kim, Jin Kyu; Lee, Chang Soo; Lee, Sang-Yup; Cho, Hyung Hee; Kim, Jong Hak

2016-12-01

Bimodal porous TiO2 (BP-TiO2) with large surface area, high porosity, good interconnectivity, and excellent light-scattering ability are synthesized via a facile one-step method using a self-assembled blend template consisting of an amphiphilic poly(vinyl chloride)-g-poly(oxyethylene methacrylate) (PVC-g-POEM) graft copolymer and a hydrophobic poly(vinyl chloride) (PVC) homopolymer. The hydrophilically surface-modified TiO2 nanoparticles selectively interact with the hydrophilic POEM chains, while the addition of the PVC homopolymer increases the hydrophobic domain size, resulting in the formation of dual pores (i.e., macropores and mesopores). The sizes and numbers of macropores can easily be controlled by changing the molecular weight and amount of the PVC homopolymer. The polymer electrolyte dye-sensitized solar cells (DSSCs) fabricated with BP-TiO2 photoanodes exhibited energy conversion efficiencies of up to 7.6% at 100 mW cm-2, which is much higher than those of mesoporous TiO2 (5.8%) with PVC-g-POEM only and conventional nanocrystalline TiO2 (4.9%) with commercial Dyesol paste. The enhanced energy conversion efficiencies mostly resulted from the light-scattering effects of the macropores, which increased the light-harvesting efficiencies. The improved light-harvesting and photovoltaic performances of the DSSCs were characterized by UV-vis spectroscopy, incident photon-to-current conversion efficiency analysis, electrochemical impedance spectroscopy, intensity-modulated photocurrent spectroscopy, and intensity-modulated photovoltage spectroscopy.

TiO2 nanoparticles versus TiO2-SiO2 nanocomposites: A comparative study of photo catalysis on acid red 88

NASA Astrophysics Data System (ADS)

Balachandran, K.; Venckatesh, Rajendran; Sivaraj, Rajeshwari; Rajiv, P.

2014-07-01

A novel, simple, less time-consuming and cost-effective wet chemical technique was used to synthesis TiO2 nanoparticles and TiO2-SiO2 nanocomposites using Titanium tetra isopropoxide (TTIP) as a precursor relatively at low temperature in acidic pH. Titania sol was prepared by hydrolysis of TTIP and was mixed with silicic acid and tetrahydrofuran mixture. The reaction was carried out under vigorous stirring for 6 h and dried at room temperature. The resulting powders were characterized by UV-Visible spectroscopy, Fourier transform infrared (FT-IR), X-ray diffraction, scanning electron microscope (SEM) and transmission electron microscope (TEM). The grain size of the particles was calculated by X-ray diffraction, surface morphology and chemical composition was determined from scanning electron microscopy-energy dispersive spectroscopy, metal oxide stretching was confirmed from FT-IR spectroscopy, band gap was calculated using UV-Visible spectroscopy. Surface area of the composite as calculated by BET analyzer and it was found to be 65 and 75 m2/g for TiO2 and TiO2-SiO2 respectively. The photocatalytic experiments were performed with aqueous solution of acid red 88 with TiO2 and TiO2-SiO2 batch studies for 4 h irradiation, direct photolysis of TiO2 and TiO2-SiO2 contributed 94.2% and 96.5% decomposition in solar radiation for the optimized concentration of acid red 88.

Annealing-Induced Bi Bilayer on Bi2Te3 Investigated via Quasi-Particle-Interference Mapping.

PubMed

Schouteden, Koen; Govaerts, Kirsten; Debehets, Jolien; Thupakula, Umamahesh; Chen, Taishi; Li, Zhe; Netsou, Asteriona; Song, Fengqi; Lamoen, Dirk; Van Haesendonck, Chris; Partoens, Bart; Park, Kyungwha

2016-09-27

Topological insulators (TIs) are renowned for their exotic topological surface states (TSSs) that reside in the top atomic layers, and hence, detailed knowledge of the surface top atomic layers is of utmost importance. Here we present the remarkable morphology changes of Bi2Te3 surfaces, which have been freshly cleaved in air, upon subsequent systematic annealing in ultrahigh vacuum and the resulting effects on the local and area-averaging electronic properties of the surface states, which are investigated by combining scanning tunneling microscopy (STM), scanning tunneling spectroscopy (STS), and Auger electron spectroscopy (AES) experiments with density functional theory (DFT) calculations. Our findings demonstrate that the annealing induces the formation of a Bi bilayer atop the Bi2Te3 surface. The adlayer results in n-type doping, and the atomic defects act as scattering centers of the TSS electrons. We also investigated the annealing-induced Bi bilayer surface on Bi2Te3 via voltage-dependent quasi-particle-interference (QPI) mapping of the surface local density of states and via comparison with the calculated constant-energy contours and QPI patterns. We observed closed hexagonal patterns in the Fourier transform of real-space QPI maps with secondary outer spikes. DFT calculations attribute these complex QPI patterns to the appearance of a "second" cone due to the surface charge transfer between the Bi bilayer and the Bi2Te3. Annealing in ultrahigh vacuum offers a facile route for tuning of the topological properties and may yield similar results for other topological materials.

Solar hydrogen and solar electricity using mesoporous materials

NASA Astrophysics Data System (ADS)

Mahoney, Luther

The development of cost-effective materials for effective utilization of solar energy is a major challenge for solving the energy problems that face the world. This thesis work relates to the development of mesoporous materials for solar energy applications in the areas of photocatalytic water splitting and the generation of electricity. Mesoporous materials were employed throughout the studies because of their favorable physico-chemical properties such as high surface areas and large porosities. The first project was related to the use of a cubic periodic mesoporous material, MCM-48. The studies showed that chromium loading directly affected the phase of mesoporous silica formed. Furthermore, within the cubic MCM-48 structure, the loading of polychromate species determined the concentration of solar hydrogen produced. In an effort to determine the potential of mesoporous materials, titanium dioxide was prepared using the Evaporation-Induced Self-Assembly (EISA) synthetic method. The aging period directly determined the amount of various phases of titanium dioxide. This method was extended for the preparation of cobalt doped titanium dioxide for solar simulated hydrogen evolution. In another study, metal doped systems were synthesized using the EISA procedure and rhodamine B (RhB) dye sensitized and metal doped titania mesoporous materials were evaluated for visible light hydrogen evolution. The final study employed various mesoporous titanium dioxide materials for N719 dye sensitized solar cell (DSSC) materials for photovoltaic applications. The materials were extensively characterized using powder X-ray diffraction (XRD), nitrogen physisorption, diffuse reflectance spectroscopy (DRS), UV-Vis spectroscopy, Fourier-Transform-Infrared Spectroscopy (FT-IR), Raman spectroscopy, chemisorption, photoluminescence (PL), X-ray photoelectron spectroscopy (XPS), and transmission electron microscopy (TEM). In addition, photoelectrochemical measurements were completed using current-voltage (I-V) curves, external quantum efficiency (EQE) curves, electrochemical impedance spectroscopy (EIS), and transient spectroscopy. The thesis work presented provides a better understanding of the role of mesoporous materials for solar hydrogen and solar electricity production.

Increase of porosity by combining semi-carbonization and KOH activation of formaldehyde resins to prepare high surface area carbons for supercapacitor applications

NASA Astrophysics Data System (ADS)

Heimböckel, Ruben; Kraas, Sebastian; Hoffmann, Frank; Fröba, Michael

2018-01-01

A series of porous carbon samples were prepared by combining a semi-carbonization process of acidic polymerized phenol-formaldehyde resins and a following chemical activation with KOH used in different ratios to increase specific surface area, micropore content and pore sizes of the carbons which is favourable for supercapacitor applications. Samples were characterized by nitrogen physisorption, powder X-ray diffraction, Raman spectroscopy and scanning electron microscopy. The results show that the amount of KOH, combined with the semi-carbonization step had a remarkable effect on the specific surface area (up to SBET: 3595 m2 g-1 and SDFT: 2551 m2 g-1), pore volume (0.60-2.62 cm3 g-1) and pore sizes (up to 3.5 nm). The carbons were tested as electrode materials for electrochemical double layer capacitors (EDLC) in a two electrode setup with tetraethylammonium tetrafluoroborate in acetonitrile as electrolyte. The prepared carbon material with the largest surface area, pore volume and pore sizes exhibits a high specific capacitance of 145.1 F g-1 at a current density of 1 A g-1. With a high specific energy of 31 W h kg-1 at a power density of 33028 W kg-1 and a short time relaxation constant of 0.29 s, the carbon showed high power capability as an EDLC electrode material.

One-step electrodeposition process to fabricate corrosion-resistant superhydrophobic surface on magnesium alloy.

PubMed

Liu, Qin; Chen, Dexin; Kang, Zhixin

2015-01-28

A simple, one-step method has been developed to construct a superhydrophobic surface by electrodepositing Mg-Mn-Ce magnesium plate in an ethanol solution containing cerium nitrate hexahydrate and myristic acid. Scanning electron microscopy, energy-dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy, and Fourier transform infrared spectroscopy were employed to characterize the surfaces. The shortest electrodeposition time to obtain a superhydrophobic surface was about 1 min, and the as-prepared superhydrophobic surfaces had a maximum contact angle of 159.8° and a sliding angle of less than 2°. Potentiodynamic polarization and electrochemical impedance spectroscopy measurements demonstrated that the superhydrophobic surface greatly improved the corrosion properties of magnesium alloy in 3.5 wt % aqueous solutions of NaCl, Na2SO4, NaClO3, and NaNO3. Besides, the chemical stability and mechanical durability of the as-prepared superhydrophobic surface were also examined. The presented method is rapid, low-cost, and environmentally friendly and thus should be of significant value for the industrial fabrication of anticorrosive superhydrophobic surfaces and should have a promising future in expanding the applications of magnesium alloys.

Study of Surface Wettability Change of Unconsolidated Sand Using Diffuse Reflectance Infrared Fourier Transform Spectroscopy and Thermogravimetric Analysis.

PubMed

Gómora-Herrera, Diana; Navarrete Bolaños, Juan; Lijanova, Irina V; Olivares-Xometl, Octavio; Likhanova, Natalya V

2018-04-01

The effects exerted by the adsorption of vapors of a non-polar compound (deuterated benzene) and a polar compound (water) on the surface of Ottawa sand and a sample of reservoir sand (Channel), which was previously impregnated with silicon oil or two kinds of surfactants, (2-hydroxyethyl) trimethylammonium oleate (HETAO) and (2-hydroxyethyl)trimethylammonium azelate (HETAA), were studied by diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) and thermogravimetric analysis (TGA). The surface chemistry of the sandstone rocks was elucidated by X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM) with energy dispersive X-ray spectroscopy (EDX). Terminal surface groups such as hydroxyls can strongly adsorb molecules that interact with these surface groups (surfactants), resulting in a wettability change. The wettability change effect suffered by the surface after treating it with surfactants was possible to be detected by the DRIFTS technique, wherein it was observed that the surface became more hydrophobic after being treated with silicon oil and HETAO; the surface became more hydrophilic after treating it with HETAA.

Architecture-dependent surface chemistry for Pt monolayers on carbon-supported Au.

PubMed

Cheng, Shuang; Rettew, Robert E; Sauerbrey, Marc; Alamgir, Faisal M

2011-10-01

Pt monolayers were grown by surface-limited redox replacement (SLRR) on two types of Au nanostructures. The Au nanostructures were fabricated electrochemically on carbon fiber paper (CFP) by either potentiostatic deposition (PSD) or potential square wave deposition (PSWD). The morphology of the Au/CFP heterostructures, examined using scanning electron microscopy (SEM), was found to depend on the type of Au growth method employed. The properties of the Pt deposit, as studied using X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XAS), and cyclic voltammetry (CV), were found to depend strongly on the morphology of the support. Specifically, it was found that smaller Au morphologies led to a higher degree of cationicity in the resulting Pt deposit, with Pt(4+) and Pt(2+) species being identified using XPS and XAS. For fuel-cell catalysts, the resistance of ultrathin catalyst deposits to surface area loss through dissolution, poisoning, and agglomeration is critical. This study shows that an equivalent of two monolayers (ML) is the low-loading limit of Pt on Au. At 1 ML or below, the Pt film decreases in activity and durability very rapidly due to presence of cationic Pt. © 2011 American Chemical Society

Structure and magnetic properties of FeSiAl-based soft magnetic composite with AlN and Al2O3 insulating layer prepared by selective nitridation and oxidation

NASA Astrophysics Data System (ADS)

Zhong, Xiaoxi; Liu, Ying; Li, Jun; Wang, Yiwei

2012-08-01

FeSiAl is widely used in switching power supply, filter inductors and pulse transformers. But when used under higher frequencies in some particular condition, it is required to reduce its high-frequency loss. Preparing a homogeneous insulating coating with good heat resistance and high resistivity, such as AlN and Al2O3, is supposed to be an effective way to reduce eddy current loss, which is less focused on. In this project, mixed AlN and Al2O3 insulating layers were prepared on the surface of FeSiAl powders after 30 min exposure at 1100 °C in high purity nitrogen atmosphere, by means of surface nitridation and oxidation. The results revealed that the insulating layers increase the electrical resistivity, and hence decrease the loss factor, improve the frequency stability and increase the quality factor, especially in the high-frequency range. The morphologies, microstructure and compositions of the oxidized and nitrided products on the surface were characterized by Scanning Electron Microscopy/Energy Disperse Spectroscopy, X-Ray Diffraction, Transmission Electron Microscopy, Selected Area Electron Diffraction and X-ray Photoelectron Spectroscopy.

Advanced oxidation (H₂O₂ and/or UV) of functionalized carbon nanotubes (CNT-OH and CNT-COOH) and its influence on the stabilization of CNTs in water and tannic acid solution.

PubMed

Czech, Bożena; Oleszczuk, Patryk; Wiącek, Agnieszka

2015-05-01

The properties of carbon nanotubes (CNTs) functionalized with -OH and -COOH groups during simulated water treatment with H2O2 and/or UV were tested. There following properties of CNTs were investigated: specific surface area, elemental composition (CHN), dynamic light scattering, Raman spectroscopy, X-ray photoelectron spectroscopy and changes in the CNTs structure were observed using transmission electron microscopy. Treatment of CNTs with H2O2 and/or UV affected their properties. This effect, however, was different depending on the functionalization of CNTs and also on the factor used (UV and/or H2O2). H2O2 plays a key role as a factor modifying the surface of CNT-OHs, whereas the properties of CNT-COOHs were most affected by UV rays. A shortening of the nanotubes, exfoliation, the opening of their ends, and changes in the surface charge were observed as a result of the action of UV and/or H2O2. The changes in observed parameters may influence the stability of the aqueous suspensions of CNTs. Copyright © 2015 Elsevier Ltd. All rights reserved.

Surface modification of a natural zeolite by treatment with cold oxygen plasma: Characterization and application in water treatment

NASA Astrophysics Data System (ADS)

De Velasco-Maldonado, Paola S.; Hernández-Montoya, Virginia; Montes-Morán, Miguel A.; Vázquez, Norma Aurea-Rangel; Pérez-Cruz, Ma. Ana

2018-03-01

In the present work the possible surface modification of natural zeolite using cold oxygen plasma was studied. The sample with and without treatment was characterized using nitrogen adsorption isotherms at -196 °C, FT-IR spectroscopy, SEM/EDX analysis and X-Ray Diffraction. Additionally, the two samples were used for the removal of lead and acid, basic, reactive and food dyes in batch systems. The natural zeolite was found to be a mesoporous material with a low specific surface area (23 m2/g). X-ray patterns confirmed that clinoptilolite was the main crystal structure present in the natural zeolite. The molecular properties of dyes and the zeolitic structure were studied using molecular simulation, with the purpose to understand the adsorption mechanism. The results pointed out that only the roughness of the clinoptilolite was affected by the plasma treatment, whereas the specific surface area, chemical functionality and crystal structure remained constant. Finally, adsorption results confirmed that the plasma treatment had no significant effects on the dyes and lead retention capacities of the natural zeolite.

New Possibilities for Understanding Complex Metal Hydrides via Synchrotron X-ray Studies

NASA Astrophysics Data System (ADS)

Dobbins, Tabbetha

2008-03-01

Ultrasmall-angle x-ray scattering (USAXS) and X-ray absorption spectroscopy (XAS) are used for the study of chemical and morphological changes in metal hydride powder (e.g. NaAlH4) both before and after transition metal salt catalytic dopant additions by high energy ball milling. The variation in surface fractal dimension and particle size with milling time and dopant content were tracked. These studies show that dopant content level (e.g. 2 mol % and 4 mol %) and dopant type (i.e. TiCl2, TiCl3, VCl3, and ZrCl4) markedly affects NaAlH4 powder particle surface area (determined using USAXS surface fractal dimension). As well, the chemical reaction between the catalyst and hydride powder was further elucidated using XAS. Ti-metal reacts with the Al desorption product (from NaAlH4) to form TiAlx product phases. These studies were able to link powder particle surface area to catalytic doping and were able to link dopant chemical state with dehydrogenation reactant and product phases.

Investigation of the surface sensitivity of positron-annihilation-induced Auger-electron spectroscopy

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

Mehl, D.R.

1990-01-01

The first surface sensitivity studies of positron-annihilation-induced Auger-electron spectroscopy (PAES) are presented. Preliminary measurements on polycrystalline Al with adsorbates indicate that PAES is more selective of the surface than conventional electron-induced Auger electron spectroscopy (EAES). PAES and EAES studies of well-defined overlayer-metal systems of Cu(110)+S and Cu(110)+Cs verify that PAES is selective of the top atomic layer. This surface selectivity is accounted for by theoretical calculations which indicate that the positron surface state is displaced away from the substrate by the over-layer, decreasing the annihilation rate of positrons with substrate core electrons.

Surface contamination analysis technology team overview

NASA Astrophysics Data System (ADS)

Burns, H. Dewitt, Jr.

1996-11-01

The surface contamination analysis technology (SCAT) team was originated as a working roup of NASA civil service, Space Shuttle contractor, and university groups. Participating members of the SCAT Team have included personnel from NASA Marshall Space Flight Center's Materials and Processes Laboratory and Langley Research Center's Instrument Development Group; contractors-Thiokol Corporation's Inspection Technology Group, AC Engineering support contractor, Aerojet, SAIC, and Lockheed MArtin/Oak Ridge Y-12 support contractor and Shuttle External Tank prime contractor; and the University of Alabama in Huntsville's Center for Robotics and Automation. The goal of the SCAT team as originally defined was to develop and integrate a multi-purpose inspection head for robotic application to in-process inspection of contamination sensitive surfaces. One area of interest was replacement of ozone depleting solvents currently used for surface cleanliness verification. The team approach brought together the appropriate personnel to determine what surface inspection techniques were applicable to multi-program surface cleanliness inspection. Major substrates of interest were chosen to simulate space shuttle critical bonding surface or surfaces sensitive to contamination such as fuel system component surfaces. Inspection techniques evaluated include optically stimulated electron emission or photoelectron emission; Fourier transform infrared spectroscopy; near infrared fiber optic spectroscopy; and, ultraviolet fluorescence. Current plans are to demonstrate an integrated system in MSFC's Productivity Enhancement Complex within five years from initiation of this effort in 1992. Instrumentation specifications and designs developed under this effort include a portable diffuse reflectance FTIR system built by Surface Optics Corporation and a third generation optically stimulated electron emission system built by LaRC. This paper will discuss the evaluation of the various techniques on a number of substrate materials contaminated with hydrocarbons, silicones, and fluorocarbons. Discussion will also include standards development for instrument calibration and testing.

Influence of head size on the development of metallic wear and on the characteristics of carbon layers in metal-on-metal hip joints

PubMed Central

Sprecher, Christoph M; Wimmer, Markus A; Milz, Stefan; Taeger, Georg

2009-01-01

Background and purpose Particles originating from the articulating surfaces of hip endoprostheses often induce an inflammatory response, which can be related to implant failure. We therefore analyzed the metal content in capsular tissue from 44 McKee-Farrar metal-on-metal hip prostheses (with 3 different head sizes) and we also analyzed the morphological structure of layers located on articulating surfaces. Methods Atomic absorption spectrometry (AAS) was used to analyze the metal content in capsular tissue. Visually detectable carbon layers located on the articulating surfaces were evaluated using scanning electron microscopy (SEM), energy-dispersive Xray spectroscopy (EDX), and X-ray photoelectron spectroscopy (XPS). Results Metallic debris was detected in all capsular tissue samples but no statistically significant differences in metal content were found in relation to implant head size. The morphological characteristics of the different layer zones allowed an exact analysis of contact and non-contact areas. Furthermore, surface layers appear to have a protective function because they can prevent sharp-edged particles from damaging the prostheses surface. Interpretation The implant head size does not appear to influence the amount of metallic debris. The layers obviously act like a lubricating agent because the protection function does not occur in regions without layers where the metal surface often shows numerous scratches. As layers are not generated immediately after the implantation of hip prostheses, these findings may at least partially explain the high amount of wear early after implantation. PMID:19421914

Multinuclear solid film state NMR studies of metal oxide catalysts and minerals

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

Maxwell, R.S.; Stec, D.F.; Ellis, P.D.

1996-10-01

Several of our investigations of heterogeneous process by novel NMR experiments and analyses are reviewed and the utility and limitations of NMR spectroscopy for these areas discussed. Out studies have included the following: dynamics and arrangements of proton-containing adsorbates, primarily Bronsted acid sites and water, on the surface of zirconia and alumina catalysts; hydrogen dynamics and coordinates in synthetic aluminum oxyhydroxides; phase separation and crystallinity of synthetic minerals. In combination with the complementary results obtained in our laboratory via infrared spectroscopy, thermal analysis (primarily TGA and DSC), and catalytic activity measurements, these NMR data provide unique and valuable information onmore » atomic and molecular dynamics, identities, and structures without requiring pristine, single crystal specimens.« less

Noble Metal Immersion Spectroscopy of Silica Alcogels and Aerogels

NASA Technical Reports Server (NTRS)

Smith, David D.; Sibille, Laurent; Cronise, Raymond J.; Noever, David A.

1998-01-01

We have fabricated aerogels containing gold and silver nanoparticles for gas catalysis applications. By applying the concept of an average or effective dielectric constant to the heterogeneous interlayer surrounding each particle, we extend the technique of immersion spectroscopy to porous or heterogeneous media. Specifically, we apply the predominant effective medium theories for the determination of the average fractional composition of each component in this inhomogeneous layer. Hence, the surface area of metal available for catalytic gas reaction is determined. The technique is satisfactory for statistically random metal particle distributions but needs further modification for aggregated or surfactant modified systems. Additionally, the kinetics suggest that collective particle interactions in coagulated clusters are perturbed during silica gelation resulting in a change in the aggregate geometry.

Interaction of hydrogen chloride with alumina. [atmospheric effluent concentrations and interaction of solid rocket propellants used in space shuttle

NASA Technical Reports Server (NTRS)

Bailey, R. R.; Wightman, J. P.

1978-01-01

The influence of temperature, pressure, and outgas conditions on the absorption of hydrogen chloride and water vapor on both alpha and gamma alumina was studied. Characterization of the adsorbents was performed using X-ray powder diffraction, scanning electron microscopy (SEM), low temperature nitrogen adsorption desorption measurements, BET nitrogen surface area measurements and electron spectroscopy for chemical analysis (ESCA). Water vapor adsorption isotherms at 30, 40, and 50 C were measured on alpha and gamma alumina after outgassing at 80, 200, and 400 C. Both outgas temperature and adsorption temperature influenced the adsorption of water vapor on the aluminas. The water vapor adsorption was completely reversible. Alpha alumina absorbed more water per unit area than gamma alumina. Differences in the adsorption capacity for water vapor of the two aluminas were explained on the basis of ideal surface models of alpha and gamma alumina. Isosteric heats of adsorption for water vapor on the aluminas were determined over a limited range of surface coverage.

Enhanced capture of elemental mercury by bamboo-based sorbents.

PubMed

Tan, Zengqiang; Xiang, Jun; Su, Sheng; Zeng, Hancai; Zhou, Changsong; Sun, Lushi; Hu, Song; Qiu, Jianrong

2012-11-15

To develop cost-effective sorbent for gas-phase elemental mercury removal, the bamboo charcoal (BC) produced from renewable bamboo and KI modified BC (BC-I) were used for elemental mercury removal. The effect of NO, SO2 on gas-phase Hg0 adsorption by KI modified BC was evaluated on a fixed bed reactor using an online mercury analyzer. BET surface area analysis, temperature programmed desorption (TPD) and X-ray photoelectron spectroscopy (XPS) were used to determine the pore structure and surface chemistry of the sorbents. The results show that KI impregnation reduced the sorbents' BET surface area and total pore volume compared with that of the original BC. But the BC-I has excellent adsorption capacity for elemental mercury at a relatively higher temperature of 140 °C and 180 °C. The presence of NO or SO2 could inhibit Hg0 capture, but BC-I has strong anti-poisoning ability. The specific reaction mechanism has been further analyzed. Copyright © 2012 Elsevier B.V. All rights reserved.

Proton NMR studies of functionalized nanoparticles in aqueous environments

NASA Astrophysics Data System (ADS)

Tataurova, Yulia Nikolaevna

Nanoscience is an emerging field that can provide potential routes towards addressing critical issues such as clean and sustainable energy, environmental remediation and human health. Specifically, porous nanomaterials, such as zeolites and mesoporous silica, are found in a wide range of applications including catalysis, drug delivery, imaging, environmental protection, and sensing. The characterization of the physical and chemical properties of nanocrystalline materials is essential to the realization of these innovative applications. The great advantage of porous nanocrystals is their increased external surface area that can control their biological, chemical and catalytic activities. Specific functional groups synthesized on the surface of nanoparticles are able to absorb heavy metals from the solution or target disease cells, such as cancer cells. In these studies, three main issues related to functionalized nanomaterials will be addressed through the application of nuclear magnetic resonance (NMR) techniques including: 1) surface composition and structure of functionalized nanocrystalline particles; 2) chemical properties of the guest molecules on the surface of nanomaterials, and 3) adsorption and reactivity of surface bound functional groups. Nuclear magnetic resonance (NMR) is one of the major spectroscopic techniques available for the characterization of molecular structure and conformational dynamics with atomic level detail. This thesis deals with the application of 1H solution state NMR to porous nanomaterial in an aqueous environment. Understanding the aqueous phase behavior of functionalized nanomaterials is a key factor in the design and development of safe nanomaterials because their interactions with living systems are always mediated through the aqueous phase. This is often due to a lack of fundamental knowledge in interfacial chemical and physical phenomena that occur on the surface of nanoparticles. The use of solution NMR spectroscopy results in high-resolution NMR spectra. This technique is selective for protons on the surface organic functional groups due to their motional averaging in solution. In this study, 1H solution NMR spectroscopy was used to investigate the interface of the organic functional groups in D2O. The pKa for these functional groups covalently bound to the surface of nanoparticles was determined using an NMR-pH titration method based on the variation in the proton chemical shift for the alkyl group protons closest to the amine group with pH. The adsorption of toxic contaminants (chromate and arsenate anions) on the surface of functionalized silicalite-1 and mesoporous silica nanoparticles has been studied by 1H solution NMR spectroscopy. With this method, the surface bound contaminants are detected. The analysis of the intensity and position of these peaks allows quantitative assessment of the relative amounts of functional groups with adsorbed metal ions. These results demonstrate the sensitivity of solution NMR spectroscopy to the electronic environment and structure of the surface functional groups on porous nanomaterials.

Characterization of Surface-Active Biofilm Protein BslA in Self-Assembling Langmuir Monolayer at the Air-Water Interface.

PubMed

Liu, Wei; Li, Shanghao; Wang, Zhuguang; Yan, Elsa C Y; Leblanc, Roger M

2017-08-01

Biofilm is an extracellular matrix of bacteria and serves as a protective shield of bacterial communities. It is crucial for microbial growth and one of the leading causes of human chronic infections as well. However, the structures and molecular mechanism of biofilm formation remain largely unknown. Here, we examined a protein, BslA, expressed in the biofilms of Bacillus subtilis. We characterized the Langmuir monolayers of BslA at the air/water interface. Using techniques in surface chemistry and spectroscopy, we found that BslA forms a stable and robust Langmuir monolayer at the air/water interface. Our results show that the BslA Langmuir monolayer underwent two-stage elasticity in the solid state phase upon mechanical compression: one is possibly due to the intermolecular interaction and the other is likely due to both the intermolecular compulsion and the intramolecular distortion. The Langmuir monolayer of BslA shows abrupt changes in rigidities and elasticities at ∼25 mN/m. This surface pressure is close to the one at which BlsA saturates the air/water interface as a self-assembled film without mechanical compression, corresponding to a mean molecular area of ∼700 Å 2 per molecule. Based on the results of surface UV-visible spectroscopy and infrared reflective-absorption spectroscopy, we propose that the BslA Langmuir monolayer carries intermolecular elasticity before ∼25 mN/m and both intermolecular and intramolecular elasticity after ∼25 mN/m. These results provide valuable insights into the understanding of biofilm-associated protein under high mechanical force, shedding light on further investigation of biofilm structure and functionalities.

Surface enhanced Raman spectroscopy: A review of recent applications in forensic science.

PubMed

Fikiet, Marisia A; Khandasammy, Shelby R; Mistek, Ewelina; Ahmed, Yasmine; Halámková, Lenka; Bueno, Justin; Lednev, Igor K

2018-05-15

Surface enhanced Raman spectroscopy has many advantages over its parent technique of Raman spectroscopy. Some of these advantages such as increased sensitivity and selectivity and therefore the possibility of small sample sizes and detection of small concentrations are invaluable in the field of forensics. A variety of new SERS surfaces and novel approaches are presented here on a wide range of forensically relevant topics. Copyright © 2018 Elsevier B.V. All rights reserved.

Laer-induced Breakdown Spectroscopy Instrument for Element Analysis of Planetary Surfaces

NASA Technical Reports Server (NTRS)

Blacic, J.; Pettit, D.; Cremers, D.; Roessler, N.

1993-01-01

One of the most fundamental pieces of information about any planetary body is the elemental and mineralogical composition of its surface materials. We are developing an instrument to obtain such data at ranges of up to several hundreds of meters using the technique of Laser-Induced Breakdown Spectroscopy (LIBS). We envision our instrument being used from a spacecraft in close rendezvous with small bodies such as comets and asteroids, or deployed on surface-rover vehicles on large bodies such as Mars and the Moon. The elemental analysis is based on atomic emission spectroscopy of a laser-induced plasma or spark. A pulsed, diode pumped Nd:YAG laser of several hundred millijoules optical energy is used to vaporize and electronically excite the constituent elements of a rock surface remotely located from the laser. Light emitted from the excited plasma is collected and introduced to the entrance slit of a small grating spectrometer. The spectrally dispersed spark light is detected with either a linear photo diode array or area CCD array. When the latter detector is used, the optical and spectrometer components of the LIBS instrument can also be used in a passive imaging mode to collect and integrate reflected sunlight from the same rock surface. Absorption spectral analysis of this reflected light gives mineralogical information that provides a remote geochemical characterization of the rock surface. We performed laboratory calibrations in air and in vacuum on standard rock powders to quantify the LIBS analysis. We performed preliminary field tests using commercially available components to demonstrate remote LIBS analysis of terrestrial rock surfaces at ranges of over 25 m, and we have demonstrated compatibility with a six-wheeled Russian robotic rover vehicle. Based on these results, we believe that all major and most minor elements expected on planetary surfaces can be measured with absolute accuracy of 10-15 percent and much higher relative accuracy. We have performed preliminary systems analysis of a LIBS instrument to evaluate probable mass and power requirements; results of this analysis are summarized.

Ultrafast and nonlinear surface-enhanced Raman spectroscopy.

PubMed

Gruenke, Natalie L; Cardinal, M Fernanda; McAnally, Michael O; Frontiera, Renee R; Schatz, George C; Van Duyne, Richard P

2016-04-21

Ultrafast surface-enhanced Raman spectroscopy (SERS) has the potential to study molecular dynamics near plasmonic surfaces to better understand plasmon-mediated chemical reactions such as plasmonically-enhanced photocatalytic or photovoltaic processes. This review discusses the combination of ultrafast Raman spectroscopic techniques with plasmonic substrates for high temporal resolution, high sensitivity, and high spatial resolution vibrational spectroscopy. First, we introduce background information relevant to ultrafast SERS: the mechanisms of surface enhancement in Raman scattering, the characterization of plasmonic materials with ultrafast techniques, and early complementary techniques to study molecule-plasmon interactions. We then discuss recent advances in surface-enhanced Raman spectroscopies with ultrafast pulses with a focus on the study of molecule-plasmon coupling and molecular dynamics with high sensitivity. We also highlight the challenges faced by this field by the potential damage caused by concentrated, highly energetic pulsed fields in plasmonic hotspots, and finally the potential for future ultrafast SERS studies.

Raman spectroscopy and atomic force microscopy study of interfacial polytypism in GaP/Ge(111) heterostructures

NASA Astrophysics Data System (ADS)

Aggarwal, R.; Ingale, Alka A.; Dixit, V. K.

2018-01-01

Effects of lattice and polar/nonpolar mismatch between the GaP layer and Ge(111) substrate are investigated by spatially resolved Raman spectroscopy. The red shifted transverse optical (TO) and longitudinal optical (LO) phonons due to residual strain, along with asymmetry to TO phonon ∼358 cm-1 are observed in GaP/Ge(111). The peak intensity variation of mode ∼358 cm-1 with respect to TO phonon across the crystallographic morphed surface of GaP micro structures is associated with the topographical variations using atomic force microscopy mapping and Raman spectroscopy performed on both in plane and cross-sectional surface. Co-existence of GaP allotropes, i.e. wurtzite phase near heterojunction interface and dominant zinc-blende phase near surface is established using the spatially resolved polarized Raman spectroscopy from the cross sectional surface of heterostructures. This consistently explains effect of surface morphology on Raman spectroscopy from GaP(111). The study shows the way to identify crystalline phases in other advanced semiconductor heterostructures without any specific sample preparation.

Spectroscopic and volumetric characterization of a non-microporous amorphous ice

NASA Astrophysics Data System (ADS)

Manca, C.; Martin, C.; Roubin, P.

2002-10-01

The aim of this Letter is to re-investigate the characterization of ice porosity. N 2, CH 4 and Ar adsorption on amorphous ice has been compared to that on crystalline ice at low temperatures, using adsorption isotherm volumetry and infrared spectroscopy simultaneously. Here we show that amorphous ice can present a large specific surface area and nevertheless be non-microporous; this provides new ways for the understanding of interstellar reactivity.

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.

Infrared Spectroscopy as a Chemical Fingerprinting Tool

NASA Technical Reports Server (NTRS)

Huff, Timothy L.

2003-01-01

Infrared (IR) spectroscopy is a powerful analytical tool in the chemical fingerprinting of materials. Any sample material that will interact with infrared light produces a spectrum and, although normally associated with organic materials, inorganic compounds may also be infrared active. The technique is rapid, reproducible and usually non-invasive to the sample. That it is non-invasive allows for additional characterization of the original material using other analytical techniques including thermal analysis and RAMAN spectroscopic techniques. With the appropriate accessories, the technique can be used to examine samples in liquid, solid or gas phase. Both aqueous and non-aqueous free-flowing solutions can be analyzed, as can viscous liquids such as heavy oils and greases. Solid samples of varying sizes and shapes may also be examined and with the addition of microscopic IR (microspectroscopy) capabilities, minute materials such as single fibers and threads may be analyzed. With the addition of appropriate software, microspectroscopy can be used for automated discrete point or compositional surface area mapping, with the latter providing a means to record changes in the chemical composition of a material surface over a defined area. Due to the ability to characterize gaseous samples, IR spectroscopy can also be coupled with thermal processes such as thermogravimetric (TG) analyses to provide both thermal and chemical data in a single run. In this configuration, solids (or liquids) heated in a TG analyzer undergo decomposition, with the evolving gases directed into the IR spectrometer. Thus, information is provided on the thermal properties of a material and the order in which its chemical constituents are broken down during incremental heating. Specific examples of these varied applications will be cited, with data interpretation and method limitations further discussed.

One-step synthesis of vertically aligned anatase thornbush-like TiO2 nanowire arrays on transparent conducting oxides for solid-state dye-sensitized solar cells.

PubMed

Roh, Dong Kyu; Chi, Won Seok; Ahn, Sung Hoon; Jeon, Harim; Kim, Jong Hak

2013-08-01

Herein, we report a facile synthesis of high-density anatase-phase vertically aligned thornbush-like TiO2 nanowires (TBWs) on transparent conducting oxide glasses. Morphologically controllable TBW arrays of 9 μm in length are generated through a one-step hydrothermal reaction at 200 °C over 11 h using potassium titanium oxide oxalate dehydrate, diethylene glycol (DEG), and water. The TBWs consist of a large number of nanoplates or nanorods, as confirmed by SEM and TEM imaging. The morphologies of TBWs are controllable by adjusting DEG/water ratios. TBW diameters gradually decrease from 600 (TBW600) to 400 (TBW400) to 200 nm (TBW200) and morphologies change from nanoplates to nanorods with an increase in DEG content. TBWs are utilized as photoanodes for quasi-solid-state dye-sensitized solar cells (qssDSSCs) and solid-state DSSCs (ssDSSCs). The energy-conversion efficiency of qssDSSCs is in the order: TBW200 (5.2%)>TBW400 (4.5%)>TBW600 (3.4%). These results can be attributed to the different surface areas, light-scattering effects, and charge transport rates, as confirmed by dye-loading measurements, reflectance spectroscopy, and incident photon-to-electron conversion efficiency and intensity-modulated photovoltage spectroscopy/intensity-modulated photocurrent spectroscopy analyses. TBW200 is further treated with a graft-copolymer-directed organized mesoporous TiO2 to increase the surface area and interconnectivity of TBWs. As a result, the energy-conversion efficiency of the ssDSSC increases to 6.7% at 100 mW cm(-2) , which is among the highest values for N719-dye-based ssDSSCs. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Surface Optical Rectification from Layered MoS2 Crystal by THz Time-Domain Surface Emission Spectroscopy.

PubMed

Huang, Yuanyuan; Zhu, Lipeng; Zhao, Qiyi; Guo, Yaohui; Ren, Zhaoyu; Bai, Jintao; Xu, Xinlong

2017-02-08

Surface optical rectification was observed from the layered semiconductor molybdenum disulfide (MoS 2 ) crystal via terahertz (THz) time-domain surface emission spectroscopy under linearly polarized femtosecond laser excitation. The radiated THz amplitude of MoS 2 has a linear dependence on ever-increasing pump fluence and thus quadratic with the pump electric field, which discriminates from the surface Dember field induced THz radiation in InAs and the transient photocurrent-induced THz generation in graphite. Theoretical analysis based on space symmetry of MoS 2 crystal suggests that the underlying mechanism of THz radiation is surface optical rectification under the reflection configuration. This is consistent with the experimental results according to the radiated THz amplitude dependences on azimuthal and incident polarization angles. We also demonstrated the damage threshold of MoS 2 due to microscopic bond breaking under the femtosecond laser irradiation, which can be monitored via THz time-domain emission spectroscopy and Raman spectroscopy.

Effect of support size on the catalytic activity of metal-oxide-doped silica particles in the glycolysis of polyethylene terephthalate.

PubMed

Wi, Rinbok; Imran, Muhammad; Lee, Kyoung G; Yoon, Sun Hong; Cho, Bong Gyoo; Kim, Do Hyun

2011-07-01

Zinc oxide (ZnO) and cerium oxide (CeO2) nanoparticles were deposited on the surface of preformed silica spheres with diameters ranging from 60 to 750 nm. Ultrasonic irradiation was employed to promote the deposition of the metal oxide nanoparticles on the surface of silica. Silica-supported zinc oxide or cerium oxide was used as a catalyst in the glycolysis of polyethylene terephthalate, one of the key processes in the depolymerization of polyethylene terephthalate. The effect of the support size on the catalytic activity was studied in terms of monomer yield, and the monomer concentration was analyzed via high-performance liquid chromatography (HPLC). The morphologies and surface properties of the catalysts were characterized using a scanning electron microscope, a transmission electron microscope, and a BET surface area analyzer, while the monomer was characterized via HPLC and nuclear-magnetic-resonance spectroscopy. Both the zinc oxide and cerium oxide deposited on a smaller support showed better distribution and less aggregation. The high specific surface area of the smaller support catalysts provided a large number of active sites. The highest monomer yield was obtained with a catalyst of 60-nm silica support.

Preparation of Pd-loaded La-doped TiO2 nanotubes and investigation of their photocatalytic activity under visible light

NASA Astrophysics Data System (ADS)

Zong, Lanlan; Li, Qiuye; Zhang, Jiwei; Wang, Xiaodong; Yang, Jianjun

2013-11-01

Orthorhombic titanic acid nanotubes (TAN) have large BET surface area and small-diameter one-dimensional nanotubular morphology, so they can work as a good supporter and a precursor of TiO2. However, in our former research, we found that calcination of TAN to anatase TiO2 would destroy the nanotubular structure and decrease the BET surface area sharply. In this work, we utilized the pillar effect of the foreign nanoparticles (La2O3) to keep the nanotubular morphology of TiO2, and obtained the anatase TiO2 nanotubes with large BET surface area. For improving the photocatalytic activity, Pd nanoparticles were loaded as the electron traps on the surface of La-doped TiO2 by photo-deposition method. The photocatalysts were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, transmission electron microscopy, diffuse reflectance spectra, and N2 adsorption-desorption isotherms measurement. Their photocatalytic activities were evaluated by the removal of propylene under visible light irradiation ( λ ≥ 420 nm). The results showed that the photocatalytic activity of Pd-loaded La-doped TiO2 nanotubes improved effectively compared with that of La-doped TiO2 and pure TiO2.

Nanoporous activated carbon derived from Lapsi (Choerospondias axillaris) seed stone for the removal of arsenic from water.

PubMed

Rajbhandari, Rinita; Shrestha, Lok Kumar; Pradhananga, Raja Ram

2012-09-01

Activated carbons were prepared from Lapsi (Choerospondias axillaris) seed stone by zinc chloride (ZnCl2) activation at three different Lapsi seed powder (LSP):ZnCl2 ratios: 1:0.5 (AC-0.5), 1:1 (AC-1), and 1:2 (AC-2). The properties of these activated carbons (ACs), including effective surface areas, pore volumes, and pore size distributions were characterized from N2 adsorption-desorption isotherms. The ACs obtained were essentially nanoporous (including both micro- and mesoporous) with effective surface area ranging from 1167 to 1328 m2/g. Fourier-transform infrared (FTIR) spectroscopy showed the presence of functional groups on the surface of ACs. Scanning electron microscopy (SEM) images showed a high pore development in the ACs. X-ray diffraction (XRD) patterns showed that, in addition to the amorphous structure, ACs contains crystalline ZnO formed during the carbonization. Presence of amorphous carbon is further confirmed by Raman scattering, where we observed only D and G bands. Iron impregnated nanoporous AC has been found to be very effective for arsenic removal from ground water; amount of arsenic is decreased from ca. 200 ppb to 10 ppb. These experimental results indicate the potential use of Lapsi seed as a precursor material for the preparation of high surface area nanoporous activated carbons.

Raman imaging of lipid bilayer membrane by surface enhanced Raman scattering

NASA Astrophysics Data System (ADS)

Mori, Motoaki; Abe, Shunsuke; Kondo, Takahiro; Saito, Yuika

2018-04-01

We investigated two-dimensional lipid bilayers by spectroscopic imaging with surface enhanced Raman spectroscopy (SERS). A DSPC lipid bilayer incubated on a glass substrate was coated with a thin layer of silver. Due to the strong electromagnetic enhancement of the silver film and the affinity to lipid molecules, the Raman spectrum of a single bilayer was obtained in a 1 s exposure time with 0.1 mW of incident laser power. In the C-H vibrational region of the spectra, which is sensitive to bilayer configurations, a randomly stacked area was dominated by the CH3 asymmetric-stretch mode, whereas flat areas including double bilayers showed typical SERS spectra. The spectral features of the randomly stacked area are explained by the existence of many free lipid molecules, which is supported by DFT calculations of paired DSPC molecules. Our method can be applied to reveal the local crystallinity of single lipid bilayers, which is difficult to assess by conventional Raman imaging.

Application of modern surface analytical tools in the investigation of surface deterioration processes

NASA Technical Reports Server (NTRS)

Buckley, D. H.

1983-01-01

Surface profilometry and scanning electron microscopy were utilized to study changes in the surface of polymers when eroded. The X-ray photoelectron spectroscopy (XPS) and depth profile analysis indicate the corrosion of metal and ceramic surfaces and reveal the diffusion of certain species into the surface to produce a change in mechanical properties. Ion implantation, nitriding and plating and their effects on the surface are characterized. Auger spectroscopy analysis identified morphological properties of coatings applied to surfaces by sputter deposition.

New constraints on deformation processes in serpentinite from sub-micron Raman Spectroscopy and TEM

NASA Astrophysics Data System (ADS)

Smith, S. A. F.; Tarling, M.; Rooney, J. S.; Gordon, K. C.; Viti, C.

2017-12-01

Extensive work has been performed to characterize the mineralogical and mechanical properties of the various serpentine minerals (i.e. antigorite, lizardite, chrysotile, polyhedral and polygonal serpentine). However, correct identification of serpentine minerals is often difficult or impossible using conventional analytical techniques such as optical- and SEM-based microscopy, X-ray diffraction and infrared spectroscopy. Transmission Electron Microscopy (TEM) is the best analytical technique to identify the serpentine minerals, but TEM requires complex sample preparation and typically results in very small analysis areas. Sub-micron confocal Raman spectroscopy mapping of polished thin sections provides a quick and relatively inexpensive way of unambiguously distinguishing the main serpentine minerals within their in-situ microstructural context. The combination of high spatial resolution (with a diffraction-limited system, 366 nm), large-area coverage (up to hundreds of microns in each dimension) and ability to map directly on thin sections allows intricate fault rock textures to be imaged at a sample-scale, which can then form the target of more focused TEM work. The potential of sub-micron Raman Spectroscopy + TEM is illustrated by examining sub-micron-scale mineral intergrowths and deformation textures in scaly serpentinites (e.g. dissolution seams, mineral growth in pressure shadows), serpentinite crack-seal veins and polished fault slip surfaces from a serpentinite-bearing mélange in New Zealand. The microstructural information provided by these techniques has yielded new insights into coseismic dehydration and amorphization processes and the interplay between creep and localised rupture in serpentinite shear zones.

Characterization of hematite nanoparticles synthesized via two different pathways

NASA Astrophysics Data System (ADS)

Das, Soumya; Hendry, M. Jim

2014-08-01

Hematite is one of the most common and thermodynamically stable iron oxides found in both natural and anthropogenic systems. Owing to its ubiquity, stability, moderate specific surface area, and ability to sequester metals and metalloids from aquatic systems, it has been the subject of a large number of adsorption studies published during the past few decades. Although preparation techniques are known to affect the surface morphology of hematite nanoparticles, the effects of aging under environmentally relevant conditions have yet to be tested with respect to surface morphology, surface area, and adsorptive capacity. We prepared hematite via two different pathways and aged it under highly alkaline conditions encountered in many mill tailings settings. Crystal habits and morphologies of the hematite nanoparticles were analyzed via scanning electron microscopy and transmission electron microscopy. X-ray diffraction, Raman spectroscopy, and Brunauer-Emmett-Teller surface area analyses were also conducted on the hematite nanoparticles before and after aging. The hematite synthesized via an Fe(III) salt solution (average particle size 37 nm) was morphologically and structurally different from the hematite synthesized via ferrihydrite aging (average particle size 144 nm). Overall, our data demonstrate that the crystallinity of hematite produced via ferrihydrite transformation is susceptible to morphological alterations/modifications. In contrast, the hematite formed via hydrolysis of an Fe(III) salt solution remains very stable in terms of structure, size, and morphology even under extreme experimental conditions.

Release of titanium after insertion of dental implants with different surface characteristics – an ex vivo animal study

PubMed Central

Pettersson, Mattias; Pettersson, Jean; Molin Thorén, Margareta; Johansson, Anders

2017-01-01

Abstract In the present study, amount of titanium (Ti) released into the surrounding bone during placement of implants with different surface structure was investigated. Quantification of Ti released during insertion from three different implants was performed in this ex vivo study. Jaw bone from pigs was used as model for installation of the implants and Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES) was used for analysis of the released Ti. Implant surface were examined with scanning electron microscopy (SEM), before and after the placement into the bone. Ti was abraded to the surrounding bone upon insertion of a dental implant and the surface roughness of the implant increased the amount of Ti found. Diameter and total area of the implant were of less importance for the Ti released to the bone. No visible damages to the implant surfaces could be identified in SEM after placement. PMID:29242814

Spectromicroscopy measurements of surface morphology and band structure of exfoliated graphene

NASA Astrophysics Data System (ADS)

Knox, Kevin; Locatelli, Andrea; Cvetko, Dean; Mentes, Tevfik; Nino, Miguel; Wang, Shancai; Yilmaz, Mehmet; Kim, Philip; Osgood, Richard; Morgante, Alberto

2011-03-01

Monolayer-thick crystals, such as graphene, are an area of intense interest in condensed matter research. ~However, crystal deformations in these 2D systems are known to adversely affect conductivity and increase local chemical reactivity. Additionally, surface roughness in graphene complicates band-mapping and limits resolution in techniques such as angle resolved photoemission spectroscopy (ARPES), the theory of which was developed for atomically flat surfaces. Thus, an understanding of the surface morphology of graphene is essential to making high quality devices and important for interpreting ARPES results. In this talk, we will describe a non-invasive approach to examining the corrugation in exfoliated graphene using a combination of low energy electron microscopy (LEEM) and micro-spot low energy electron diffraction (LEED). We will also describe how such knowledge of surface roughness can be used in the analysis of ARPES data to improve resolution and extract useful information about the band-structure.

New methods for image collection and analysis in scanning Auger microscopy

NASA Technical Reports Server (NTRS)

Browning, R.

1985-01-01

While scanning Auger micrographs are used extensively for illustrating the stoichiometry of complex surfaces and for indicating areas of interest for fine point Auger spectroscopy, there are many problems in the quantification and analysis of Auger images. These problems include multiple contrast mechanisms and the lack of meaningful relationships with other Auger data. Collection of multielemental Auger images allows some new approaches to image analysis and presentation. Information about the distribution and quantity of elemental combinations at a surface are retrievable, and particular combinations of elements can be imaged, such as alloy phases. Results from the precipitate hardened alloy Al-2124 illustrate multispectral Auger imaging.

Surface photovoltage spectroscopy applied to gallium arsenide surfaces

NASA Technical Reports Server (NTRS)

Bynik, C. E.

1975-01-01

The experimental and theoretical basis for surface photovoltage spectroscopy is outlined. Results of this technique applied to gallium arsenide surfaces, are reviewed and discussed. The results suggest that in gallium arsenide the surface voltage may be due to deep bulk impurity acceptor states that are pinned at the Fermi level at the surface. Establishment of the validity of this model will indicate the direction to proceed to increase the efficiency of gallium arsenide solar cells.

Surface degradation of uranium tetrafluoride

DOE PAGES

Tobin, J. G.; Duffin, A. M.; Yu, S. -W.; ...

2017-05-01

A detailed analysis of a single crystal of uranium tetrafluoride has been carried out. The techniques include x-ray absorption spectroscopy, as well as x-ray photoelectron spectroscopy and x-ray emission spectroscopy. Evidence will be presented for the presence of a uranyl species, possibly UO 2F 2, as a product of, or participant in the surface degradation.

Chemical kinetic studies of atmospheric reactions using tunable diode laser spectroscopy

NASA Technical Reports Server (NTRS)

Worsnop, Douglas R.; Nelson, David D.; Zahniser, Mark S.

1993-01-01

IR absorption using tunable diode laser spectroscopy provides a sensitive and quantitative detection method for laboratory kinetic studies of atmospheric trace gases. Improvements in multipass cell design, real time signal processing, and computer controlled data acquisition and analysis have extended the applicability of the technique. We have developed several optical systems using off-axis resonator mirror designs which maximize path length while minimizing both the sample volume and the interference fringes inherent in conventional 'White' cells. Computerized signal processing using rapid scan (300 kHz), sweep integration with 100 percent duty cycle allows substantial noise reduction while retaining the advantages of using direct absorption for absolute absorbance measurements and simultaneous detection of multiple species. Peak heights and areas are determined by curve fitting using nonlinear least square methods. We have applied these techniques to measurements of: (1) heterogeneous uptake chemistry of atmospheric trace gases (HCl, H2O2, and N2O5) on aqueous and sulfuric acid droplets; (2) vapor pressure measurements of nitric acid and water over prototypical stratospheric aerosol (nitric acid trihydrate) surfaces; and (3) discharge flow tube kinetic studies of the HO2 radical using isotopic labeling for product channel and mechanistic analysis. Results from each of these areas demonstrate the versatility of TDL absorption spectroscopy for atmospheric chemistry applications.

FT-Raman spectroscopic characterization of enamel surfaces irradiated with Nd:YAG and Er:YAG lasers

PubMed Central

Shahabi, Sima; Fekrazad, Reza; Johari, Maryam; Chiniforoush, Nasim; Rezaei, Yashar

2016-01-01

Background. Despite recent advances in dental caries prevention, caries is common and remains a serious health problem. Laser irradiation is one of the most common methods in preventive measures in recent years. Raman spectroscopy technique is utilized to study the microcrystalline structure of dental enamel. In this study, FT-Raman spectroscopy was used to evaluate chemical changes in enamel structure irradiated with Nd:YAG and Er:YAG lasers. Methods. We used 15 freshly-extracted, non-carious, human molars that were treated as follows: No treatment was carried out in group A (control group); Group B was irradiated with Er:YAG laser for 10 seconds under air and water spray; and Group C was irradiated with Nd:YAG laser for 10 seconds under air and water spray. After treatment, the samples were analyzed by FT-Raman spectroscopy. Results. The carbonate content evaluation with regard to the integrated area under the curve (1065/960 cm–1) exhibited a significant reduction in its ratio in groups B and C. The organic content (2935/960 cm-1) area exhibited a significant decrease after laser irradiation in group B and C. Conclusion. The results showed that the mineral and organic matrices of enamel structure were affected by laser irradiation; therefore, it might be a suitable method for caries prevention. PMID:28096945

Quantitative modeling of forces in electromagnetic tweezers

NASA Astrophysics Data System (ADS)

Bijamov, Alex; Shubitidze, Fridon; Oliver, Piercen M.; Vezenov, Dmitri V.

2010-11-01

This paper discusses numerical simulations of the magnetic field produced by an electromagnet for generation of forces on superparamagnetic microspheres used in manipulation of single molecules or cells. Single molecule force spectroscopy based on magnetic tweezers can be used in applications that require parallel readout of biopolymer stretching or biomolecular binding. The magnetic tweezers exert forces on the surface-immobilized macromolecule by pulling a magnetic bead attached to the free end of the molecule in the direction of the field gradient. In a typical force spectroscopy experiment, the pulling forces can range between subpiconewton to tens of piconewtons. In order to effectively provide such forces, an understanding of the source of the magnetic field is required as the first step in the design of force spectroscopy systems. In this study, we use a numerical technique, the method of auxiliary sources, to investigate the influence of electromagnet geometry and material parameters of the magnetic core on the magnetic forces pulling the target beads in the area of interest. The close proximity of the area of interest to the magnet body results in deviations from intuitive relations between magnet size and pulling force, as well as in the force decay with distance. We discuss the benefits and drawbacks of various geometric modifications affecting the magnitude and spatial distribution of forces achievable with an electromagnet.

Diamond /111/ studied by electron energy loss spectroscopy in the characteristic loss region

NASA Technical Reports Server (NTRS)

Pepper, S. V.

1982-01-01

Unoccupied surface states on diamond (111) annealed at greater than 900 C are studied by electron energy loss spectroscopy with valence band excitation. A feature found at 2.1 eV loss energy is attributed to an excitation from occupied surface states into unoccupied surface states of energy within the bulk band gap. A surface band gap of approximately 1 eV is estimated. This result supports a previous suggestion for unoccupied band gap states based on core level energy loss spectroscopy. Using the valence band excitation energy loss spectrosocpy, it is also suggested that hydrogen is removed from the as-polished diamond surface by a Menzel-Gomer-Redhead mechanism.

Improving the Thermodynamic Stability of Aluminate Spinel Nanoparticles with Rare Earths

DOE PAGES

Hasan, M. M.; Dey, Sanchita; Nafsin, Nazia; ...

2016-06-29

Surface energy is a key parameter to understand and predict the stability of catalysts. In this work, the surface energy of MgAl 2O 4, an important base material for catalyst support, was reduced by using dopants prone to form surface excess (surface segregation): Y 3+, Gd 3+, and La 3+. The energy reduction was predicted by atomistic simulations of spinel surfaces and experimentally demonstrated by using microcalorimetry. The surface energy of undoped MgAl 2O 4 was directly measured as 1.65 ± 0.04 J/m 2 and was reduced by adding 2 mol % of the dopants to 1.55 ± 0.04 J/mmore » 2 for Y-doping, 1.45 ± 0.05 J/m 2 for Gd-doping, and 1.26 ± 0.06 J/m 2 for La-doping. Atomistic simulations are qualitatively consistent with the experiments, reinforcing the link between the role of dopants in stabilizing the surface and the energy of segregation. Surface segregation was experimentally assessed using electron energy loss spectroscopy mapping in a scanning transmission electron microscopy image. Finally, the reduced energy resulted in coarsening inhibition for the doped samples and, hence, systematically smaller particle sizes (larger surface areas), meaning increased stability for catalytic applications. Moreover, both experiment and modeling reveal preferential dopant segregation to specific surfaces, which leads to the preponderance of {111} surface planes and suggests a strategy to enhance the area of desired surfaces in nanoparticles for better catalyst support activity.« less

Pinhole mediated electrical transport across LaTiO3/SrTiO3 and LaAlO3/SrTiO3 oxide hetero-structures

NASA Astrophysics Data System (ADS)

Kumar, Pramod; Dogra, Anjana; Toutam, Vijaykumar

2013-11-01

Metal-insulator-metal configuration of LaTiO3/SrTiO3 and LaAlO3/SrTiO3 hetero-structures between two dimensional electron gas formed at the interface and different area top electrodes is employed for Conductive Atomic force microscopy (CAFM) imaging, Current-Voltage (I-V), and Capacitance-Voltage (C-V) spectroscopy. Electrode area dependent I-V characteristics are observed for these oxide hetero-structures. With small area electrodes, rectifying I-V characteristics are observed, compared to, both tunneling and leakage current characteristics for large area electrodes. CAFM mapping confirmed the presence of pinholes on both surfaces. Resultant I-V characteristics have a contribution from both tunneling and leakage due to pinholes.

Biopolymer protected silver nanoparticles on the support of carbon nanotube as interface for electrocatalytic applications

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

Satyanarayana, M.; Kumar, V. Sunil; Gobi, K. Vengatajalabathy, E-mail: drkvgobi@gmail.com, E-mail: satyam.nitw@gmail.com

In this research, silver nanoparticles (SNPs) are prepared on the surface of carbon nanotubes via chitosan, a biopolymer linkage. Here chitosan act as stabilizing agent for nanoparticles and forms a network on the surface of carbon nanotubes. Synthesized silver nanoparticles-MWCNT hybrid composite is characterized by UV-Visible spectroscopy, XRD analysis, and FESEM with EDS to evaluate the structural and chemical properties of the nanocomposite. The electrocatalytic activity of the fabricated SNP-MWCNT hybrid modified glassy carbon electrode has been evaluated by cyclic voltammetry and electrochemical impedance analysis. The silver nanoparticles are of size ∼35 nm and are well distributed on the surface ofmore » carbon nanotubes with chitosan linkage. The prepared nanocomposite shows efficient electrocatalytic properties with high active surface area and excellent electron transfer behaviour.« less

Improved solar-driven photocatalytic performance of Ag{sub 2}CO{sub 3}/(BiO){sub 2}CO{sub 3} prepared in-situ

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

Zhong, Junbo, E-mail: junbozhong@163.com; Li, Jianzhang, E-mail: lschmanuscript@163.com; Huang, Shengtian

Highlights: • Ag{sub 2}CO{sub 3}/(BiO){sub 2}CO{sub 3} photocatalysts were prepared in-situ. • The photo-induced charge separation rate has been greatly increased. • The photocatalytic activity has been greatly promoted. - Abstract: Ag{sub 2}CO{sub 3}/(BiO){sub 2}CO{sub 3} composites have been fabricated in-situ via a facile parallel flaw co-precipitation method. The specific surface area, structure, morphology, and the separation rate of photo-induced charge pairs of the photocatalysts were characterized by Brunauer–Emmett–Teller (BET) method, X-ray diffraction (XRD), UV–vis diffuse reflectance spectroscopy(DRS), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), and surface photovoltage (SPV) spectroscopy, respectively. XRD patterns and DRS demonstrated that Ag{submore » 2}CO{sub 3} has no effect on the crystal phase and bandgap of (BiO){sub 2}CO{sub 3}. The existence of Ag{sub 2}CO{sub 3} in the composites enhances the separation rate of photo-induced charge pairs of the photocatalysts. The photocatalytic performance of Ag{sub 2}CO{sub 3}/(BiO){sub 2}CO{sub 3} was evaluated by the decolorization of methyl orange (MO) aqueous solution under simulated solar irradiation. It was found that the simulated solar-induced photocatalytic activity of Ag{sub 2}CO{sub 3}/(BiO){sub 2}CO{sub 3} copmposites was significantly improved, which was mainly attributed to the enhanced surface area and the separation rate of photo-induced charge pairs.« less

Synthesis and characterization of Co3O4 prepared from atmospheric pressure acid leach liquors of nickel laterite ores

NASA Astrophysics Data System (ADS)

Meng, Long; Guo, Zhan-cheng; Qu, Jing-kui; Qi, Tao; Guo, Qiang; Hou, Gui-hua; Dong, Peng-yu; Xi, Xin-guo

2018-01-01

A chemical precipitation-thermal decomposition method was developed to synthesize Co3O4 nanoparticles using cobalt liquor obtained from the atmospheric pressure acid leaching process of nickel laterite ores. The effects of the precursor reaction temperature, the concentration of Co2+, and the calcination temperature on the specific surface area, morphology, and the electrochemical behavior of the obtained Co3O4 particles were investigated. The precursor basic cobaltous carbonate and cobaltosic oxide products were characterized and analyzed by Fourier transform infrared spectroscopy, thermogravimetric differential thermal analysis, X-ray diffraction, field-emission scanning electron microscopy, specific surface area analysis, and electrochemical analysis. The results indicate that the specific surface area of the Co3O4 particles with a diameter of 30 nm, which were obtained under the optimum conditions of a precursor reaction temperature of 30°C, 0.25 mol/L Co2+, and a calcination temperature of 350°C, was 48.89 m2/g. Electrodes fabricated using Co3O4 nanoparticles exhibited good electrochemical properties, with a specific capacitance of 216.3 F/g at a scan rate of 100 mV/s.

High-Surface-Area Nitrogen-Doped Reduced Graphene Oxide for Electric Double-Layer Capacitors.

PubMed

Youn, Hee-Chang; Bak, Seong-Min; Kim, Myeong-Seong; Jaye, Cherno; Fischer, Daniel A; Lee, Chang-Wook; Yang, Xiao-Qing; Roh, Kwang Chul; Kim, Kwang-Bum

2015-06-08

A two-step method consisting of solid-state microwave irradiation and heat treatment under NH3 gas was used to prepare nitrogen-doped reduced graphene oxide (N-RGO) with a high specific surface area (1007 m(2)  g(-1) ), high electrical conductivity (1532 S m(-1) ), and low oxygen content (1.5 wt %) for electrical double-layer capacitor applications. The specific capacitance of N-RGO was 291 F g(-1) at a current density of 1 A g(-1) , and a capacitance of 261 F g(-1) was retained at 50 A g(-1) , which indicated a very good rate capability. N-RGO also showed excellent cycling stability and preserved 96 % of the initial specific capacitance after 100 000 cycles. Near-edge X-ray absorption fine-structure spectroscopy results provided evidenced for the recovery of π conjugation in the carbon networks with the removal of oxygenated groups and revealed chemical bonding of the nitrogen atoms in N-RGO. The good electrochemical performance of N-RGO is attributed to its high surface area, high electrical conductivity, and low oxygen content. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A novel route for synthesis of nanocrystalline hydroxyapatite from eggshell waste.

PubMed

Siva Rama Krishna, D; Siddharthan, A; Seshadri, S K; Sampath Kumar, T S

2007-09-01

The eggshell waste has been value engineered to a nanocrystalline hydroxyapatite (HA) by microwave processing. To highlight the advantages of eggshell as calcium precursor in the synthesis of HA (OHA), synthetic calcium hydroxide was also used to form HA (SHA) following similar procedure and were compared with a commercially available pure HA (CHA). All the HAs were characterized by X-ray powder diffraction (XRD) method, Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and specific surface area measurements. Nanocrystalline nature of OHA is revealed through characteristic broad peaks in XRD patterns, platelets of length 33-50 nm and width 8-14 nm in TEM micrograph and size calculations from specific surface area measurements. FT-IR spectra showed characteristic bands of HA and additionally peaks of carbonate ions. The cell parameter calculations suggest the formation of carbonated HA of B-type. The OHA exhibits superior sinterability in terms of hardness and density than both SHA and CHA may be due to larger surface area of its spherulite structure. The in vitro dissolution study shows longer stability in phosphate buffer and cell culture test using osteoblast cells establishes biocompatibility of OHA.

SnO2 Nanostructures: Effect of Processing Parameters on Their Structural and Functional Properties

NASA Astrophysics Data System (ADS)

Dontsova, Tetiana A.; Nagirnyak, Svitlana V.; Zhorov, Vladyslav V.; Yasiievych, Yuriy V.

2017-05-01

Zero- and 1D (one-dimensional) tin (IV) oxide nanostructures have been synthesized by thermal evaporation method, and a comparison of their morphology, crystal structure, sorption properties, specific surface area, as well as electrical characteristics has been performed. Synthesized SnO2 nanomaterials were studied by X-ray diffraction, scanning and transmission electron microscopy (SEM and TEM), N2 sorption/desorption technique, IR spectroscopy and, in addition, their current-voltage characteristics have also been measured. The single crystalline structures were obtained both in case of 0D (zero-dimensional) SnO2 powders and in case of 0D nanofibers, as confirmed by electron diffraction of TEM. It was found that SnO2 synthesis parameters significantly affect materials' properties by contributing to the difference in morphology, texture formation, changes in IR spectra of 1D structure as compared to 0D powders, increases in the specific surface area of nanofibers, and the alteration of current-voltage characteristics 0D and 1D SnO2 nanostructures. It was established that gas sensors utilizing of 1D nanofibers significantly outperform those based on 0D powders by providing higher specific surface area and ohmic I-V characteristics.

Topography and surface energy dependent calcium phosphate formation on Sol-Gel derived TiO2 coatings.

PubMed

Järn, Mikael; Areva, Sami; Pore, Viljami; Peltonen, Jouko; Linden, Mika

2006-09-12

Heterogeneous nucleation and growth of calcium phosphate (CaP) on sol-gel derived TiO(2) coatings was investigated in terms of surface topography and surface energy. The topography of the coatings was derived from AFM measurements, while the surface energy was determined with contact angle measurements. The degree of precipitation was examined with scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The precipitation of CaP was found to be dependent on both topography and surface energy. A high roughness value when combining the RMS roughness parameter S(q) with the number of local maxima per unit area parameter S(ds) enhances CaP formation. The hydrophilicity of the coating was also found to be of importance for CaP formation. We suggest that the water contact angle, which is a direct measure of the hydrophilicity of the surface, may be used to evaluate the surface energy dependent precipitation kinetics rather than using the often applied Lewis base parameter.

Study of reticulated vitreous carbon surface treated by plasma immersion ion implantation for electrodes production

NASA Astrophysics Data System (ADS)

Silva, L. L. G.; Conceição, D. A. S.; Oishi, S. S.; Toth, A.; Ueda, M.

2012-03-01

RVC samples were treated by nitrogen plasma immersion ion implantation (N-PIII) for electrodes production. High-voltage pulses with amplitudes of -3.0 kV or -10.0 kV were applied to the RVC samples while the treatment time was 10, 20 and 30 min. The samples were characterized by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and electrochemical measurements. The SEM images present an apparent enhancement of the surface roughness after the treatment probably due to the surface sputtering during the PIII process. This observation is in agreement with the specific electrochemical surface area (SESA) of RVC electrodes. An increase was observed of the SESA values for the PIII-treated samples compared to the untreated specimen. Some oxygen and nitrogen containing groups were introduced on the RVC surface after the PIII treatment. Both plasma-induced process: the surface roughening and the introduction of the polar species on the RVC surface are beneficial for the RVC electrodes application.

Effect of Atmospheric Plasma Treatment to Titanium Surface on Initial Osteoblast-Like Cell Spreading. .

PubMed

Kim, In-Hye; Son, Jun-Sik; Kwon, Tae-Yub; Kim, Kyo-Han

2015-01-01

Plasma treatments are becoming a popular method for modifying the characteristics of a range of substrate surfaces. Atmospheric pressure plasma is cost-efficient, safe and simple compared to high-pressure plasma. This study examined the effects of atmospheric pressure plasma to a titanium (Ti) surface on osteoblast-like cell (osteoblast) spreading and cellular networks. The characteristics of the Ti surface before and after the atmospheric plasma treatment were analyzed by X-ray photoemission spectroscopy (XPS), scanning electron microscopy (SEM), contact angle measurements, and an optical 3D profiling system. The morphology of osteoblasts attached to the Ti surfaces was observed by SEM and confocal laser scanning microscopy. The atmospheric pressure plasma made the Ti surfaces more hydrophilic. The osteoblasts that adhered to the untreated surface were round and spherical, whereas the cells covered a larger surface area on the plasma-treated surface. The plasma-treated Ti surface showed enhanced cell spreading and migration with more developed cellular networks. In conclusion, an atmospheric plasma treatment is a potential surface modifying method that can enhance the initial the cell affinity at the early stages in vitro.

Deuterium trapping in the carbon-silicon co-deposition layers prepared by RF sputtering in D2 atmosphere

NASA Astrophysics Data System (ADS)

Zhang, Hongliang; Zhang, Weiyuan; Su, Ranran; Tu, Hanjun; Shi, Liqun; Hu, Jiansheng

2018-04-01

Deuterated carbon-silicon layers co-deposited on graphite and silicon substrates by radio frequency magnetron sputtering in pure D2 plasma were produced to study deuterium trapping and characteristics of the C-Si layers. The C-Si co-deposited layers were examined by ion beam analysis (IBA), Raman spectroscopy (RS), infrared absorption (IR) spectroscopy, thermal desorption spectroscopy (TDS) and scanning electron microscopy (SEM). It was found that the growth rate of the C-Si co-deposition layer decreased with increasing temperature from 350 K to 800 K, the D concentration and C/Si ratios increased differently on graphite and silicon substrates. TDS shows that D desorption is mainly as D2, HD, HDO, CD4, and C2D4 and release peaks occurred at temperatures of less than 900 K. RS and IR analysis reveal that the structure of the C-Si layers became more disordered with increasing temperatures. Rounded areas of peeling with 1-2 μm diameters were observed on the surface.

Formation of continuous activated carbon fibers for barrier fabrics

NASA Astrophysics Data System (ADS)

Liang, Ying

1997-08-01

Commercial protective suits made of active carbon granules or nonwoven fabrics are heavy, have low moisture vapor transport rate, and are uncomfortable. Inherent problems due to construction of barrier fabrics lead to severe heat stress when worn for even short time in warm environments. One proposed method to eliminate these problems is to facilitate the construction of a fabric made of continuous activated carbon fibers (CACF). This study is directed toward investigating the possibility of developing CAFC from two precursors: aramid and fibrillated PAN fiber. It was shown in this study that Kevlar-29 fibers could be quickly carbonized and activated to CACF with high adsorptivity and relatively low weight loss. CACF with high surface area (>500 msp2/g) and reasonable tenacity (≈1g/denier) were successfully prepared from Kevlar fibers through a three-step process: pretreatment, carbonization, and activation. X-ray diffraction, Fourier Transform Infrared Spectroscopy (FTIR), and thermal analysis were conducted to understand the evolution of physical and chemical properties during pretreatment. The influence of temperature, heating rate, and pyrolysis environment on the thermal behavior was determined by DSC and TGA/DTA and used as an indicator for optimizing the pyrolysis conditions. Surface analysis by nitrogen isotherms indicated that the resultant fibers had micropores and mesopores on the surface of CACF. This was also inferred by studies on the surface morphology through Scanning Electron Microscopy (SEM) and Scanning Tunneling Microscopy (STM). An investigation of the surface chemical structure by X-ray photoelectron spectroscopy (XPS) before and after activation and elemental analysis confirmed that adsorption of Kevlar based CACF mainly arises due to the physisorption instead of chemisorption. A multistep stabilization along with carbonization and activation was used to prepare active carbon fiber from fibrillated PAN fiber. The resultant fiber retained its fibrillar structure and provided a very high surface area, up to 1400 msp2/g, but was brittle. The characterization of the thermal behavior, mechanical properties, and surface structure of the pyrolyzed fiber at each processing step was also carried out by using various techniques, such as DSC and TGA, Instron, and SEM. These studies provide directions for preparation of CACF from novel precursors.

Eco-synthesis of graphene and its use in dihydronicotinamide adenine dinucleotide sensing.

PubMed

Amouzadeh Tabrizi, Mahmoud; Jalilzadeh Azar, Somayeh; Nadali Varkani, Javad

2014-09-01

In this paper, we report a green and eco-friendly approach to synthesize reduced graphene oxide (rGO) via a mild hydrothermal process using malt as a reduced agent. The proposed method is based on the reduction of graphene oxide (GO) in malt solution by making use of the reducing capability of phenolic compounds contained in malt solution. The obtained rGO was characterized by atomic force microscopy (AFM), ultraviolet-visible (UV-vis) absorption spectroscopy, X-ray diffraction spectroscopy (XRD), Raman spectroscopy, Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Electrochemical impedance spectroscopy analysis revealed that the charge transfer resistance of rGO modified glassy carbon (GC) electrode was much lower than that of the GC electrode. The electrochemical behavior of dihydronicotinamide adenine dinucleotide (NADH) on rGO modified GC electrode was investigated by cyclic voltammetry and amperometry. Electrochemical experiments indicated that rGO/GC electrode exhibited excellent electrocatalytic activity toward the NADH, which can be attributed to excellent electrical conductivity and high specific surface area of the rGO composite. The resulting biosensor showed highly sensitive amperometric response to NADH with a low detection limit (0.33μM). Copyright © 2014 Elsevier Inc. All rights reserved.

Field emission study of carbon nanostructures

NASA Astrophysics Data System (ADS)

Zhao, Xin

Recently, carbon nanosheets (CNS), a novel nanostructure, were developed in our laboratory as a field emission source for high emission current. To characterize, understand and improve the field emission properties of CNS, a ultra-high vacuum surface analysis system was customized to conduct relevant experimental research in four distinct areas. The system includes Auger electron spectroscopy (AES), field emission energy spectroscopy (FEES), field emission I-V testing, and thermal desorption spectroscopy (TDS). Firstly, commercial Mo single tips were studied to calibrate the customized system. AES and FEES experiments indicate that a pyramidal nanotip of Ca and O elements formed on the Mo tip surface by field induced surface diffusion. Secondly, field emission I-V testing on CNS indicates that the field emission properties of pristine nanosheets are impacted by adsorbates. For instance, in pristine samples, field emission sources can be built up instantaneously and be characterized by prominent noise levels and significant current variations. However, when CNS are processed via conditioning (run at high current), their emission properties are greatly improved and stabilized. Furthermore, only H2 desorbed from the conditioned CNS, which indicates that only H adsorbates affect emission. Thirdly, the TDS study on nanosheets revealed that the predominant locations of H residing in CNS are sp2 hybridized C on surface and bulk. Fourthly, a fabricating process was developed to coat low work function ZrC on nanosheets for field emission enhancement. The carbide triple-peak in the AES spectra indicated that Zr carbide formed, but oxygen was not completely removed. The Zr(CxOy) coating was dispersed as nanobeads on the CNS surface. Although the work function was reduced, the coated CNS emission properties were not improved due to an increased beta factor. Further analysis suggest that for low emission current (<1 uA), the H adsorbates affect emission by altering the work function. In high emission current (>10 uA), thermal, ionic or electronic transition effects may occur, which differently affect the field emission process.

Using Raman Spectroscopy and Surface-Enhanced Raman Scattering to Identify Colorants in Art: An Experiment for an Upper-Division Chemistry Laboratory

ERIC Educational Resources Information Center

Mayhew, Hannah E.; Frano, Kristen A.; Svoboda, Shelley A.; Wustholz, Kristin L.

2015-01-01

Surface-enhanced Raman scattering (SERS) studies of art represent an attractive way to introduce undergraduate students to concepts in nanoscience, vibrational spectroscopy, and instrumental analysis. Here, we present an undergraduate analytical or physical chemistry laboratory wherein a combination of normal Raman and SERS spectroscopy is used to…

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…

Estimation of reactive surface area using a combined method of laboratory analyses and digital image processing

NASA Astrophysics Data System (ADS)

Ma, Jin; Kong, Xiang-Zhao; Saar, Martin O.

2017-04-01

Fluid-rock interactions play an important role in the engineering processes such as chemical stimulation of enhanced geothermal systems and carbon capture, utilization, and storage. However, these interactions highly depend on the accessible reactive surface area of the minerals that are generally poorly constrained for natural geologic samples. In particular, quantifying surface area of each reacting mineral within whole rock samples is challenging due to the heterogeneous distribution of minerals and pore space. In this study, detailed laboratory analyses were performed on sandstone samples from deep geothermal sites in Lithuania. We measure specific surface area of whole rock samples using a gas adsorption method (so-called B.E.T.) with N2 at a temperature of 77.3K. We also quantify their porosity and pore size distribution by a Helium gas pycnometer and a Hg porosimetry, respectively. Rock compositions are determined by a combination of X-ray fluorescence (XRF) and quantitative scanning electron microscopy (SEM) - Energy-dispersive X-ray spectroscopy (EDS), which are later geometrically mapped on images of two-dimensional SEM- Backscattered electrons (BSE) with a resolution of 1.2 μm and three-dimensional micro-CT with a resolution of 10.3 μm to produce a digital mineral map for further constraining the accessibility of reactive minerals. Moreover, we attempt to link the whole rock porosity, pore size distribution, and B.E.T. specific surface area with the digital mineral maps. We anticipate these necessary analyses to provide in-depth understanding of fluid sample chemistry from later hydrothermal reactive flow-through experiments on whole rock samples at elevated pressure and temperature.

Vertical and horizontal distribution of radionuclides (232Th, 238U and 40K) in sediment from Manjung coastal water area Perak, Malaysia

NASA Astrophysics Data System (ADS)

Abdullah, Anisa; Hamzah, Zaini; Saat, Ahmad; Wood, Ab. Khalik

2016-01-01

Distribution of radionuclides from anthropogenic activities has been widely studied in marine coastal area. Due to rapid population growth and socio-economic development in Manjung area such as coal fired power plant, iron foundries, port development, waste discharged from factories and agriculture runoff may contribute to increase in pollution rate. The radioactive materials from anthropogenic activities could deteriorate the quality of the marine ecosystem and thus lead to possible radiological health risk to the population. Radionuclides (232Th, 238U and 40K) content in surface and profile sediment from Manjung coastal area was determined in this study. Radionuclides in sediment from seven locations were collected using sediment core sampling and measurements were carried out using Energy Dispersive X-ray Fluorescence (EDXRF) spectroscopy. The results show that the concentration of radionuclides in surface sediment and distribution trend of depth vertical profile sediment generally varies depending on locations. Enrichment factors (EF), geo-accumulation index (Igeo) and pollution index (PI) were applied to determine level of pollution of this study area. The radiological risks related to human exposure were evaluated based on external hazard index (Hex).

Lateral overgrowth of diamond film on stripes patterned Ir/HPHT-diamond substrate

NASA Astrophysics Data System (ADS)

Wang, Yan-Feng; Chang, Xiaohui; Liu, Zhangcheng; Liu, Zongchen; Fu, Jiao; Zhao, Dan; Shao, Guoqing; Wang, Juan; Zhang, Shaopeng; Liang, Yan; Zhu, Tianfei; Wang, Wei; Wang, Hong-Xing

2018-05-01

Epitaxial lateral overgrowth (ELO) of diamond films on patterned Ir/(0 0 1)HPHT-diamond substrates have been carried out by microwave plasma CVD system. Ir/(0 0 1)HPHT-diamond substrates are fabricated by photolithographic and magnetron sputtering technique. The morphology of the as grown ELO diamond film is characterized by optical microscopy and scanning electronic microscopy. The quality and stress of the ELO diamond film are investigated by surface etching pit density and micro-Raman spectroscopy. Two ultraviolet photodetectors are fabricated on ELO diamond area and non-ELO diamond area prepared on same substrate, and that one on ELO diamond area indicates better photoelectric properties. All results indicate quality of ELO diamond film is improved.

Stress Analysis of Silicon Carbide Microelectromechanical Systems Using Raman Spectroscopy

DTIC Science & Technology

2003-03-01

conformally coated with SiC[2]...........................4 2.1: Silicon carbide grinding stones or “carborundum” [1...open up contact areas to SiC-2 (mask SiC2_SiC3_VIA). Then, a 1.5 µm- thick SiC “cap” layer (SiC-3) is deposited. Note that the SiC-3 conformally coats ...84 5.2: Surface profile across the teeth of a SiC3 comb drive...........................................85 xi

Surface Functionalization of Diamond Films by Photoreaction of Elemental Sulfur and Their Surface Properties

NASA Astrophysics Data System (ADS)

Nakamura, Takako; Ohana, Tsuguyori

2012-08-01

A useful method for direct sulfurization of diamond film surfaces by photoreaction of elemental sulfur was developed. The introduction of thiol groups onto the diamond films was confirmed by X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, and scanning electron microscopy (SEM) analyses. The sulfur-modified diamond films attached to gold nanoparticles by self-assembly. The degrees of thiol group introduction and gold attachment were found to depend on photoirradiation time by monitoring by XPS. The gold-modified diamond film was observed to act as a surface-enhanced Raman scattering substrate for measurement of picric acid.

Laser-induced reduction of graphene oxide powders by high pulsed ultraviolet laser irradiations

NASA Astrophysics Data System (ADS)

Yang, Chii-Rong; Tseng, Shih-Feng; Chen, Yu-Ting

2018-06-01

This study aims to develop a laser-induced reduction approach for graphene oxide (GO) powders fabricated by using high pulsed ultraviolet laser irradiations. Before and after the laser irradiation with different fluences, the physical and electrical properties of homemade GO powders and reduced graphene oxide (rGO) powders were measured and analyzed using Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), surface area analyzer, and four-point probe instrument. The laser irradiation parameters included the pulse repetition frequency of 100 kHz, the scanning speed of galvanometers of 50 mm/s, the number of laser irradiated cycles of 10, and the laser fluences of ranging from 0.153 mJ/cm2 to 0.525 mJ/cm2. The laser reduction experiments of GO powders demonstrated that the largest relative intensity of the 2D peak and specific surface area were found at the laser fluence of 0.438 mJ/cm2. Moreover, the electrical resistance sharply decreased from 280 MΩ in the initial GO powders to 0.267 MΩ in rGO powders at a laser irradiation fluence of 0.438. The C/O ratio was increased from 0.232 in the initial GO powders to 1.86 in the rGO powders at a laser irradiation fluence of 0.525 mJ/cm2; furthermore, the C/O ratios increased with increasing the laser fluences.

Photocatalytic activity enhancement of anatase-graphene nanocomposite for methylene removal: Degradation and kinetics.

PubMed

Rezaei, Mostafa; Salem, Shiva

2016-10-05

In the present research, the TiO2-graphene nanocomposite was synthesized by an eco-friendly method. The blackberry juice was introduced to graphene oxide (GO) as a reducing agent to produce the graphene nano-sheets. The nanocomposite of anatase-graphene was developed as a photocatalyst for the degradation of methylene blue, owing to the larger specific surface area and synergistic effect of reduced graphene oxide (RGO). The UV spectroscopy measurements showed that the prepared nanocomposite exhibited an excellent photocatalytic activity toward the methylene blue degradation. The rate of electron transfer of redox sheets is much higher than that observed on GO, indicating the applicability of proposed method for the production of anatase-RGO nanocomposite for treatment of water contaminated by cationic dye. The prepared materials were characterized with Fourier transform infrared spectroscopy, X-ray diffraction, Brunauer-Emmett-Teller surface area measurement, scanning electron microscopy and transmission electron microscopy. A facile and rapid route was applied for the uniform deposition of anatase nanoparticles on the sheets. The resulting nanocomposite contained nanoparticles with a mean diameter of 10nm. A mechanism for the photocatalytic activity of nanocomposite was suggested and the degradation reaction obeyed the second-order kinetics. It was concluded that the degradation kinetics is changed due to the reduction of GO in the presence of blackberry juice. Copyright © 2016 Elsevier B.V. All rights reserved.

Relationships between groundwater, surface water, and soil salinity in Polder 32, Southwest Bangladesh

NASA Astrophysics Data System (ADS)

Fry, D. C.; Ayers, J. C.

2014-12-01

In the coastal areas of Southwest Bangladesh polders are surrounded by tidal channels filled with brackish water. In the wet season, farmers create openings in the embankments to irrigate rice paddies. In the dry season, farmers do the same to create saline shrimp ponds. Residents on Polder 32, located within the Ganges-Brahmaputra-Meghna delta system, practice these seasonal farming techniques. Soils in the area are entisols, being sediment recently deposited, and contain mostly silt-sized particles. Brackish water in brine shrimp ponds may deposit salt in the soil, causing soil salinization. However, saline connate groundwater could also be contributing to soil salinization. Groundwater, surface water (fresh water pond, rice paddy and tidal channel water) and soil samples have been analyzed via inductively coupled plasma optical emission spectroscopy, inductively coupled plasma mass spectroscopy and ion chromatography in an attempt to correlate salinity measurements with each other in order to determine major sources of soil salinity. Multiple parameters, including distances of samples from tidal channels, inland streams, shrimp ponds and tube wells were measured to see if spatial correlations exist. Similarly, values from wet and dry seasons were compared to quantify temporal variations. Salt content in many soil samples were found to be high enough to significantly decrease rice yields. Continued soil salinization can decrease these yields even more, leading to farmers not producing enough food to sustain their families.

Degradation and Mineralization of Benzohydroxamic Acid by Synthesized Mesoporous La/TiO2

PubMed Central

Luo, Xianping; Wang, Junyu; Wang, Chunying; Zhu, Sipin; Li, Zhihui; Tang, Xuekun; Wu, Min

2016-01-01

Rare earth element La-doped TiO2 (La/TiO2) was synthesized by the sol-gel method. Benzohydroxamic acid was used as the objective pollutant to investigate the photocatalytic activity of La/TiO2. The physicochemical properties of the prepared materials were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, UV-vis diffuse reflectance spectroscopy, specific surface area and porosity, scanning electron microscopy and transmission electron microscopy. As a result, the doping of La could inhibit the crystal growth of TiO2, increase its specific surface area and expand its response to visible light, thus improving its photocatalytic activity. La/TiO2 with the doping ratio of 0.75% calcined at 500 °C, showing the highest photocatalytic activity to degrade benzohydroxamic acid under the irradiation of 300 W mercury lamp. About 94.1% of benzohydroxamic acid with the original concentration at 30 mg·L−1 was removed after 120 min in a solution of pH 4.4 with an La/TiO2 amount of 0.5 g·L−1. Furthermore, 88.5% of the total organic carbon was eliminated after 120 min irradiation. In addition, after four recycling runs, La/TiO2 still kept high photocatalytic activity on the photodegradation of benzohydroxamic acid. The interfacial charge transfer processes were also hypothesized. PMID:27735877

Investigation of Carrageenan Aerogel Microparticles as a Potential Drug Carrier.

PubMed

Obaidat, Rana M; Alnaief, Mohammad; Mashaqbeh, Hadeia

2018-05-07

Carrageenan is an anionic polysaccharide offering many advantages to be used in drug delivery applications. These include availability, thermo-stability, low toxicity, and encapsulating properties. Combination of these properties with aerogel properties like large surface area and porosity make them an ideal candidate for drug adsorption and delivery applications. Emulsion-gelation technique was used to prepare carrageenan gel microparticles with supercritical CO 2 for drying and loading purposes. Ibuprofen has been selected as a model drug for drug loading inside. The prepared microparticles were characterized using particle size analysis, X-ray diffraction, differential scanning calorimetry, Fourier transform infrared spectroscopy, density measurements, surface area, and porosity measurements. Finally, dissolution was applied to the loaded preparations to test in vitro drug release. Ibuprofen was successfully loaded in the amorphous form inside the prepared microparticles with a significant enhancement in the drug release profile. In conclusion, prepared carrageenan aerogel microparticles showed an excellent potential for use as a drug carrier.

Supercapacitors from Activated Carbon Derived from Granatum.

PubMed

Wang, Qiannan; Yang, Lin; Wang, Zhao; Chen, Kexun; Zhang, Lipeng

2015-12-01

Granatum carbon (GC) as electrode materials for supercapacitors is prepared via the chemical activation with different activating agent such as ZnC2 and KOH with an intention to improve the surface area and their electrochemical performance. The structure and electrochemical properties of GC materials are characterized with N2 adsorption/desorption measurements, scanning electron microscope (SEM), cyclic voltammetry (CV), galvanostatic charge/discharge cycling and electrochemical impedance spectroscopy (EIS). The obtained results show that the specific surface area of the granatum-based activated carbons increased obviously from 573 m2 x g(-1) to 1341 m2 x g(-1) by ZnC2 activation and to 930 m2 x g(-1) by KOH treatment. Furthermore, GCZ also delivers specific capacitance of 195.1 Fx g(-1) at the current density of 0.1 A x g(-1) in 30 wt.% KOH aqueous electrolyte and low capacitance loss of 28.5% when the current density increased by 10 times.

Surface-enhanced Raman scattering biomedical applications of plasmonic colloidal particles.

PubMed

Abalde-Cela, Sara; Aldeanueva-Potel, Paula; Mateo-Mateo, Cintia; Rodríguez-Lorenzo, Laura; Alvarez-Puebla, Ramón A; Liz-Marzán, Luis M

2010-08-06

This review article presents a general view of the recent progress in the fast developing area of surface-enhanced Raman scattering spectroscopy as an analytical tool for the detection and identification of molecular species in very small concentrations, with a particular focus on potential applications in the biomedical area. We start with a brief overview of the relevant concepts related to the choice of plasmonic nanostructures for the design of suitable substrates, their implementation into more complex materials that allow generalization of the method and detection of a wide variety of (bio)molecules and the strategies that can be used for both direct and indirect sensing. In relation to indirect sensing, we devote the final section to a description of SERS-encoded particles, which have found wide application in biomedicine (among other fields), since they are expected to face challenges such as multiplexing and high-throughput screening.

Controlled Patterning of Plasmonic Dimers by Using an Ultrathin Nanoporous Alumina Membrane as a Shadow Mask.

PubMed

Hao, Qi; Huang, Hao; Fan, Xingce; Yin, Yin; Wang, Jiawei; Li, Wan; Qiu, Teng; Ma, Libo; Chu, Paul K; Schmidt, Oliver G

2017-10-18

We report on design and fabrication of patterned plasmonic dimer arrays by using an ultrathin anodic aluminum oxide (AAO) membrane as a shadow mask. This strategy allows for controllable fabrication of plasmonic dimers where the location, size, and orientation of each particle in the dimer pairs can be independently tuned. Particularly, plasmonic dimers with ultrasmall nanogaps down to the sub-10 nm scale as well as a large dimer density up to 1.0 × 10 10 cm -2 are fabricated over a centimeter-sized area. The plasmonic dimers exhibit significant surface-enhanced Raman scattering (SERS) enhancement with a polarization-dependent behavior, which is well interpreted by finite-difference time-domain (FDTD) simulations. Our results reveal a facile approach for controllable fabrication of large-area dimer arrays, which is of fundamental interest for plasmon-based applications in surface-enhanced spectroscopy, biochemical sensing, and optoelectronics.

Preparation and Electrochemical Characterization of Mesoporous Polyaniline-Silica Nanocomposites as an Electrode Material for Pseudocapacitors

PubMed Central

Zu, Lei; Cui, Xiuguo; Jiang, Yanhua; Hu, Zhongkai; Lian, Huiqin; Liu, Yang; Jin, Yushun; Li, Yan; Wang, Xiaodong

2015-01-01

Mesoporous polyaniline-silica nanocomposites with a full interpenetrating structure for pseudocapacitors were synthesized via the vapor phase approach. The morphology and structure of the nanocomposites were deeply investigated by scanning electron microscopy, infrared spectroscopy, X-ray diffraction, thermal gravimetric analysis and nitrogen adsorption-desorption tests. The results present that the mesoporous nanocomposites possess a uniform particle morphology and full interpenetrating structure, leading to a continuous conductive polyaniline network with a large specific surface area. The electrochemical performances of the nanocomposites were tested in a mixed solution of sulfuric acid and potassium iodide. With the merits of a large specific surface area and suitable pore size distribution, the nanocomposite showed a large specific capacitance (1702.68 farad (F)/g) due to its higher utilization of the active material. This amazing value is almost three-times larger than that of bulk polyaniline when the same mass of active material was used. PMID:28788006

Synthesis and characterization of MOF-aminated graphite oxide composites for CO2 capture

NASA Astrophysics Data System (ADS)

Zhao, Yunxia; Ding, Huiling; Zhong, Qin

2013-11-01

A kind of metal-organic frameworks (MOF-5) and aminated graphite oxide (AGO) composites were prepared for CO2 capture to mitigate global warming. MOF-5, MOF-5/GO (composite of MOF-5 and graphite oxide) and MOF-5/AGO samples were characterized by X-ray powder diffraction (XRD), infrared spectroscopy (IR), scanning electron microscope (SEM), nitrogen adsorption as well as thermogravimetric analysis to figure out their chemistry and structure information. Three types of samples with suitable specific surface area and pore diameter were chosen to test CO2 adsorption performance and stability under humidity conditions. The results indicate that high surface area and pore volume, pore similar in size to the size of gas adsorbate, and extra reactive sites modified in the composites contributes to the high CO2 capacity. Besides, the composites involved by GO or AGO show better anti-moisture performance than the parent MOF.

Surface-enhanced Raman scattering biomedical applications of plasmonic colloidal particles

PubMed Central

Abalde-Cela, Sara; Aldeanueva-Potel, Paula; Mateo-Mateo, Cintia; Rodríguez-Lorenzo, Laura; Alvarez-Puebla, Ramón A.; Liz-Marzán, Luis M.

2010-01-01

This review article presents a general view of the recent progress in the fast developing area of surface-enhanced Raman scattering spectroscopy as an analytical tool for the detection and identification of molecular species in very small concentrations, with a particular focus on potential applications in the biomedical area. We start with a brief overview of the relevant concepts related to the choice of plasmonic nanostructures for the design of suitable substrates, their implementation into more complex materials that allow generalization of the method and detection of a wide variety of (bio)molecules and the strategies that can be used for both direct and indirect sensing. In relation to indirect sensing, we devote the final section to a description of SERS-encoded particles, which have found wide application in biomedicine (among other fields), since they are expected to face challenges such as multiplexing and high-throughput screening. PMID:20462878

Macrostructure-dependent photocatalytic property of high-surface-area porous titania films

NASA Astrophysics Data System (ADS)

Kimura, T.

2014-11-01

Porous titania films with different macrostructures were prepared with precise control of condensation degree and density of the oxide frameworks in the presence of spherical aggregates of polystyrene-block-poly(oxyethylene) (PS-b-PEO) diblock copolymer. Following detailed explanation of the formation mechanisms of three (reticular, spherical, and large spherical) macrostructures by the colloidal PS-b-PEO templating, structural variation of the titania frameworks during calcination were investigated by X-ray diffraction and X-ray photoelectron spectroscopy. Then, photocatalytic performance of the macroporous titania films was evaluated through simple degradation experiments of methylene blue under an UV irradiation. Consequently, absolute surface area of the film and crystallinity of the titania frameworks were important for understanding the photocatalytic performance, but the catalytic performance can be improved further by the macrostructural design that controls diffusivity of the targeted molecules inside the film and their accessibility to active sites.

Photocatalytic reduction of CO2 with H2O to CH4 on Cu(I) supported TiO2 nanosheets with defective {001} facets.

PubMed

Zhu, Shuying; Liang, Shijing; Tong, Yuecong; An, Xiaohan; Long, Jinlin; Fu, Xianzhi; Wang, Xuxu

2015-04-21

Highly dispersed Cu2O clusters loaded on TiO2 nanosheets with dominant exposed {001} facets are prepared by a hydrothermal treatment followed by photodeposition. The physicochemical properties of the as-prepared samples are characterized carefully. The deposition position and chemical state of the Cu2O clusters are characterized by X-ray diffraction, transmission electron microscopy, UV-vis diffuse reflectance spectroscopy, EPR spectroscopy, and in situ CO-adsorbed FTIR spectroscopy, respectively. The results show that in situ Cu deposition leads to in situ formation of abundant oxygen vacancies (Vo) on the surface of the TiO2 nanosheets. Interestingly, the co-existence of Vo and Cu2O clusters could promote the photoactivity of CO2 reduction efficiently. The surface Vo play a significant role in the reduction of CO2. Meanwhile, the deposited Cu(I) species serve also as active sites for the formation of CH4, and then protect CH4 from degradation by generated oxidation species. For the photoreduction of CO2 to CH4, it is found that the content level of Cu2O has a significant influence on the activity. Cu-TiO2-1.0 shows the highest photocatalytic activity, which is over 30 times higher than that of the parent TiO2. This great enhancement of photocatalytic activity may be contributed by high CO2 adsorption capacity, high electron mobility, and high concentration of Vo. However, the effect of the surface area of the samples on the activity is negligible. All of this evidence is obtained by CO2-sorption, electrochemistry, in situ FTIR spectroscopy, in situ ERP techniques, etc. The reaction intermediates are detected by in situ FTIR spectroscopy. Finally, a probable mechanism is proposed based on the experimental results. It is hoped that our work could render one of the most effective strategies to achieve advanced properties over photofunctional materials for solar energy conversion of CO2.

Chemical synthesis and supercapacitive properties of lanthanum telluride thin film.

PubMed

Patil, S J; Lokhande, A C; Lee, D-W; Kim, J H; Lokhande, C D

2017-03-15

Lanthanum telluride (La 2 Te 3 ) thin films are synthesized via a successive ionic layer adsorption and reaction (SILAR) method. The crystal structure, surface morphology and surface wettability properties are investigated using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Field emission scanning electron microscopy (FE-SEM) and contact angle goniometer techniques, respectively. The La 2 Te 3 material exhibits a specific surface area of 51m 2 g -1 determined by Brunauer-Emmett-Teller (BET) method. La 2 Te 3 thin film electrode has a hydrophilic surface which consists of interconnected pine leaf-like flaky arrays that affect the performance of the supercapacitor. The supercapacitive performance of La 2 Te 3 film electrode is evaluated in 1M LiClO 4 /PC electrolyte using cyclic voltammetry, galvanostatic charge-discharge, and electrochemical impedance spectroscopy techniques. La 2 Te 3 film electrode exhibits a specific capacitance of 194Fg -1 at a scan rate of 5mVs -1 and stored energy density of 60Whkg -1 with delivering power density of 7.22kWkg -1 . La 2 Te 3 film electrode showed capacitive retention of 82% over 1000cycles at a scan rate of 100mVs -1 . Further, flexible La 2 Te 3 |LiClO 4 -PVA|La 2 Te 3 supercapacitor cell is fabricated. Copyright © 2016 Elsevier Inc. All rights reserved.

Surface Characterization.

ERIC Educational Resources Information Center

Fulghum, J. E.; And Others

1989-01-01

This review is divided into the following analytical methods: ion spectroscopy, electron spectroscopy, scanning tunneling microscopy, atomic force microscopy, optical spectroscopy, desorption techniques, and X-ray techniques. (MVL)

TiO2 nanoparticles versus TiO2-SiO2 nanocomposites: a comparative study of photo catalysis on acid red 88.

PubMed

Balachandran, K; Venckatesh, Rajendran; Sivaraj, Rajeshwari; Rajiv, P

2014-07-15

A novel, simple, less time-consuming and cost-effective wet chemical technique was used to synthesis TiO2 nanoparticles and TiO2-SiO2 nanocomposites using Titanium tetra isopropoxide (TTIP) as a precursor relatively at low temperature in acidic pH. Titania sol was prepared by hydrolysis of TTIP and was mixed with silicic acid and tetrahydrofuran mixture. The reaction was carried out under vigorous stirring for 6h and dried at room temperature. The resulting powders were characterized by UV-Visible spectroscopy, Fourier transform infrared (FT-IR), X-ray diffraction, scanning electron microscope (SEM) and transmission electron microscope (TEM). The grain size of the particles was calculated by X-ray diffraction, surface morphology and chemical composition was determined from scanning electron microscopy-energy dispersive spectroscopy, metal oxide stretching was confirmed from FT-IR spectroscopy, band gap was calculated using UV-Visible spectroscopy. Surface area of the composite as calculated by BET analyzer and it was found to be 65 and 75 m(2)/g for TiO2 and TiO2-SiO2 respectively. The photocatalytic experiments were performed with aqueous solution of acid red 88 with TiO2 and TiO2-SiO2 batch studies for 4h irradiation, direct photolysis of TiO2 and TiO2-SiO2 contributed 94.2% and 96.5% decomposition in solar radiation for the optimized concentration of acid red 88. Copyright © 2014 Elsevier B.V. All rights reserved.

A Mossbauer investigation of iron-rich terrestrial hydrothermal vent systems: lessons for Mars exploration.

PubMed

Wade, M L; Agresti, D G; Wdowiak, T J; Armendarez, L P; Farmer, J D

1999-04-25

Hydrothermal spring systems may well have been present on early Mars and could have served as a habitat for primitive life. The integrated instrument suite of the Athena Rover has, as a component on the robotic arm, a Mossbauer spectrometer. In the context of future Mars exploration we present results of Mossbauer analysis of a suite of samples from an iron-rich thermal spring in the Chocolate Pots area of Yellowstone National Park (YNP) and from Obsidian Pool (YNP) and Manitou Springs, Colorado. We have found that Mossbauer spectroscopy can discriminate among the iron-bearing minerals in our samples. Those near the vent and on the surface are identified as ferrihydrite, an amorphous ferric mineraloid. Subsurface samples, collected from cores, which are likely to have undergone inorganic and/or biologically mediated alteration (diagenesis), exhibit spectral signatures that include nontronite (a smectite clay), hematite (alpha-Fe2O3), small-particle/nanophase goethite (alpha-FeOOH), and siderite (FeCO3). We find for iron minerals that Mossbauer spectroscopy is at least as efficient in identification as X-ray diffraction. This observation is important from an exploration standpoint. As a planetary surface instrument, Mossbauer spectroscopy can yield high-quality spectral data without sample preparation (backscatter mode). We have also used field emission scanning electron microscopy (FESEM), in conjunction with energy-dispersive X ray (EDX) fluorescence spectroscopy, to characterize the microbiological component of surface sinters and the relation between the microbiological and the mineralogical framework. Evidence is presented that the minerals found in these deposits can have multi-billion-year residence times and thus may have survived their possible production in a putative early Martian hot spring up to the present day. Examples include the nanophase property and the Mossbauer signature for siderite, which has been identified in a 2.09-billion-year old hematite-rich chert stromatolite. Our research demonstrates that in situ Mossbauer spectroscopy can help determine whether hydrothermal mineral deposits exist on Mars, which is significant for exobiology because of the issue of whether that world ever had conditions conductive to the origin of life. As a useful tool for selection of samples suitable for transport to Earth, Mossbauer spectroscopy will not only serve geological interests but will also have potential for exopaleontology.

A Mossbauer investigation of iron-rich terrestrial hydrothermal vent systems: lessons for Mars exploration

NASA Technical Reports Server (NTRS)

Wade, M. L.; Agresti, D. G.; Wdowiak, T. J.; Armendarez, L. P.; Farmer, J. D.

1999-01-01

Hydrothermal spring systems may well have been present on early Mars and could have served as a habitat for primitive life. The integrated instrument suite of the Athena Rover has, as a component on the robotic arm, a Mossbauer spectrometer. In the context of future Mars exploration we present results of Mossbauer analysis of a suite of samples from an iron-rich thermal spring in the Chocolate Pots area of Yellowstone National Park (YNP) and from Obsidian Pool (YNP) and Manitou Springs, Colorado. We have found that Mossbauer spectroscopy can discriminate among the iron-bearing minerals in our samples. Those near the vent and on the surface are identified as ferrihydrite, an amorphous ferric mineraloid. Subsurface samples, collected from cores, which are likely to have undergone inorganic and/or biologically mediated alteration (diagenesis), exhibit spectral signatures that include nontronite (a smectite clay), hematite (alpha-Fe2O3), small-particle/nanophase goethite (alpha-FeOOH), and siderite (FeCO3). We find for iron minerals that Mossbauer spectroscopy is at least as efficient in identification as X-ray diffraction. This observation is important from an exploration standpoint. As a planetary surface instrument, Mossbauer spectroscopy can yield high-quality spectral data without sample preparation (backscatter mode). We have also used field emission scanning electron microscopy (FESEM), in conjunction with energy-dispersive X ray (EDX) fluorescence spectroscopy, to characterize the microbiological component of surface sinters and the relation between the microbiological and the mineralogical framework. Evidence is presented that the minerals found in these deposits can have multi-billion-year residence times and thus may have survived their possible production in a putative early Martian hot spring up to the present day. Examples include the nanophase property and the Mossbauer signature for siderite, which has been identified in a 2.09-billion-year old hematite-rich chert stromatolite. Our research demonstrates that in situ Mossbauer spectroscopy can help determine whether hydrothermal mineral deposits exist on Mars, which is significant for exobiology because of the issue of whether that world ever had conditions conductive to the origin of life. As a useful tool for selection of samples suitable for transport to Earth, Mossbauer spectroscopy will not only serve geological interests but will also have potential for exopaleontology.

Preliminary design of laser-induced breakdown spectroscopy for proto-Material Plasma Exposure eXperiment

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

Shaw, G., E-mail: shawgc@ornl.gov; University of Tennessee, Knoxville, Tennessee 37996; Martin, M. Z.

2014-11-15

Laser-induced breakdown spectroscopy (LIBS) is a technique for measuring surface matter composition. LIBS is performed by focusing laser radiation onto a target surface, ablating the surface, forming a plasma, and analyzing the light produced. LIBS surface analysis is a possible diagnostic for characterizing plasma-facing materials in ITER. Oak Ridge National Laboratory has enabled the initial installation of a laser-induced breakdown spectroscopy diagnostic on the prototype Material-Plasma Exposure eXperiment (Proto-MPEX), which strives to mimic the conditions found at the surface of the ITER divertor. This paper will discuss the LIBS implementation on Proto-MPEX, preliminary design of the fiber optic LIBS collectionmore » probe, and the expected results.« less

Spectroscopy and computational studies on the interaction of octyl, dodecyl, and hexadecyl derivatives of anionic and cationic surfactants with adenosine deaminase.

PubMed

Ajloo, Davood; Mahmoodabadi, Najmeh; Ghadamgahi, Maryam; Saboury, Ali Akbar

2016-07-01

Effects of sodium (octyl, dodecyl, hexadecyl) sulfate and their cationic analogous on the structure of adenosine deaminase (ADA) were investigated by fluorescence and circular dichroism spectroscopy as well as molecular dynamics simulation and docking calculation. Root-mean-square derivations, radius of gyration, solvent accessible surface area, and radial distribution function were obtained. The results showed that anionic and cationic surfactants reduce protein stability. Cationic surfactants have more effect on the ADA structure in comparison with anionic surfactants. More concentration and longer surfactants are parallel to higher denaturation. Furthermore, aggregation in the presence of anionic surfactants is more than cationic surfactants. Docking data showed that longer surfactants have more interaction energy and smaller ones bound to the active site.

Internal Reflection Spectra of Surface Compounds and Adsorbed Molecules

NASA Astrophysics Data System (ADS)

Zolotarev, V. M.; Lygin, V. I.; Tarasevich, B. N.

1981-01-01

The application of attenuated total reflection (ATR) spectroscopy in surface studies of inorganic adsorbents and catalysts, polymers, and optically transparent electrodes is discussed. The basic principles of ATR spectroscopy as applied to surface phenomena are considered, with special reference to thin films, industrial adsorbents and catalysts, and polymer degradation processes. 276 references.

Second Harmonic Correlation Spectroscopy: Theory and Principles for Determining Surface Binding Kinetics.

PubMed

Sly, Krystal L; Conboy, John C

2017-06-01

A novel application of second harmonic correlation spectroscopy (SHCS) for the direct determination of molecular adsorption and desorption kinetics to a surface is discussed in detail. The surface-specific nature of second harmonic generation (SHG) provides an efficient means to determine the kinetic rates of adsorption and desorption of molecular species to an interface without interference from bulk diffusion, which is a significant limitation of fluorescence correlation spectroscopy (FCS). The underlying principles of SHCS for the determination of surface binding kinetics are presented, including the role of optical coherence and optical heterodyne mixing. These properties of SHCS are extremely advantageous and lead to an increase in the signal-to-noise (S/N) of the correlation data, increasing the sensitivity of the technique. The influence of experimental parameters, including the uniformity of the TEM00 laser beam, the overall photon flux, and collection time are also discussed, and are shown to significantly affect the S/N of the correlation data. Second harmonic correlation spectroscopy is a powerful, surface-specific, and label-free alternative to other correlation spectroscopic methods for examining surface binding kinetics.

Characterization of Colloidal Quantum Dot Ligand Exchange by X-ray Photoelectron Spectroscopy

NASA Astrophysics Data System (ADS)

Atewologun, Ayomide; Ge, Wangyao; Stiff-Roberts, Adrienne D.

2013-05-01

Colloidal quantum dots (CQDs) are chemically synthesized semiconductor nanoparticles with size-dependent wavelength tunability. Chemical synthesis of CQDs involves the attachment of long organic surface ligands to prevent aggregation; however, these ligands also impede charge transport. Therefore, it is beneficial to exchange longer surface ligands for shorter ones for optoelectronic devices. Typical characterization techniques used to analyze surface ligand exchange include Fourier-transform infrared spectroscopy, x-ray diffraction, transmission electron microscopy, and nuclear magnetic resonance spectroscopy, yet these techniques do not provide a simultaneously direct, quantitative, and sensitive method for evaluating surface ligands on CQDs. In contrast, x-ray photoelectron spectroscopy (XPS) can provide nanoscale sensitivity for quantitative analysis of CQD surface ligand exchange. A unique aspect of this work is that a fingerprint is identified for shorter surface ligands by resolving the regional XPS spectrum corresponding to different types of carbon bonds. In addition, a deposition technique known as resonant infrared matrix-assisted pulsed laser evaporation is used to improve the CQD film uniformity such that stronger XPS signals are obtained, enabling more accurate analysis of the ligand exchange process.

The Sulphur Poisoning Behaviour of Gadolinia Doped Ceria Model Systems in Reducing Atmospheres

PubMed Central

Gerstl, Matthias; Nenning, Andreas; Iskandar, Riza; Rojek-Wöckner, Veronika; Bram, Martin; Hutter, Herbert; Opitz, Alexander Karl

2016-01-01

An array of analytical methods including surface area determination by gas adsorption using the Brunauer, Emmett, Teller (BET) method, combustion analysis, XRD, ToF-SIMS, TEM and impedance spectroscopy has been used to investigate the interaction of gadolinia doped ceria (GDC) with hydrogen sulphide containing reducing atmospheres. It is shown that sulphur is incorporated into the GDC bulk and might lead to phase changes. Additionally, high concentrations of silicon are found on the surface of model composite microelectrodes. Based on these data, a model is proposed to explain the multi-facetted electrochemical degradation behaviour encountered during long term electrochemical measurements. While electrochemical bulk properties of GDC stay largely unaffected, the surface polarisation resistance is dramatically changed, due to silicon segregation and reaction with adsorbed sulphur. PMID:28773771

Copper Antimonide Nanowire Array Lithium Ion Anodes Stabilized by Electrolyte Additives.

PubMed

Jackson, Everett D; Prieto, Amy L

2016-11-09

Nanowires of electrochemically active electrode materials for lithium ion batteries represent a unique system that allows for intensive investigations of surface phenomena. In particular, highly ordered nanowire arrays produced by electrodeposition into anodic aluminum oxide templates can lead to new insights into a material's electrochemical performance by providing a high-surface-area electrode with negligible volume expansion induced pulverization. Here we show that for the Li-Cu x Sb ternary system, stabilizing the surface chemistry is the most critical factor for promoting long electrode life. The resulting solid electrolyte interphase is analyzed using a mix of electron microscopy, X-ray photoelectron spectroscopy, and lithium ion battery half-cell testing to provide a better understanding of the importance of electrolyte composition on this multicomponent alloy anode material.

Ferrocene-decorated nanocrystalline cellulose with charge carrier mobility.

PubMed

Eyley, Samuel; Shariki, Sara; Dale, Sara E C; Bending, Simon; Marken, Frank; Thielemans, Wim

2012-04-24

Ferrocene-decorated cellulose nanowhiskers were prepared by the grafting of ethynylferrocene onto azide functionalized cotton-derived cellulose nanowhiskers using azide-alkyne cycloaddition. Successful surface modification and retention of the crystalline morphology of the nanocrystals was confirmed by elemental analysis, inductively coupled plasma-atomic emission spectroscopy, X-ray photoelectron spectroscopy, and X-ray diffraction. The coverage with ferrocenyl is high (approximately 1.14 × 10(-3) mol g(-1) or 4.6 × 10(13) mol cm(-2) corresponding to a specific area of 61 Å(2) per ferrocene). Cyclic voltammetry measurements of films formed by deposition of ferrocene-decorated nanowhiskers showed that this small spacing of redox centers along the nanowhisker surface allowed conduction hopping of electrons. The apparent diffusion coefficient for electron (or hole) hopping via Fe(III/II) surface sites is estimated as Dapp = 10(-19) m(2)s(-1) via impedance methods, a value significantly less than nonsolvated ferrocene polymers, which would be expected as the 1,2,3-triazole ring forms a rigid linker tethering the ferrocene to the nanowhisker surface. In part, this is believed to be also due to "bottleneck" diffusion of charges across contact points where individual cellulose nanowhiskers contact each other. However, the charge-communication across the nanocrystal surface opens up the potential for use of cellulose nanocrystals as a charge percolation template for the preparation of conducting films via covalent surface modification (with applications similar to those using adsorbed conducting polymers), for use in bioelectrochemical devices to gently transfer and remove electrons without the need for a solution-soluble redox mediator, or for the fabrication of three-dimensional self-assembled conducting networks.

Spinal muscle evaluation in healthy individuals and low-back-pain patients: a literature review.

PubMed

Demoulin, Christophe; Crielaard, Jean-Michel; Vanderthommen, Marc

2007-01-01

This article reviews available techniques for spinal muscle investigation, as well as data on spinal muscles in healthy individuals and in patients with low back pain. In patients with chronic low back pain, medical imaging studies show paraspinal muscle wasting with reductions in cross-sectional surface area and fiber density. In healthy individuals, the paraspinal muscles contain a high proportion of slow-twitch fibers (Type I), reflecting their role in maintaining posture. The proportion of Type I fibers is higher in females, leading to better adaptation to aerobic exertion compared to males. Abnormalities seen in paraspinal muscles from patients with chronic low back pain include marked Type II fiber atrophy, conversion of Type I to Type II fibers, and an increased number of nonspecific abnormalities. Limited data are available from magnetic resonance spectroscopy used to investigate muscle metabolism and from near infrared spectroscopy used to measure oxygen uptake by the paraspinal muscles. Surface electromyography in patients with chronic low back pain shows increased paraspinal muscle fatigability, often with abolition of the flexion-relaxation phenomenon.

Gate-Variable Mid-Infrared Optical Transitions in a (Bi1-xSbx)2Te3 Topological Insulator.

PubMed

Whitney, William S; Brar, Victor W; Ou, Yunbo; Shao, Yinming; Davoyan, Artur R; Basov, D N; He, Ke; Xue, Qi-Kun; Atwater, Harry A

2017-01-11

We report mid-infrared spectroscopy measurements of ultrathin, electrostatically gated (Bi 1-x Sb x ) 2 Te 3 topological insulator films in which we observe several percent modulation of transmittance and reflectance as gating shifts the Fermi level. Infrared transmittance measurements of gated films were enabled by use of an epitaxial lift-off method for large-area transfer of topological insulator films from infrared-absorbing SrTiO 3 growth substrates to thermal oxidized silicon substrates. We combine these optical experiments with transport measurements and angle-resolved photoemission spectroscopy to identify the observed spectral modulation as a gate-driven transfer of spectral weight between both bulk and 2D topological surface channels and interband and intraband channels. We develop a model for the complex permittivity of gated (Bi 1-x Sb x ) 2 Te 3 and find a good match to our experimental data. These results open the path for layered topological insulator materials as a new candidate for tunable, ultrathin infrared optics and highlight the possibility of switching topological optoelectronic phenomena between bulk and spin-polarized surface regimes.

Surface-enhanced Raman spectroscopy on litographically constructed microelectrodes

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

Zhelyaskov, V.R.; Milne, E.T.; Weldon, M.K.

1995-12-31

A novel silicon substrate microelectrode array has been demonstrated to function as a surface-enhanced Raman Spectroscopy (SERS) microelectrode. SERS from adenosine and pyridine down to 10 mM concentration on silver coated iridium and gold microelectrode arrays have been observed with excitation at 532 nm and 633 nm correspondingly. Ag/AgCl reference electrode and platinum or integrated on the microelectrode iridium counter electrodes were used. Owing to the small area of the activated sites on the microelectrode (10 mm x 15 mm) the SERS signal exhibited a strong laser power dependence. The optimal laser power on the activated site was shown tomore » be in the order of x 100 mW. Good quality SERS spectra were recorded with exposure times of 10s and less. The small size of the electrodes makes them promising for studies in confined spaces. This includes potential applications as capillary electrophoreses detectors and probes of chemistry of biological organisms. A work on detection of lipids adhered to self-organized monolayers (SAM)s of alkanethiols on the activated microelectrodes is in progress.« less

Gold-nanofève surface-enhanced Raman spectroscopy visualizes hypotaurine as a robust anti-oxidant consumed in cancer survival.

PubMed

Shiota, Megumi; Naya, Masayuki; Yamamoto, Takehiro; Hishiki, Takako; Tani, Takeharu; Takahashi, Hiroyuki; Kubo, Akiko; Koike, Daisuke; Itoh, Mai; Ohmura, Mitsuyo; Kabe, Yasuaki; Sugiura, Yuki; Hiraoka, Nobuyoshi; Morikawa, Takayuki; Takubo, Keiyo; Suina, Kentaro; Nagashima, Hideaki; Sampetrean, Oltea; Nagano, Osamu; Saya, Hideyuki; Yamazoe, Shogo; Watanabe, Hiroyuki; Suematsu, Makoto

2018-04-19

Gold deposition with diagonal angle towards boehmite-based nanostructure creates random arrays of horse-bean-shaped nanostructures named gold-nanofève (GNF). GNF generates many electromagnetic hotspots as surface-enhanced Raman spectroscopy (SERS) excitation sources, and enables large-area visualization of molecular vibration fingerprints of metabolites in human cancer xenografts in livers of immunodeficient mice with sufficient sensitivity and uniformity. Differential screening of GNF-SERS signals in tumours and those in parenchyma demarcated tumour boundaries in liver tissues. Furthermore, GNF-SERS combined with quantum chemical calculation identified cysteine-derived glutathione and hypotaurine (HT) as tumour-dominant and parenchyma-dominant metabolites, respectively. CD44 knockdown in cancer diminished glutathione, but not HT in tumours. Mechanisms whereby tumours sustained HT under CD44-knockdown conditions include upregulation of PHGDH, PSAT1 and PSPH that drove glycolysis-dependent activation of serine/glycine-cleavage systems to provide one-methyl group for HT synthesis. HT was rapidly converted into taurine in cancer cells, suggesting that HT is a robust anti-oxidant for their survival under glutathione-suppressed conditions.

Surface enhanced Raman spectroscopy (SERS) for in vitro diagnostic testing at the point of care

NASA Astrophysics Data System (ADS)

Marks, Haley; Schechinger, Monika; Garza, Javier; Locke, Andrea; Coté, Gerard

2017-06-01

Point-of-care (POC) device development is a growing field that aims to develop low-cost, rapid, sensitive in-vitro diagnostic testing platforms that are portable, self-contained, and can be used anywhere - from modern clinics to remote and low resource areas. In this review, surface enhanced Raman spectroscopy (SERS) is discussed as a solution to facilitating the translation of bioanalytical sensing to the POC. The potential for SERS to meet the widely accepted "ASSURED" (Affordable, Sensitive, Specific, User-friendly, Rapid, Equipment-free, and Deliverable) criterion provided by the World Health Organization is discussed based on recent advances in SERS in vitro assay development. As SERS provides attractive characteristics for multiplexed sensing at low concentration limits with a high degree of specificity, it holds great promise for enhancing current efforts in rapid diagnostic testing. In outlining the progression of SERS techniques over the past years combined with recent developments in smart nanomaterials, high-throughput microfluidics, and low-cost paper diagnostics, an extensive number of new possibilities show potential for translating SERS biosensors to the POC.

Enhancing the photocatalytic degradation of Fe-Ti over SiO2 nanocomposite material for paraquat removal

NASA Astrophysics Data System (ADS)

Kruanetr, Senee; Wanchanthuek, Ratchaneekorn

2018-05-01

The effect of Fe and Ti loaded over SiO2 (called FeTi/SiO2) in paraquat degradation was studied for both the catalytic activity and the catalyst surface properties. Sufficient characterization techniques were used to obtain the physical and chemical properties of the FeTi/SiO2 system, such as the adsorption-desorption isotherm, surface area and porous structure, XRD diffraction, FTIR spectroscopy, UV–vis diffuse reflection spectrometry and XPS spectroscopy. The catalytic activity in paraquat degradation studies showed that the bimetallic Fe-Ti over SiO2 had higher activity than the monometallic of either Fe or Ti over SiO2 and also the order of the Fe and Ti loading was the significant parameter affecting the activity. The XPS showed that the level of Fe3+ over the catalyst was related to the obtained activity. Moreover, the optimum Fe:Ti ratio in the FeTi/SiO2 system was 1:1 (by weight). Finally, the effect of the support pretreatment (SiO2 pretreatment) was studied and showed a negative effect on the expressed activity.

Effect of alkaline earth metals on the liquid-phase hydrogenation of hydroquinone over Ru-based catalysts

NASA Astrophysics Data System (ADS)

Li, Hongwei; Ji, Dong; Li, Yu; Liang, Yalan; Li, Gui Xian

2015-12-01

A series of Ru-based catalysts modified by alkaline earth metals were prepared by the impregnation-precipitation method and characterized using transmission electron microscopy, X-ray diffraction, ICP optical emission spectroscopy, Infrared Spectroscopy of adsorbed pyridine analysis and surface area analysis. The performance of the catalysts was measured via liquid-phase hydroquinone hydrogenation reaction. Results show that the Ru-Sr/NaY catalyst has the best activity and selectivity among those Ru-based catalysts. The conversion of hydroquinone and the selectivity to 1,4-cyclohexanediol reached up to 99.6% and 89.6% at optimum reaction condition (700 r/min, 423 K and 5 MPa pressure of H2 in 3 h). This may be attributed to the fact that the right amount of Strontium is beneficial to the good dispersion of the ruthenium nanoclusters on the surface of NaY and modify the acidic properties of the catalyst. Moreover, IR of adsorbed pyridine analysis suggested the proper ratio of L/B acid of the catalysts played an important role in the performance of the hydroquinone hydrogenation reaction.

High performance NO2 sensor using MoS2 nanowires network

NASA Astrophysics Data System (ADS)

Kumar, Rahul; Goel, Neeraj; Kumar, Mahesh

2018-01-01

We report on a high-performance NO2 sensor based on a one dimensional MoS2 nanowire (NW) network. The MoS2 NW network was synthesized using chemical transport reaction through controlled turbulent vapor flow. The crystal structure and surface morphology of MoS2 NWs were confirmed by X-ray diffraction, Raman spectroscopy, X-ray photoelectron spectroscopy, and scanning electron microscopy. Further, the sensing behavior of the nanowires was investigated at different temperatures for various concentrations of NO2 and the sensor exhibited about 2-fold enhanced sensitivity with a low detection limit of 4.6 ppb for NO2 at 60 °C compared to sensitivity at room temperature. Moreover, it showed a fast response (16 s) with complete recovery (172 s) at 60 °C, while sensitivity of the device was decreased at 120 °C. The efficient sensing with reliable selectivity toward NO2 of the nanowires is attributed to a combination of abundant active edge sites along with a large surface area and tuning of the potential barrier at the intersections of nanowires during adsorption/desorption of gas molecules.

Fourier Transform Infrared Absorption Spectroscopy of Gas-Phase and Surface Reaction Products during Si Etching in Inductively Coupled Cl2 Plasmas

NASA Astrophysics Data System (ADS)

Miyata, Hiroki; Tsuda, Hirotaka; Fukushima, Daisuke; Takao, Yoshinori; Eriguchi, Koji; Ono, Kouichi

2011-10-01

A better understanding of plasma-surface interactions is indispensable during etching, including the behavior of reaction or etch products, because the products on surfaces and in the plasma are important in passivation layer formation through their redeposition on surfaces. In practice, the nanometer-scale control of plasma etching would still rely largely on such passivation layer formation as well as ion-enhanced etching on feature surfaces. This paper presents in situ Fourier transform infrared (FTIR) absorption spectroscopy of gas-phase and surface reaction products during inductively coupled plasma (ICP) etching of Si in Cl2. The observation was made in the gas phase by transmission absorption spectroscopy (TAS), and also on the substrate surface by reflection absorption spectroscopy (RAS). The quantum chemical calculation was also made of the vibrational frequency of silicon chloride molecules. The deconvolution of the TAS spectrum revealed absorption features of Si2Cl6 and SiClx (x = 1-3) as well as SiCl4, while that of the RAS spectrum revealed relatively increased absorption features of unsaturated silicon chlorides. A different behavior was also observed in bias power dependence between the TAS and RAS spectra.

Hexadecylamine Adsorption at the Iron Oxide–Oil Interface

PubMed Central

2013-01-01

The adsorption behavior of a model additive, hexadecylamine, onto an iron surface from hexadecane oil has been characterized using polarized neutron reflectometry, sum-frequency generation spectroscopy, solution depletion isotherm, and X-ray photoelectron spectroscopy (XPS). The amine showed a strong affinity for the metal surface, forming a dense monolayer at relatively low concentrations; a layer thickness of 16 (±3) Å at low concentrations, increasing to 20 (±3) Å at greater amine concentrations, was determined from the neutron data. These thicknesses suggest that the molecules in the layer are tilted. Adsorption was also indicated by sum-frequency generation spectroscopy and XPS, the latter indicating that the most dominant amine–surface interaction was via electron donation from the nitrogen lone pair to the positively charged iron ions. Sum-frequency generation spectroscopy was used to determine the alkyl chain conformation order and orientation on the surface. PMID:24106786

Visible-light-driven Bi 2 O 3 /WO 3 composites with enhanced photocatalytic activity

DOE PAGES

Adhikari, Shiba P.; Dean, Hunter; Hood, Zachary D.; ...

2015-10-19

Semiconductor heterojunctions (composites) have been shown to be effective photocatalytic materials to overcome the drawbacks of low photocatalytic efficiency that results from electron–hole recombination and narrow photo-response range. We prepared a novel visible-light-driven Bi 2O 3/WO 3 composite photocatalyst by hydrothermal synthesis. The composite was characterized by scanning transmission electron microscopy (STEM), scanning electron microscopy (SEM), powder X-ray diffraction (PXRD), X-ray photoelectron spectroscopy (XPS), Brunauer–Emmett–Teller (BET) surface area, Raman spectroscopy, photoluminescence spectroscopy (PL) and electrochemical impedance spectroscopy (EIS) to better understand the structures, compositions, morphologies and optical properties. Bi 2O 3/WO 3 heterojunction was found to exhibit significantly higher photocatalyticmore » activity towards the decomposition of Rhodamine B (RhB) and 4-nitroaniline (4-NA) under visible light irradiation compared to that of Bi 2O 3 and WO 3. A tentative mechanism for the enhanced photocatalytic activity of the heterostructured composite is discussed based on observed activity, band position calculations, photoluminescence, and electrochemical impedance data. Our study provides a new strategy for the design of composite materials with enhanced visible light photocatalytic performance.« less

TiO2-graphene oxide nanocomposite as advanced photocatalytic materials.

PubMed

Stengl, Václav; Bakardjieva, Snejana; Grygar, Tomáš Matys; Bludská, Jana; Kormunda, Martin

2013-02-27

Graphene oxide composites with photocatalysts may exhibit better properties than pure photocatalysts via improvement of their textural and electronic properties. TiO2-Graphene Oxide (TiO2 - GO) nanocomposite was prepared by thermal hydrolysis of suspension with graphene oxide (GO) nanosheets and titania peroxo-complex. The characterization of graphene oxide nanosheets was provided by using an atomic force microscope and Raman spectroscopy. The prepared nanocomposites samples were characterized by Brunauer-Emmett-Teller surface area and Barrett-Joiner-Halenda porosity, X-ray Diffraction, Infrared Spectroscopy, Raman Spectroscopy and Transmission Electron Microscopy. UV/VIS diffuse reflectance spectroscopy was employed to estimate band-gap energies. From the TiO2 - GO samples, a 300 μm thin layer on a piece of glass 10×15 cm was created. The photocatalytic activity of the prepared layers was assessed from the kinetics of the photocatalytic degradation of butane in the gas phase. The best photocatalytic activity under UV was observed for sample denoted TiGO_100 (k = 0.03012 h-1), while sample labeled TiGO_075 (k = 0.00774 h-1) demonstrated the best activity under visible light.

TiO2-graphene oxide nanocomposite as advanced photocatalytic materials

PubMed Central

2013-01-01

Background Graphene oxide composites with photocatalysts may exhibit better properties than pure photocatalysts via improvement of their textural and electronic properties. Results TiO2-Graphene Oxide (TiO2 - GO) nanocomposite was prepared by thermal hydrolysis of suspension with graphene oxide (GO) nanosheets and titania peroxo-complex. The characterization of graphene oxide nanosheets was provided by using an atomic force microscope and Raman spectroscopy. The prepared nanocomposites samples were characterized by Brunauer–Emmett–Teller surface area and Barrett–Joiner–Halenda porosity, X-ray Diffraction, Infrared Spectroscopy, Raman Spectroscopy and Transmission Electron Microscopy. UV/VIS diffuse reflectance spectroscopy was employed to estimate band-gap energies. From the TiO2 - GO samples, a 300 μm thin layer on a piece of glass 10×15 cm was created. The photocatalytic activity of the prepared layers was assessed from the kinetics of the photocatalytic degradation of butane in the gas phase. Conclusions The best photocatalytic activity under UV was observed for sample denoted TiGO_100 (k = 0.03012 h-1), while sample labeled TiGO_075 (k = 0.00774 h-1) demonstrated the best activity under visible light. PMID:23445868

Functionalized MIL-101 with imidazolium-based ionic liquids for the cycloaddition of CO2 and epoxides under mild condition

NASA Astrophysics Data System (ADS)

Liu, Dan; Li, Gang; Liu, Haiou

2018-01-01

A kind of multi-functional sites metal-organic framework (MOF) composite (MIL-101-IMBr) was successfully prepared by post-synthesis modification of MIL-101 with imidazolium-based ionic liquids. The ionic liquids not only functionalize as basic sites but also provide halide anions, which serve as a nucleophile in cycloaddition reaction. The prepared functional MOF materials were characterized by X-ray diffraction, fourier transform infrared spectroscopy, scanning electron microscopy, energy dispersive spectroscopy, N2 adsorption-desorption and CO2 temperature programmed desorption. The results of fourier transform infrared spectroscopy and energy dispersive spectroscopy show that the MIL-101-IMBr composite was successfully synthesized. The N2 adsorption-desorption results clearly demonstrated that the modified composites still preserve high BET surface area and total pore volume. The composite exhibits high catalytic activity for the cycloaddition of CO2 with epoxides under mild and co-catalyst free conditions. The conversion of propylene oxide was 95.8% and the selectivity of cyclic carbonate was 97.6% under 0.8 MPa at 80 °C for 4 h. Moreover, the catalyst can be used for at least five times.

An Assessment of macro-scale in situ Raman and ultraviolet-induced fluorescence spectroscopy for rapid characterization of frozen peat and ground ice

NASA Astrophysics Data System (ADS)

Laing, Janelle R.; Robichaud, Hailey C.; Cloutis, Edward A.

2016-04-01

The search for life on other planets is an active area of research. Many of the likeliest planetary bodies, such as Europa, Enceladus, and Mars are characterized by cold surface environments and ice-rich terrains. Both Raman and ultraviolet-induced fluorescence (UIF) spectroscopies have been proposed as promising tools for the detection of various kinds of bioindicators in these environments. We examined whether macro-scale Raman and UIF spectroscopy could be applied to the analysis of unprocessed terrestrial frozen peat and clear ground ice samples for detection of bioindicators. It was found that this approach did not provide unambiguous detection of bioindicators, likely for a number of reasons, particularly due to strong broadband induced fluorescence. Other contributing factors may include degradation of organic matter in frozen peat to the point that compound-specific emitted fluorescence or Raman peaks were not resolvable. Our study does not downgrade the utility of either UIF or Raman spectroscopy for astrobiological investigations (which has been demonstrated in previous studies), but does suggest that the choice of instrumentation, operational conditions and sample preparation are important factors in ensuring the success of these techniques.

Optical emission generated by collisions of 5 eV O(3P) atoms with surface-absorbed hydrazine

NASA Technical Reports Server (NTRS)

Orient, O. J.; Martus, K. E.; Chutjian, A.; Murad, E.

1992-01-01

Optical emission has been observed corresponding to vibrational bands in the NH (A 3Pi - X 3Sigma(-)) electronic transition during collisions of 5 eV, ground-state oxygen O(3P) atoms with MgF2 and Ni surfaces continuously exposed to a beam of hydrazine (N2H4). The NH emission intensity is observed to be about five times greater for MgF2 than for Ni. No dependence on temperature was observed for either surface in the range 240 - 340 K, implying that the NH-producing intermediate species is tightly bound. The half-lifetime for desorption of hydrazine from each surface was measured. This was found to be 120 min for the MgF2 surface at 240 K, and less than 20 min for Ni. After exposure, the surface composition was measured using X-ray photoelectron spectroscopy on the exposed and unexposed areas of both targets.

Surface plasmon microscopy with low-cost metallic nanostructures for biosensing I

NASA Astrophysics Data System (ADS)

Lindquist, Nathan; Oh, Sang-Hyun; Otto, Lauren

2012-02-01

The field of plasmonics aims to manipulate light over dimensions smaller than the optical wavelength by exploiting surface plasmon resonances in metallic films. Typically, surface plasmons are excited by illuminating metallic nanostructures. For meaningful research in this exciting area, the fabrication of high-quality nanostructures is critical, and in an undergraduate setting, low-cost methods are desirable. Careful optical characterization of the metallic nanostructures is also required. Here, we present the use of novel, inexpensive nanofabrication techniques and the development of a customized surface plasmon microscopy setup for interdisciplinary undergraduate experiments in biosensing, surface-enhanced Raman spectroscopy, and surface plasmon imaging. A Bethel undergraduate student performs the nanofabrication in collaboration with the University of Minnesota. The rewards of mentoring undergraduate students in cooperation with a large research university are numerous, exposing them to a wide variety of opportunities. This research also interacts with upper-level, open-ended laboratory projects, summer research, a semester-long senior research experience, and will enable a large range of experiments into the future.

Cu(In,Ga)Se2 surface treatment with Na and NaF: A combined photoelectron spectroscopy and surface photovoltage study in ultra-high vacuum

NASA Astrophysics Data System (ADS)

Parvan, V.; Mizrak, A.; Majumdar, I.; Ümsür, B.; Calvet, W.; Greiner, D.; Kaufmann, C. A.; Dittrich, T.; Avancini, E.; Lauermann, I.

2018-06-01

Either metallic Na or NaF were deposited onto Cu(In,Ga)Se2 surfaces and studied by photoelectron spectroscopy and surface photovoltage spectroscopy without breaking the ultra-high vacuum. The deposition of elemental Na at room temperature led to the formation of an intermediate Cu and Ga rich layer at the CIGSe surface, whereas for NaF the composition of the CIGSe surface remained unchanged. A metal like surface induced by an inverted near surface region with a reduced number of defect states was formed after the deposition of Na. Under the chosen experimental conditions, the near surface layer was independent on the amount of Na and stable in time. In contrast, the usage of NaF weakened the inversion and led to an increased band bending compared to the untreated CIGSe sample. The SPV signals decreased with proceeding time after the deposition of NaF.

Electrochemical and Structural Study of a Chemically Dealloyed PtCu Oxygen Reduction Catalyst

PubMed Central

Dutta, Indrajit; Carpenter, Michael K; Balogh, Michael P; Ziegelbauer, Joseph M; Moylan, Thomas E; Atwan, Mohammed H; Irish, Nicholas P

2013-01-01

A carbon-supported, dealloyed platinum-copper (Pt-Cu) oxygen reduction catalyst was prepared using a multi-step synthetic procedure. Material produced at each step was characterized using high angle annular dark field scanning transmission electron microscopy (HAADF-STEM), electron energy loss spectroscopy (EELS) mapping, x-ray absorption spectroscopy (XAS), x-ray diffraction (XRD), and cyclic voltammetry (CV), and its oxygen reduction reaction (ORR) activity was measured by a thin-film rotating disk electrode (TF-RDE) technique. The initial synthetic step, a co-reduction of metal salts, produced a range of poorly crystalline Pt, Cu, and Pt-Cu alloy nanoparticles that nevertheless exhibited good ORR activity. Annealing this material alloyed the metals and increased particle size and crystallinity. TEM shows the annealed catalyst to include particles of various sizes, large (>25 nm), medium (12–25 nm), and small (<12 nm). Most of the small and medium-sized particles exhibited a partial or complete coreshell (Cu-rich core and Pt shell) structure with the smaller particles typically having more complete shells. The appearance of Pt shells after annealing indicates that they are formed by a thermal diffusion mechanism. Although the specific activity of the catalyst material was more than doubled by annealing, the concomitant decrease in Pt surface area resulted in a drop in its mass activity. Subsequent dealloying of the catalyst by acid treatment to partially remove the copper increased the Pt surface area by changing the morphology of the large and some medium particles to a “Swiss cheese” type structure having many voids. The smaller particles retained their core-shell structure. The specific activity of the catalyst material was little reduced by dealloying, but its mass activity was more than doubled due to the increase in surface area. The possible origins of these results are discussed in this report. PMID:23807900

Infrared fiber optic evanescent wave spectroscopy: applications in biology and medicine

NASA Astrophysics Data System (ADS)

Afanasyeva, Natalia I.; Bruch, Reinhard F.; Katzir, Abraham

1999-04-01

A new powerful and highly sensitive technique for non-invasive biomedical diagnostics in vivo has been developed using Infrared Fiberoptic Evanescent Wave Fourier Transform Spectroscopy (FEW-FTIR). This compact and portable method allows to detect functional chemical groups and bonds via vibrational spectroscopy directly from surfaces including living tissue. Such differences and similarities in molecular structure of tissue and materials can be evaluated online. Operating in the attenuated total reflection (ATR) regime in the middle-infrared (MIR) range, the FEW-FTIR technique provides direct contact between the fiber probe and tissue for non-destructive, non-invasive, fast and remote (few meters) diagnostics and quality control of materials. This method utilizes highly flexible and extremely low loss unclad fibers, for example silver halide fibers. Applications of this method include investigations of normal skin, precancerous and cancerous conditions, monitoring of the process of aging, allergic reactions and radiation damage to the skin. This setup is suitable as well for the detection of the influence of environmental factors (sun, water, pollution, and weather) on skin surfaces. The FEW-FTIR technique is very promising also for fast histological examinations in vitro. In this review, we present recent investigations of skin, breast, lung, stomach, kidney tissues in vivo and ex vivo (during surgery) to define the areas of tumor localization. The main advantages of the FEW-FTIR technique for biomedical, clinical, and environmental applications are discussed.

Enhanced sunlight-driven photocatalytic performance of Bi-doped CdMoO4 benefited from efficient separation of photogenerated charge pairs

NASA Astrophysics Data System (ADS)

Huang, Jiao; Liu, Huanhuan; Zhong, Junbo; Yang, Qi; Chen, Jiufu; Li, Jianzhang; Ma, Dongmei; duan, Ran

2018-06-01

In this paper, to further boost the photocatalytic performance of CdMoO4, Bi3+ was successfully doped into CdMoO4 by a facile microwave hydrothermal method. The Bi-doped CdMoO4 photocatalysts prepared were characterized by Brunauer-Emmett-Teller (BET) method, X-ray diffraction (XRD), UV-Vis diffuse reflectance spectroscopy (DRS), scanning electron microscopy (SEM), energy dispersive spectrometer (EDS), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), electron spin-resonance (ESR) and surface photovoltage spectroscopy (SPS). The results exhibit that doping Bi3+ into CdMoO4 remarkably boosts the separation rate of photoinduced charge pairs and the specific surface area, decrease the crystal size, narrows the band gap of the CdMoO4 and induces the binding energy shift of Cd, all these advantageous factors result in the promoted photocatalytic performance of CdMoO4. Using rhodamine B (RhB) as model toxic pollutant, the photocatalytic activities of the photocatalysts were evaluated under a 500 W Xe lamp irradiation. When the molar ratio of Bi/Cd is 0.2%, Bi-CdMoO4 prepared displays the best photocatalytic performance, the photocatalytic performance of the 0.2% sample is more than twice of that of the reference CdMoO4.

Synthesis and characterization of manganese diselenide nanoparticles (MnSeNPs): Determination of capsaicin by using MnSeNP-modified glassy carbon electrode.

PubMed

Sukanya, Ramaraj; Sakthivel, Mani; Chen, Shen-Ming; Chen, Tse-Wei; Al-Hemaid, Fahad M A; Ajmal Ali, M; Elshikh, Mohamed Soliman

2018-06-02

A new type of manganese diselenide nanoparticles (MnSeNPs) was synthesized by using a hydrothermal method. Their surface morphology, crystallinity and elemental distribution were characterized by using transmission electron microscopy, X-ray diffraction, energy dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy which scrutinize the formation of the NPs. The NPs were coated on a glassy carbon electrode (GCE), and electrochemical impedance spectroscopy, cyclic voltammetry and differential pulse voltammetry were applied to study the electroanalytical properties towards the oxidation of the food additive capsaicin. The modified GCE displays lower charge transfer resistance (R ct  = 29.52 Ω), a larger active surface area (0.089 cm 2 /g, and more efficient electrochemical oxidation of capsaicin compared to a MnS 2 /GCE and a bare GCE. The oxidation peak potential is 0.43 V (vs. Ag/AgCl) which is lower than that of previously reported GCEs. The sensor has a detection limit as low as 0.05 μM and an electrochemical sensitivity of 2.41 μA μM -1  cm -2 . The method was applied to the determination of capsaicin in pepper samples. Graphical abstract Electrochemical determination of capsaicin in pepper extract by using MnSeNPs modified electrode.

Reflectance spectroscopy in planetary science: Review and strategy for the future

NASA Technical Reports Server (NTRS)

Mccord, Thomas B. (Editor)

1987-01-01

Reflectance spectroscopy is a remote sensing technique used to study the surfaces and atmospheres of solar system bodies. It provides first-order information on the presence and amounts of certain ions, molecules, and minerals on a surface or in an atmosphere. Reflectance spectroscopy has become one of the most important investigations conducted on most current and planned NASA Solar System Exploration Program space missions. This book reviews the field of reflectance spectroscopy, including information on the scientific technique, contributions, present conditions, and future directions and needs.

Design and fabrication of an electrochemical aptasensor using Au nanoparticles/carbon nanoparticles/cellulose nanofibers nanocomposite for rapid and sensitive detection of Staphylococcus aureus.

PubMed

Ranjbar, Saba; Shahrokhian, Saeed

2018-04-27

Since that pathogenic bacteria are major threats to human health, this paper describes the fabrication of an effective and durable sensing platform based on gold nanoparticles/carbon nanoparticles/cellulose nanofibers nanocomposite (AuNPs/CNPs/CNFs) at the surface of glassy carbon electrode for sensitive and selective detection of Staphylococcus aureus (S. aureus). The AuNPs/CNPs/CNFs nanocomposite with the high surface area, excellent conductivity, and good biocompatibility was used for self-assembled of the thiolated specific S. aureus aptamer as a sensing element. The surface morphology of AuNPs/CNPs/CNFs nanocomposite was characterized with field emission scanning electron microscopy (FESEM), energy dispersive spectroscopy (EDS), dynamic light scattering (DLS) and ultraviolet-visible (UV-Vis) spectrophotometric methods. Each aptasensor modification step was monitored with cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) techniques. The fabricated aptasensor exhibited a wide linear dynamic range (1.2 × 10 1 to 1.2 × 10 8 ) CFU mL -1 with a LOD of 1 CFU mL -1 and was be capable to accurate detection and determination of Staphylococcus aureus in human blood serum as a clinical sample with a complex matrix. Copyright © 2018 Elsevier B.V. All rights reserved.

Photocatalytic performance of Ag doped SnO2 nanoparticles modified with curcumin

NASA Astrophysics Data System (ADS)

Vignesh, K.; Hariharan, R.; Rajarajan, M.; Suganthi, A.

2013-07-01

Visible light active Ag doped SnO2 nanoparticles modified with curcumin (Cur-Ag-SnO2) have been prepared by a combined precipitation and chemical impregnation route. The optical properties, phase structures and morphologies of the as-prepared nanoparticles were characterized using UV-visible diffuse reflectance spectra (UV-vis-DRS), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS). The surface area was measured by Brunauer. Emmett. Teller (B.E.T) analysis. Compared to bare SnO2, the surface modified photocatalysts (Ag-SnO2 and Cur-Ag-SnO2) showed a red shift in the visible region. The photocatalytic activity was monitored via the degradation of rose bengal (RB) dye and the results revealed that Cur-Ag-SnO2 shows better photocatalytic activity than that of Ag-SnO2 and SnO2. The superior photocatalytic activity of Cur-Ag-SnO2 could be attributed to the effective electron-hole separation by surface modification. The effect of photocatalyst concentration, initial dye concentration and electron scavenger on the photocatalytic activity was examined in detail. Furthermore, the antifungal activity of the photocatalysts and the reusability of Cur-Ag-SnO2 were tested.

A novel surface modification approach for protein and cell microarrays

NASA Astrophysics Data System (ADS)

Kurkuri, Mahaveer D.; Driever, Chantelle; Thissen, Helmut W.; Voelcker, Nicholas H.

2007-01-01

Tissue engineering and stem cell technologies have led to a rapidly increasing interest in the control of the behavior of mammalian cells growing on tissue culture substrates. Multifunctional polymer coatings can assist research in this area in many ways, for example, by providing low non-specific protein adsorption properties and reactive functional groups at the surface. The latter can be used for immobilization of specific biological factors that influence cell behavior. In this study, glass slides were coated with copolymers of glycidyl methacrylate (GMA) and poly(ethylene glycol) methacrylate (PEGMA). The coatings were prepared by three different methods based on dip and spin coating as well as polymer grafting procedures. Coatings were characterized by X-ray photoelectron spectroscopy, surface sensitive infrared spectroscopy, ellipsometry and contact angle measurements. A fluorescently labelled protein was deposited onto reactive coatings using a contact microarrayer. Printing of a model protein (fluorescein labeled bovine serum albumin) was performed at different protein concentrations, pH, temperature, humidity and using different micropins. The arraying of proteins was studied with a microarray scanner. Arrays printed at a protein concentration above 50 μg/mL prepared in pH 5 phosphate buffer at 10°C and 65% relative humidity gave the most favourable results in terms of the homogeneity of the printed spots and the fluorescence intensity.

OH radical production in an atmospheric pressure surface micro-discharge array

NASA Astrophysics Data System (ADS)

Li, D.; Nikiforov, A.; Britun, N.; Snyders, R.; Kong, M. G.; Leys, C.

2016-11-01

The generation of OH radicals from an array of surface micro-discharges working in atmospheric pressure He/Ar/H2O mixtures is investigated. The absolute OH density and its temporal-and-spatial dynamics are detected by UV broadband absorption spectroscopy (UV-BAS) and laser-induced fluorescence (LIF) spectroscopy. The measured absolute density of OH(X) state is about 1021 m-3 in Ar/H2O mixture reaching a peak at 0.05% of H2O. In the case of He/H2O mixtures however, the peaking at ~1019 m-3 is approximately two orders of magnitude lower and decreases monotonously with increasing H2O content. From a control standpoint, the ratio of the Ar/He mixture may be adjusted to tune the OH density over two orders of magnitude and to modulate the H2O content dependence of the OH density. The capability of modulating the OH radical production over a large density range is of practical interest for many applications such as atmospheric chemistry and biochemistry. With the array of atmospheric micro-discharges sustained over a large electrode area, a uniform distribution of its OH density can be achieved in a plane parallel to the electrodes thus enabling spatially controlled surface treatment of large samples.

Self-assembly and enhanced photocatalytic properties of BiOI hollow microspheres via a reactable ionic liquid.

PubMed

Xia, Jiexiang; Yin, Sheng; Li, Huaming; Xu, Hui; Yan, Yongsheng; Zhang, Qi

2011-02-01

BiOI uniform flowerlike hollow microspheres with a hole in its surface structures have been successfully synthesized through an EG-assisted solvothermal process in the presence of ionic liquid 1-butyl-3-methylimidazolium iodine ([Bmim]I). The as-prepared samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDS), nitrogen sorption, and diffuse reflectance spectroscopy (DRS). A possible formation mechanism for the growth of hollow microspheres was discussed. During the reactive process, ionic liquid not only acted as solvents and templates but also as an I source for the fabrication of BiOI hollow microspheres and was vital for the structure of hollow microspheres. Additionally, we evaluated the photocatalytic activities of BiOI on the degradation of methyl orange (MO) under visible light irradiation and found that as-prepared BiOI hollow microspheres exhibited higher photocatalytic activity than BiOI nanoplates and TiO(2) (Degussa, P25) did. On the basis of such analysis, it can be assumed that the enhanced photocatalytic activities of BiOI hollow microspheres could be ascribed to its energy band structure, high BET surface area, high surface-to-volume ratios, and light absorbance.

Corrosion evaluation of heat recovery steam generator superheater tube in two methods of testing: Tafel polarization and electrochemical impedance spectroscopy (EIS)

NASA Astrophysics Data System (ADS)

Santoso, Rio Pudjidarma; Riastuti, Rini

2018-05-01

The purpose of this research is to evaluate the corrosion process which occurs on the water side of Heat Recovery Steam Generator (HRSG) superheater tube. The tube was 13CrMo44 and divided into 3 types of specimen: new tube, used tube (with oxide layer on surface), cleaned-used tube (without oxide layer on surface). The evaluation of corrosion parameters wasperformed using deaerated ultra-high purity water (boiler feed water) in two methods of testing: Tafel polarization and Electrochemical Impedance Spectroscopy (EIS). Tafel polarization was excellent as its capability to show the value of corrosion current and the corrosion rate explicitly, on the other hand, EIS was excellent as its capability to explain for corrosion mechanism on metal interface in detail. Both methods showed that the increase of electrolyte temperature from 25°C to 55°C would increase the corrosion rate with the mechanism of decreasing polarization resistance due to thinning out the passive film thickness and enlarge the area of reduction reaction of cathode. Magnetite oxide scale which is laid on the surface of used tube specimen shows protective nature to reduce the corrosion rate, and clear up this oxide would increase the corrosion rate back as new tube.

Plasmonic behaviour of phenylenediamine functionalised silver nanoparticles

NASA Astrophysics Data System (ADS)

Akmal Che Lah, Nurul; Samykano, Mahendran; Rafie Johan, Mohd; Syahierah Othman, Nuurul; Mawardi Saari, Mohd; Bey Fen, Leo; Zalikha Khalil, Nur

2017-09-01

The surface functionalisation of AgNPs has demonstrated improved capability for various applications by modifying their surface chemical conditions. In this study, AgNPs functionalised with p-phenylenediamine (PPD) ligand were prepared, and the plasmonic effects of the nanocomposites were then investigated. The synthesis and functionalisation of Ag nanocomposites were achieved through chemical modification reaction of naphthalene group through hydrothermal synthesis. The influence of the chemical modification reaction on the plasmonic behaviour and size variation were obtained via optical measurement techniques such as UV-visible spectroscopy (UV-Vis) for absorbance characteristic, photoluminescence for emission response and micro-Raman spectroscopy (MRS) for SERS study on the presence of regions containing AgNPs and PPD ligand. It was observed that the one-step process of deprotonation of the amino group on the aromatic rings gives the re-arrangement of the electron cloud towards the π-conjugated system. High-resolution transmission electron microscope (TEM) analysis showed the formation of the nanocomposites and the AgNPs (for ~4 and ~5 nm of diameter sizes) are well-dispersed over the PPD matrix. The nanocomposites are assembled into higher dimensional structures through coordination with functional PPD ligand and also increasing the PPD amount led to the increase in the surface area of the nanoparticles.

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.

Stable Weyl points, trivial surface states, and particle-hole compensation in WP2

NASA Astrophysics Data System (ADS)

Razzoli, E.; Zwartsenberg, B.; Michiardi, M.; Boschini, F.; Day, R. P.; Elfimov, I. S.; Denlinger, J. D.; Süss, V.; Felser, C.; Damascelli, A.

2018-05-01

A possible connection between extremely large magnetoresistance and the presence of Weyl points has garnered much attention in the study of topological semimetals. Exploration of these concepts in transition-metal diphosphides WP2 has been complicated by conflicting experimental reports. Here we combine angle-resolved photoemission spectroscopy (ARPES) and density functional theory (DFT) calculations to disentangle surface and bulk contributions to the ARPES intensity, the superposition of which has plagued the determination of the band structure in WP2. Our results show that while the hole- and electronlike Fermi surface sheets originating from surface states have different areas, the bulk-band structure of WP2 is electron-hole compensated in agreement with DFT. Furthermore, the ARPES band structure is compatible with the presence of at least four temperature-independent Weyl points, confirming the topological nature of WP2 and its stability against lattice distortions.

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

Zhang, Li; Wu, Zili; Nelson, Nicholas

Catalytic performance and the nature of surface adsorbates were investigated for high-surface-area ceria during ethylbenzene oxidative dehydrogenation (ODH) reaction using CO2 as a soft oxidant. A template assisted method was used to synthesize the high-surface-area ceria. The interactions between ethylbenzene, styrene and CO2 on the surface of ceria and the role of CO2 for the ethylbenzene ODH reaction have been investigated in detail by using activity test, in situ Diffuse Reflectance Infrared and Raman spectroscopy. Not only did CO2 as an oxidant favor the higher yield of styrene, but it also inhibited the deposition of coke during the ethylbenzene ODHmore » reaction. Ethylbenzene ODH reaction over ceria followed a two-step pathway: Ethylbenzene is first dehydrogenated to styrene with H2 formed simultaneously, and then CO2 reacts with H2 via the reverse water gas shift. The styrene produced can easily polymerize to form polystyrene, a key intermediate for coke formation. In the absence of CO2, the polystyrene transforms into graphite-like coke at temperatures above 500 °C, which leads to catalyst deactivation. While in the presence of CO2, the coke deposition can be effectively removed via oxidation with CO2.« less

Anodized Steel Electrodes for Supercapacitors.

PubMed

Sagu, Jagdeep S; Wijayantha, K G Upul; Bohm, Mallika; Bohm, Siva; Kumar Rout, Tapan

2016-03-09

Steel was anodized in 10 M NaOH to enhance its surface texture and internal surface area for application as an electrode in supercapacitors. A mechanism was proposed for the anodization process. Field-emission gun scanning electron microscopy (FEGSEM) studies of anodized steel revealed that it contains a highly porous sponge like structure ideal for supercapacitor electrodes. X-ray photoelectron spectroscopy (XPS) measurements showed that the surface of the anodized steel was Fe2O3, whereas X-ray diffraction (XRD) measurements indicated that the bulk remained as metallic Fe. The supercapacitor performance of the anodized steel was tested in 1 M NaOH and a capacitance of 18 mF cm(-2) was obtained. Cyclic voltammetry measurements showed that there was a large psueudocapacitive contribution which was due to oxidation of Fe to Fe(OH)2 and then further oxidation to FeOOH, and the respective reduction of these species back to metallic Fe. These redox processes were found to be remarkably reversible as the electrode showed no loss in capacitance after 10000 cycles. The results demonstrate that anodization of steel is a suitable method to produce high-surface-area electrodes for supercapacitors with excellent cycling lifetime.

Design and Preparation of Nanoparticle Dimers for SERS Detection

DTIC Science & Technology

2012-09-10

sensitivity afforded by surface enhanced Raman spectroscopy (SERS). Metal nanoparticles dimers were synthesized that incorporate SERS reporters...and antigens, based on the remarkable sensitivity afforded by surface enhanced Raman spectroscopy (SERS). Metal nanoparticles dimers were...Potma, V. A._Apkarian. High Sensitivity Surface-Enhanced Raman Scattering in Solution Using Engineered Silver Nanosphere Dimers, The Journal of

Use of Surface-Enhanced Raman Spectroscopy in Inorganic Syntheses for an Upper-Level Exploratory Lab

ERIC Educational Resources Information Center

Seney, Caryn S.; Yelverton, Joshua C.; Eanes, Sharon; Patel, Vikas; Riggs, Julia; Wright, Sarah; Bright, Robin M.

2007-01-01

An experiment is designed where students will be using both gold and silver nanoparticles to study the enhancement factors of organic molecules adsorbed to the surface of the nanoparticles during or after synthesis by using surface-enhanced Raman spectroscopy (SERS). The experiment has helped students learn about the theory and experimental…

Localized surface plasmon resonances in nanostructures to enhance nonlinear vibrational spectroscopies: towards an astonishing molecular sensitivity

PubMed Central

2014-01-01

Summary Vibrational transitions contain some of the richest fingerprints of molecules and materials, providing considerable physicochemical information. Vibrational transitions can be characterized by different spectroscopies, and alternatively by several imaging techniques enabling to reach sub-microscopic spatial resolution. In a quest to always push forward the detection limit and to lower the number of needed vibrational oscillators to get a reliable signal or imaging contrast, surface plasmon resonances (SPR) are extensively used to increase the local field close to the oscillators. Another approach is based on maximizing the collective response of the excited vibrational oscillators through molecular coherence. Both features are often naturally combined in vibrational nonlinear optical techniques. In this frame, this paper reviews the main achievements of the two most common vibrational nonlinear optical spectroscopies, namely surface-enhanced sum-frequency generation (SE-SFG) and surface-enhanced coherent anti-Stokes Raman scattering (SE-CARS). They can be considered as the nonlinear counterpart and/or combination of the linear surface-enhanced infrared absorption (SEIRA) and surface-enhanced Raman scattering (SERS) techniques, respectively, which are themselves a branching of the conventional IR and spontaneous Raman spectroscopies. Compared to their linear equivalent, those nonlinear vibrational spectroscopies have proved to reach higher sensitivity down to the single molecule level, opening the way to astonishing perspectives for molecular analysis. PMID:25551056

Fabrication of phytic acid sensor based on mixed phytase-lipid Langmuir-Blodgett films.

PubMed

Caseli, Luciano; Moraes, Marli L; Zucolotto, Valtencir; Ferreira, Marystela; Nobre, Thatyane M; Zaniquelli, Maria Elisabete D; Rodrigues Filho, Ubirajara P; Oliveira, Osvaldo N

2006-09-26

This paper reports the surface activity of phytase at the air-water interface, its interaction with lipid monolayers, and the construction of a new phytic acid biosensor on the basis of the Langmuir-Blodgett (LB) technique. Phytase was inserted in the subphase solution of dipalmitoylphosphatidylglycerol (DPPG) Langmuir monolayers, and its incorporation to the air-water interface was monitored with surface pressure measurements. Phytase was able to incorporate into DPPG monolayers even at high surface pressures, ca. 30 mN/m, under controlled ionic strength, pH, and temperature. Mixed Langmuir monolayers of phytase and DPPG were characterized by surface pressure-area and surface potential-area isotherms, and the presence of the enzyme provided an expansion in the monolayers (when compared to the pure lipid at the interface). The enzyme incorporation also led to significant changes in the equilibrium surface compressibility (in-plane elasticity), especially in liquid-expanded and liquid-condensed regions. The dynamic surface elasticity for phytase-containing interfaces was investigated using harmonic oscillation and axisymmetric drop shape analysis. The insertion of the enzyme at DPPG monolayers caused an increase in the dynamic surface elasticity at 30 mN m(-)(1), indicating a strong interaction between the enzyme and lipid molecules at a high-surface packing. Langmuir-Blodgett (LB) films containing 35 layers of mixed phytase-DPPG were characterized by ultraviolet-visible and fluorescence spectroscopy and crystal quartz microbalance nanogravimetry. The ability in detecting phytic acid was studied with voltammetric measurements.

Biochar characteristics produced from rice husks and their sorption properties for the acetanilide herbicide metolachlor.

PubMed

Wei, Lan; Huang, Yufen; Li, Yanliang; Huang, Lianxi; Mar, Nyo Nyo; Huang, Qing; Liu, Zhongzhen

2017-02-01

Rice husk biochar (RHBC) was prepared for use as adsorbents for the herbicide metolachlor. The characteristics and sorption properties of metolachlor adsorbed by the RHBC prepared at different pyrolysis temperatures were determined by analysis of physico-chemical characteristics, Fourier transform infrared spectroscopy (FTIR), Boehm titration, scanning electron microscopy (SEM), and thermodynamics and kinetics adsorption. With increasing pyrolysis temperature, the RHBC surface area greatly increased (from 2.57 to 53.08 m 2  g -1 ). RHBC produced at the highest temperature (750 °C) had the greatest surface area; SEM also showed the formation of a porous surface on RH-750 biochar. The sorption capacity of RHBC also increased significantly with increasing pyrolysis temperature and was characterized by the Freundlich constant K f for the adsorption capacity increasing from 125.17-269.46 (pyrolysis at 300 °C) to 339.94-765.24 (pyrolysis at 750 °C). The results indicated that the surface area and pore diameter of RHBC produced with high pyrolysis temperature (i.e., 750 °C) had the greatest impact on the adsorption of metolachlor. The FTIR, Boehm titration, and SEM analysis showed that the greatest number of surface groups were on RHBC produced at the lowest temperature (300 °C). The biochars produced at different pyrolysis temperatures had different mechanisms of adsorbing metolachlor, which exhibited a transition from hydrogen bonds dominant at low pyrolytic temperature to pore-filling dominant at higher pyrolytic temperature.

Multicharged Ion Promoted Desorption (MIPD) of Reaction Co-Products

DTIC Science & Technology

2015-02-13

measurements of surface modifications using mass spectrometry, Raman spectroscopy and XPS were made to 1. REPORT DATE (DD-MM-YYYY) 4. TITLE AND...desorption and ex-situ measurements of surface modifications using mass spectrometry, Raman spectroscopy and XPS were made to determine ion-induced...irradiations were made with the samples at normal incidence to the incoming beams and post-analysis of these samples was achieved using Raman spectroscopy. It

Preparation and Characterization of Impregnated Commercial Rice Husks Activated Carbon with Piperazine for Carbon Dioxide (CO2) Capture

NASA Astrophysics Data System (ADS)

Masoum Raman, S. N.; Ismail, N. A.; Jamari, S. S.

2017-06-01

Development of effective materials for carbon dioxide (CO2) capture technology is a fundamental importance to reduce CO2 emissions. This work establishes the addition of amine functional group on the surface of activated carbon to further improve the adsorption capacity of CO2. Rice husks activated carbon were modified using wet impregnation method by introducing piperazine onto the activated carbon surfaces at different concentrations and mixture ratios. These modified activated carbons were characterized by using X-Ray Diffraction (XRD), Brunauer, Emmett and Teller (BET), Fourier Transform Infrared Spectroscopy (FTIR) and Field Emission Scanning Electron Microscopy (FESEM). The results from XRD analysis show the presence of polyethylene butane at diffraction angles of 21.8° and 36.2° for modified activated carbon with increasing intensity corresponding to increase in piperazine concentration. BET results found the surface area and pore volume of non-impregnated activated carbon to be 126.69 m2/g and 0.081 cm3/g respectively, while the modified activated carbons with 4M of piperazine have lower surface area and pore volume which is 6.77 m2/g and 0.015 cm3/g respectively. At 10M concentration, the surface area and pore volume are the lowest which is 4.48 m2/g and 0.0065 cm3/g respectively. These results indicate the piperazine being filled inside the activated carbon pores thus, lowering the surface area and pore volume of the activated carbon. From the FTIR analysis, the presence of peaks at 3312 cm-1 and 1636 cm-1 proved the existence of reaction between carboxyl groups on the activated carbon surfaces with piperazine. The surface morphology of activated carbon can be clearly seen through FESEM analysis. The modified activated carbon contains fewer pores than non-modified activated carbon as the pores have been covered with piperazine.

Conformal Surface Coatings to Enable High Volume Expansion Li-Ion Anode Materials

DTIC Science & Technology

2010-07-12

the formation of a metastable amor - phous alloy, sustaining up to 4.4 Li+ per Si.[2] Transition metal oxides undergo a conversion reaction at lower...in Figure 1a. The ele - mental composition of the circular area labeled P1 was exam- ined using energy dispersive X-ray spectroscopy (EDS) to verify...electrodes were of a 70:10:20 composition active material (AM): acetylene black ( AB ): binder (PVDF) and subjected to 250 8C heat treatment. For

Nitrogen-doped hierarchical porous carbon microsphere through KOH activation for supercapacitors.

PubMed

Jiang, Jingui; Chen, Hao; Wang, Zhao; Bao, Luke; Qiang, Yiwei; Guan, Shiyou; Chen, Jianding

2015-08-15

A porous carbon microsphere with moderate specific surface area and superior specific capacitance for supercapacitors is fabricated from polyphosphazene microsphere as the single heteroatoms source by the carbonization and subsequent KOH activation under N2 atmosphere. With KOH activation, X-ray photoelectron spectroscopy analysis confirms that the phosphorus of polyphosphazene microsphere totally vanishes, and the doping content of nitrogen and its population of various functionalities on porous carbon microsphere surface are tuned. Compared with non-porous carbon microsphere, the texture property of the resultant porous carbon microsphere subjected to KOH activation has been remarkably developed with the specific surface area growing from 315 to 1341 m(2) g(-1)and the pore volume turning from 0.17 to 0.69 cm(3) g(-1). Prepared with the KOH/non-porous carbon microsphere weight ratio at 1.0, the porous carbon microsphere with moderate specific surface area of 568 m(2) g(-1), exhibits intriguing electrochemical behavior in 1 M H2SO4 aqueous electrolyte, with superior specific capacitance (278 F g(-1) at 0.1 A g(-1)), good rate capability (147 F g(-1) remained at 10 A g(-1)) and robust cycling durability (No capacitance loss after 5000 cycles). The promising electrochemical performance could be ascribed to the synergy of nitrogen heteroatom functionalities and the porous morphology. Copyright © 2015 Elsevier Inc. All rights reserved.

Surface Inspection Machine Infrared (SIMIR). Final CRADA report

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

Powell, G.L.; Neu, J.T.; Beecroft, M.

This Cooperative Research and Development Agreement was a one year effort to make the surface inspection machine based on diffuse reflectance infrared spectroscopy (Surface Inspection Machine-Infrared, SIMIR), being developed by Surface Optics Corporation, perform to its highest potential as a practical, portable surface inspection machine. The design function of the SIMIR is to inspect metal surfaces for cleanliness (stains). The system is also capable of evaluating graphite-resin systems for cure and heat damage, and for measuring the effects of moisture exposure on lithium hydride, corrosion on uranium metal, and the constituents of and contamination on wood, paper, and fabrics. Overmore » the period of the CRADA, extensive experience with the use of the SIMIR for surface cleanliness measurements have been achieved through collaborations with NASA and the Army. The SIMIR was made available to the AMTEX CRADA for Finish on Yarn where it made a very significant contribution. The SIMIR was the foundation of a Forest Products CRADA that was developed over the time interval of this CRADA. Surface Optics Corporation and the SIMIR have been introduced to the chemical spectroscopy on-line analysis market and have made staffing additions and arrangements for international marketing of the SIMIR as an on-line surface inspection device. LMES has been introduced to a wide range of aerospace applications, the research and fabrication skills of Surface Optics Corporation, has gained extensive experience in the areas of surface cleanliness from collaborations with NASA and the Army, and an extensive introduction to the textile and forest products industries. The SIMIR, marketed as the SOC-400, has filled an important new technology need in the DOE-DP Enhanced Surveillance Program with instruments delivered to or on order by LMES, LANL, LLNL, and Pantex, where extensive collaborations are underway to implement and improve this technology.« less

VERITAS (Venus Emissivity, Radio Science, InSAR, Topo-graphy And Spectroscopy): A Proposed Discovery Mission

NASA Astrophysics Data System (ADS)

Smrekar, Suzanne; Dyar, Melinda; Hensley, Scott; Helbert, Joern; VERITAS Science Team

2016-10-01

VERITAS addresses one of the most fundamental questions in planetary evolution: How Earth-like is Venus? These twin planets diverged down different evolutionary paths, yet Venus may hold lessons for past and future Earth, as well as for Earth-sized exoplanets. VERITAS will search for the mineralogical fingerprints of past water, follow up on the discoveries of recent volcanism and the possible young surface age, and reveal the conditions that have prevented plate tectonics from developing. Collectively these questions address how Venus ended up a sulfurous inferno while Earth became habitable.VERITAS carries the Venus Interferometric Synthetic Aperture Radar (VISAR) and the Venus Emissivity Mapper (VEM), plus a gravity science investigation.The VISAR X-band radar produces: 1) a global digital elevation model (DEM) with 250 m postings, 5 m height accuracy, 2) Synthetic aperture radar (SAR) global imaging with 30 m pixels, 3) SAR imaging at 15 m for targeted areas, and 4) surface deformation from repeat pass interferometry (RPI) at 2 mm height precision for targeted, potentially active areas. VEM [see Helbert abstract] will measure surface emissivity, look for active volcanic flows and outgassing of water over ~78% of the surface using 6 NIR surface bands within 5 atmospheric windows and 8 bands for calibration of clouds, stray light, and water vapor.VERITAS uses Ka-band uplink and downlink to create a global gravity field with 3 mgal accuracy and 145 km resolution (130 spherical harmonic degree and order or d&o) and providing a significantly higher resolution field with much more uniform resolution than that available from Magellan.VERITAS will create a rich data set of high resolution topography, imaging, spectroscopy, and gravity. These co-registered data sets will be on par with those acquired for Mercury, Mars and the Moon that have revolutionized our understanding of these bodies. VERITAS would be a valuable asset for future lander or probe missions, collecting the data needed to select landing or entry sites. VERITAS also provides a baseline for future missions to detect surface change, and contributes to our ability to predict the nature of Earth-sized exoplanets.

Applications of surface analytical techniques in Earth Sciences

NASA Astrophysics Data System (ADS)

Qian, Gujie; Li, Yubiao; Gerson, Andrea R.

2015-03-01

This review covers a wide range of surface analytical techniques: X-ray photoelectron spectroscopy (XPS), scanning photoelectron microscopy (SPEM), photoemission electron microscopy (PEEM), dynamic and static secondary ion mass spectroscopy (SIMS), electron backscatter diffraction (EBSD), atomic force microscopy (AFM). Others that are relatively less widely used but are also important to the Earth Sciences are also included: Auger electron spectroscopy (AES), low energy electron diffraction (LEED) and scanning tunnelling microscopy (STM). All these techniques probe only the very top sample surface layers (sub-nm to several tens of nm). In addition, we also present several other techniques i.e. Raman microspectroscopy, reflection infrared (IR) microspectroscopy and quantitative evaluation of minerals by scanning electron microscopy (QEMSCAN) that penetrate deeper into the sample, up to several μm, as all of them are fundamental analytical tools for the Earth Sciences. Grazing incidence synchrotron techniques, sensitive to surface measurements, are also briefly introduced at the end of this review. (Scanning) transmission electron microscopy (TEM/STEM) is a special case that can be applied to characterisation of mineralogical and geological sample surfaces. Since TEM/STEM is such an important technique for Earth Scientists, we have also included it to draw attention to the capability of TEM/STEM applied as a surface-equivalent tool. While this review presents most of the important techniques for the Earth Sciences, it is not an all-inclusive bibliography of those analytical techniques. Instead, for each technique that is discussed, we first give a very brief introduction about its principle and background, followed by a short section on approaches to sample preparation that are important for researchers to appreciate prior to the actual sample analysis. We then use examples from publications (and also some of our known unpublished results) within the Earth Sciences to show how each technique is applied and used to obtain specific information and to resolve real problems, which forms the central theme of this review. Although this review focuses on applications of these techniques to study mineralogical and geological samples, we also anticipate that researchers from other research areas such as Material and Environmental Sciences may benefit from this review.

Dynamics of CrO 3 –Fe 2 O 3 Catalysts during the High-Temperature Water-Gas Shift Reaction: Molecular Structures and Reactivity

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

Keturakis, Christopher J.; Zhu, Minghui; Gibson, Emma K.

2016-06-13

A series of supported CrO 3/Fe 2O 3 catalysts were investigated for the high-temperature water-gas shift (WGS) and reverse-WGS reactions and extensively characterized using in situ and operando IR, Raman, and XAS spectroscopy during the high-temperature WGS/RWGS reactions. The in situ spectroscopy examinations reveal that the initial oxidized catalysts contain surface dioxo (O=) 2Cr 6+O 2 species and a bulk Fe 2O 3 phase containing some Cr 3+ substituted into the iron oxide bulk lattice. Operando spectroscopy studies during the high-temperature WGS/RWGS reactions show that the catalyst transforms during the reaction. The crystalline Fe 2O 3 bulk phase becomes Femore » 3O 4 ,and surface dioxo (O=) 2Cr 6+O 2 species are reduced and mostly dissolve into the iron oxide bulk lattice. Consequently, the chromium–iron oxide catalyst surface is dominated by FeO x sites, but some minor reduced surface chromia sites are also retained. The Fe 3–-xCr xO 4 solid solution stabilizes the iron oxide phase from reducing to metallic Fe0 and imparts an enhanced surface area to the catalyst. Isotopic exchange studies with C 16O 2/H 2 → C 18O 2/H 2 isotopic switch directly show that the RWGS reaction proceeds via the redox mechanism and only O* sites from the surface region of the chromium–iron oxide catalysts are involved in the RWGS reaction. The number of redox O* sites was quantitatively determined with the isotope exchange measurements under appropriate WGS conditions and demonstrated that previous methods have undercounted the number of sites by nearly 1 order of magnitude. The TOF values suggest that only the redox O* sites affiliated with iron oxide are catalytic active sites for WGS/RWGS, though a carbonate oxygen exchange mechanism was demonstrated to exist, and that chromia is only a textural promoter that increases the number of catalytic active sites without any chemical promotion effect.« less

Inherent substrate-dependent growth initiation and selective-area atomic layer deposition of TiO{sub 2} using “water-free” metal-halide/metal alkoxide reactants

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

Atanasov, Sarah E.; Kalanyan, Berç; Parsons, Gregory N., E-mail: gnp@ncsu.edu

2016-01-15

Titanium dioxide atomic layer deposition (ALD) is shown to proceed selectively on oxidized surfaces with minimal deposition on hydrogen-terminated silicon using titanium tetrachloride (TiCl{sub 4}) and titanium tetra-isopropoxide [Ti(OCH(CH{sub 3}){sub 2}){sub 4}, TTIP] precursors. Ex situ x-ray photoelectron spectroscopy shows a more rapid ALD nucleation rate on both Si–OH and Si–H surfaces when water is the oxygen source. Eliminating water delays the oxidation of the hydrogen-terminated silicon, thereby impeding TiO{sub 2} film growth. For deposition at 170 °C, the authors achieve ∼2 nm of TiO{sub 2} on SiO{sub 2} before substantial growth takes place on Si–H. On both Si–H and Si–OH, themore » surface reactions proceed during the first few TiCl{sub 4}/TTIP ALD exposure steps where the resulting products act to impede subsequent growth, especially on Si–H surfaces. Insight from this work helps expand understanding of “inherent” substrate selective ALD, where native differences in substrate surface reaction chemistry are used to promote desired selective-area growth.« less

The functionalization of carbon nanosheets

NASA Astrophysics Data System (ADS)

Quinlan, Ronald A.

Carbon nanosheets are a novel two-dimensional nanostructure made up of 2-20 graphene atomic planes oriented with their in-plane axis perpendicular to the growth substrate. Previous efforts in developing nanosheet technology have focused on the characterization of the system and their development as an electron source due to the high atomic enhancement factor (beta) and low turn on field. Further investigation of nanosheets as high surface area electrodes revealed poor wetting by polymeric material and extreme hydrophobic behavior. Because nanosheet technology has promise as a high surface area electrode material, this thesis research has focused on three areas of interest: the enhancement of nanosheets through chemical modification, the incorporation of the nanosheets into a polymeric composite and the delivery of a proof of concept measurement. We have successfully introduced defects into the graphene lattice of the nanosheet system via an acid treatment. Inspection of these defects by x-ray absorption near-edge spectroscopy (XANES) shows the introduction of two features in the spectra assigned to C=O pi* and C-O sigma* transitions. Thermal desorption spectroscopy (TDS) was used to identify the oxygen containing groups created during the functionalization as carboxylic and hydroxyl functional groups. These groups were identified through the combination of carboxylic, hydroxyl, anhydride and lactone peaks in the CO2, CO and H 2O TDS spectra. Deconvolution of the TDS spectra using 1st and 2nd order Polanyi-Wigner equations enables the calculation of desorption energy values for individual features and for the estimation of the number of atoms desorbing from the surface during a particular event. Identification of the exact nature of the functional groups was attempted through high resolution x-ray photoelectron spectroscopy (XPS) of the C(1s) and O(1s) peaks. Though the pairing of sub-peaks with specific functionalities of the system was not possible due to the complexities of the spectra, the trends observed in the data support the data gathered via the XANES and TDS experiments. Also, a procedure for the classification of defect density and exact functionality was outlined. Deconvolution of the TDS spectra using 1 st and 2nd order Polanyi-Wigner equations enabled the calculation of desorption energy values for individual features and for the estimation of the number of atoms desorbing from the surface during a particular event. This information along with the changing sub-peak areas from dedicated and calibrated XPS system would allow for not only a more accurate estimation of defect density, but also for the identification of sub-peaks in the C(1s) and O(1s) spectra. Finally, photoluminescence measurements of poly[2-methoxy-5-(2'-ethyl-hexyloxy)-1,4-phenylene vinylene] (MEH-PPV) and MEH-PPV/nanosheet systems showed a quenching of three orders of magnitude for the MEH-PPV/nanosheet system suggesting that nanosheets are a viable option for excition separation in organic photovoltaics.

Surface functionalization of cyclic olefin copolymer with aryldiazonium salts: A covalent grafting method

NASA Astrophysics Data System (ADS)

Brisset, Florian; Vieillard, Julien; Berton, Benjamin; Morin-Grognet, Sandrine; Duclairoir-Poc, Cécile; Le Derf, Franck

2015-02-01

Covalent immobilization of biomolecules on the surface of cyclic olefin copolymer (COC) is still a tough challenge. We developed a robust method for COC surface grafting through reaction with aryldiazonium. Chemical diazonium reduction generated an aryl radical and the formation of a grafted film layer on the organic surface. We also demonstrated that the chemical reduction of diazonium salt was not sufficient to form a film on the COC surface. UV illumination had to be combined with chemical reduction to graft an aryl layer onto the COC surface. We optimized organic film deposition by using different chemical reducers, different reaction times and reagent proportions. We characterized surface modifications by fluorescence microscopy and contact angle measurements, infrared spectroscopy, X-ray photoemission spectroscopy and Raman spectroscopy, and assessed the topography of the aryl film by atomic force microscopy. This original strategy allowed us to evidence various organic functions to graft biomolecules onto COC surfaces with a fast and efficient technique.

Biomass-derived functional porous carbons as novel electrode material for the practical detection of biomolecules in human serum and snail hemolymph.

PubMed

Veeramani, Vediyappan; Madhu, Rajesh; Chen, Shen-Ming; Lou, Bih-Show; Palanisamy, Jayabal; Vasantha, Vairathevar Sivasamy

2015-05-22

The biomass-derived activated carbons (ACs) have been prepared with high surface areas up to 793 m(2) g(-1) is by ZnCl2 activation at three different temperatures, viz. AC700, AC800, and AC900. The AC samples were characterized by a variety of analytical and spectroscopy techniques. The as-synthesized ACs were adopted for the simultaneous electrochemical detection of ascorbic acid (AA), dopamine (DA), and uric acid (UA). For comparison, reduced graphene oxide (RGO) was employed for the proposed sensor. The high surface area, modulated pore size and the presence of oxygen surface functional groups like heteroatoms (83.427% C, 1.085% N, 0.383% S, and 0.861% H) in the biomass-derived AC is found to be responsible for the excellent catalytic activities of biomolecules. Fascinatingly, the facile sensor further used to detect biomolecules levels in the snail hemolymph and human blood serum. Notably, the obtained analytical parameters for the biomolecules detection over the AC modified GCE, outperforming several carbon-based modified electrodes in literatures.

Effect of calcination temperatures on microstructures and photocatalytic activity of tungsten trioxide hollow microspheres.

PubMed

Yu, Jiaguo; Qi, Lifang; Cheng, Bei; Zhao, Xiufeng

2008-12-30

Tungsten trioxide hollow microspheres were prepared by immersing SrWO4 microspheres in a concentrated HNO3 solution, and then calcined at different temperatures. The prepared tungsten oxide samples were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, Fourier transform infrared spectra, differential thermal analysis-thermogravimetry, UV-visible spectrophotometry, scanning electron microscopy, N2 adsorption/desorption measurements. The photocatalytic activity of the samples was evaluated by photocatalytic decolorization of rhodamine B aqueous solution under visible-light irradiation. It was found that with increasing calcination temperatures, the average crystallite size and average pore size increased, on the contrary, Brunauer-Emmett-Teller-specific surface areas decreased. However, pore volume and porosity increased firstly, and then decreased. Increasing calcination temperatures resulted in the changes of surface morphology of hollow microspheres. The un-calcined and 300 degrees C-calcined samples showed higher photocatalytic activity than other samples. At 400 degrees C, the photocatalytic activity decreased greatly due to the decrease of specific surface areas. At 500 degrees C, the photocatalytic activity of the samples increased again due to the junction effect of two phases.

Biomass-derived functional porous carbons as novel electrode material for the practical detection of biomolecules in human serum and snail hemolymph

PubMed Central

Veeramani, Vediyappan; Madhu, Rajesh; Chen, Shen-Ming; Lou, Bih-Show; Palanisamy, Jayabal; Vasantha, Vairathevar Sivasamy

2015-01-01

The biomass-derived activated carbons (ACs) have been prepared with high surface areas up to 793 m2 g−1 is by ZnCl2 activation at three different temperatures, viz. AC700, AC800, and AC900. The AC samples were characterized by a variety of analytical and spectroscopy techniques. The as-synthesized ACs were adopted for the simultaneous electrochemical detection of ascorbic acid (AA), dopamine (DA), and uric acid (UA). For comparison, reduced graphene oxide (RGO) was employed for the proposed sensor. The high surface area, modulated pore size and the presence of oxygen surface functional groups like heteroatoms (83.427% C, 1.085% N, 0.383% S, and 0.861% H) in the biomass-derived AC is found to be responsible for the excellent catalytic activities of biomolecules. Fascinatingly, the facile sensor further used to detect biomolecules levels in the snail hemolymph and human blood serum. Notably, the obtained analytical parameters for the biomolecules detection over the AC modified GCE, outperforming several carbon-based modified electrodes in literatures. PMID:25998156

Biomass-derived functional porous carbons as novel electrode material for the practical detection of biomolecules in human serum and snail hemolymph

NASA Astrophysics Data System (ADS)

Veeramani, Vediyappan; Madhu, Rajesh; Chen, Shen-Ming; Lou, Bih-Show; Palanisamy, Jayabal; Vasantha, Vairathevar Sivasamy

2015-05-01

The biomass-derived activated carbons (ACs) have been prepared with high surface areas up to 793 m2 g-1 is by ZnCl2 activation at three different temperatures, viz. AC700, AC800, and AC900. The AC samples were characterized by a variety of analytical and spectroscopy techniques. The as-synthesized ACs were adopted for the simultaneous electrochemical detection of ascorbic acid (AA), dopamine (DA), and uric acid (UA). For comparison, reduced graphene oxide (RGO) was employed for the proposed sensor. The high surface area, modulated pore size and the presence of oxygen surface functional groups like heteroatoms (83.427% C, 1.085% N, 0.383% S, and 0.861% H) in the biomass-derived AC is found to be responsible for the excellent catalytic activities of biomolecules. Fascinatingly, the facile sensor further used to detect biomolecules levels in the snail hemolymph and human blood serum. Notably, the obtained analytical parameters for the biomolecules detection over the AC modified GCE, outperforming several carbon-based modified electrodes in literatures.

Interaction of hydrogen chloride and water with oxide surfaces. III - Titanium dioxide

NASA Technical Reports Server (NTRS)

Siriwardane, R. V.; Wightman, J. P.

1983-01-01

The adsorption of hydrogen chloride and water vapors on five TiO2 powders in both the anatase and rutile crystalline forms was studied as a function of temperature, pressure, and outgas conditions. The adsorbents were characterized utilizing X-ray powder diffraction, scanning electron microscopy, surface area analysis, indicator method, microelectrophoresis, XPS, and infrared spectroscopy. It was found that both outgas temperature and adsorption temperature influenced the adsorption of water vapor on TiO2, while water vapor adsorption on TiO2 was completely reversible. It is argued that the number of hydroxyl groups present on the surface determines the adsorption capacity of water on the different titanium dioxides. It was found that heats of immersion in water were affected significantly by outgas temperature. Hydrogen chloride adsorption isotherms at 30 C measured on TiO2 after outgassing at 100-400 C showed that a part of the total HCl adsorbed was irreversibly adsorbed. The highest HCl adsorption capacity per unit area was exhibited by anatase, while pure rutile exhibited the lowest adsorption capacity.

Analysis of the surface effects on adhesion in MEMS structures

NASA Astrophysics Data System (ADS)

Rusu, F.; Pustan, M.; Bîrleanu, C.; Müller, R.; Voicu, R.; Baracu, A.

2015-12-01

One of the main failure causes in microelectromechanical systems (MEMS) is stiction. Stiction is the adhesion of contacting surfaces due to surface forces. Adhesion force depends on the operating conditions and is influenced by the contact area. In this study, the adhesion force between MEMS materials and the AFM tips is analyzed using the spectroscopy in point mode of the AFM. The aim is to predict the stiction failure mode in MEMS. The investigated MEMS materials are silicon, polysilicon, platinum, aluminum, and gold. Three types of investigations were conducted. The first one aimed to determine the variation of the adhesion force with respect to the variation of the roughness. The roughness has a strong influence on the adhesion because the contact area between components increases if the roughness decreases. The second type of investigation aimed to determine the adhesion force in multiple points of each considered sample. The values obtained experimentally for the adhesion force were also validated using the JKR and DMT models. The third type of investigation was conducted with the purpose of determining the influence of the temperature on the adhesion force.

Preparation and application of nanoglued binary titania-silica aerogel.

PubMed

Luo, Liang; Cooper, Adrienne T; Fan, Maohong

2009-01-15

Nanoglued binary titania (TiO2)-silica (SiO2) aerogel, as a novel type of photocatalyst, has been synthesized on glass substrates. Using an about-to-gel SiO2 sol as nanoglue, anatase TiO2 aerogel was immobilized into a three-dimensional mesoporous network of the SiO2. Factorial designs were employed to optimize both TiO2 aerogel and binary TiO2-SiO2 aerogel synthesis. Characterization of the as-prepared TiO2 and binary samples by surface area, porosity, and surface chemical composition showed that the photocatalysts were high-surface-area nanoporous materials, with a Ti4+ valency. The binary aerogel exhibited high photocatalytic activity for the degradation of methylene blue (MB) under simulated solar light; the reaction followed the pseudo first-order Langmuir-Hinshelwood (L-H) kinetic model. Fluorescence spectroscopy revealed that the hydroxyl (*OH) radical was formed during the illumination of the binary TiO2-SiO2 aerogel in a solution of probe molecules, which corroborates the probable mechanism of hydroxyl radical oxidation of contaminants in photocatalytic reactions.

Direct observation of spin-resolved full and empty electron states in ferromagnetic surfaces

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

Berti, G., E-mail: giulia.berti@polimi.it; Calloni, A.; Brambilla, A.

2014-07-15

We present a versatile apparatus for the study of ferromagnetic surfaces, which combines spin-polarized photoemission and inverse photoemission spectroscopies. Samples can be grown by molecular beam epitaxy and analyzed in situ. Spin-resolved photoemission spectroscopy analysis is done with a hemispherical electron analyzer coupled to a 25 kV-Mott detector. Inverse photoemission spectroscopy experiments are performed with GaAs crystals as spin-polarized electron sources and a UV bandpass photon detector. As an example, measurements on the oxygen passivated Fe(100)-p(1×1)O surface are presented.

A fundamental approach to the sticking of insect residues to aircraft wings

NASA Technical Reports Server (NTRS)

Yi, O.; Eiss, N. S.; Wightman, J. P.

1988-01-01

The aircraft industry is concerned with the increase of drag on planes due to the sticking of insects on critical airfoil areas. The objectives of the present study were to investigate the effects of surface energy and elasticity on the number of insects sticking onto the polymer coatings on a modified aircraft wing and to determine the mechanism by which insects stick onto surfaces during high velocity impact. Analyses including scanning electron microscopy, electron spectroscopy for chemical analysis and contact angle measurements of uncoated and polymer coated aluminum surfaces were performed. A direct relation between the number of insects sticking on a sample and its surface energy was obtained. Since the sticky liquid from a burst open insect will not spread on the low energy surface, it will ball up providing poor adhesion between the insect debris and the surface. The incoming air flow can easily blow off the insect debris and thus reducing the number of insects that remain stuck on the surface. Also a direct relation between the number of insect sticking onto a surface and their modulus of elasticity was obtained.

Chemically exfoliating large sheets of phosphorene via choline chloride urea viscosity-tuning

NASA Astrophysics Data System (ADS)

Ng, A.; Sutto, T. E.; Matis, B. R.; Deng, Y.; Ye, P. D.; Stroud, R. M.; Brintlinger, T. H.; Bassim, N. D.

2017-04-01

Exfoliation of two-dimensional phosphorene from bulk black phosphorous through chemical means is demonstrated where the solvent system of choice (choline chloride urea diluted with ethanol) has the ability to successfully exfoliate large-area multi-layer phosphorene sheets and further protect the flakes from ambient degradation. The intercalant solvent molecules, aided by low-powered sonication, diffuse between the layers of the bulk black phosphorus, allowing for the exfoliation of the multi-layer phosphorene through breaking of the interlayer van der Waals bonds. Through viscosity tuning, the optimal parameters (1:1 ratio between the intercalant and the diluting solvent) at which the exfoliation takes place is determined. Our exfoliation technique is shown to produce multi-layer phosphorene flakes with surface areas greater than 3 μm2 (a factor of three larger than what has previously been reported for a similar exfoliation method) while limiting exposure to the ambient environment, thereby protecting the flakes from degradation. Characterization techniques such as optical microscopy, Raman spectroscopy, ultraviolet-visible spectroscopy, and (scanning) transmission electron microscopy are used to investigate the quality, quantity, and thickness of the exfoliated flakes.

Pressure injury prediction using diffusely scattered light

NASA Astrophysics Data System (ADS)

Diaz, David; Lafontant, Alec; Neidrauer, Michael; Weingarten, Michael S.; DiMaria-Ghalili, Rose Ann; Scruggs, Ericka; Rece, Julianne; Fried, Guy W.; Kuzmin, Vladimir L.; Zubkov, Leonid

2017-02-01

Pressure injuries (PIs) originate beneath the surface of the skin at the interface between bone and soft tissue. We used diffuse correlation spectroscopy (DCS) and diffuse near-infrared spectroscopy (DNIRS) to predict the development of PIs by measuring dermal and subcutaneous red cell motion and optical absorption and scattering properties in 11 spinal cord injury subjects with only nonbleachable redness in the sacrococcygeal area in a rehabilitation hospital and 20 healthy volunteers. A custom optical probe was developed to obtain continuous DCS and DNIRS data from sacrococcygeal tissue while the subjects were placed in supine and lateral positions to apply pressure from body weight and to release pressure, respectively. Rehabilitation patients were measured up to four times over a two-week period. Three rehabilitation patients developed open PIs (POs) within four weeks and eight patients did not (PNOs). Temporal correlation functions in the area of redness were significantly different (p<0.01) during both baseline and applied pressure stages for POs and PNOs. The results show that our optical method may be used for the early prediction of ulcer progression.

Self-assembled nanoparticle aggregates: Organizing disorder for high performance surface-enhanced spectroscopy

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

Fasolato, C.; Center for Life Nanoscience@Sapienza, Istituto Italiano di Tecnologia, Rome; Domenici, F., E-mail: fabiodomenici@gmail.com

2015-06-23

The coherent oscillations of the surface electron gas, known as surface plasmons, in metal nanostructures can give rise to the localization of intense electromagnetic fields at the metal-dielectric interface. These strong fields are exploited in surface enhanced spectroscopies, such as Surface Enhanced Raman Scattering (SERS), for the detection and characterization of molecules at very low concentration. Still, the implementation of SERS-based biosensors requires a high level of reproducibility, combined with cheap and simple fabrication methods. For this purpose, SERS substrates based on self-assembled aggregates of commercial metallic nanoparticles (Nps) can meet all the above requests. Following this line, we reportmore » on a combined micro-Raman and Atomic Force Microscopy (AFM) analysis of the SERS efficiency of micrometric silver Np aggregates (enhancement factors up to 10{sup 9}) obtained by self-assembly. Despite the intrinsic disordered nature of these Np clusters, we were able to sort out some general rules relating the specific aggregate morphology to its plasmonic response. We found strong evidences of cooperative effects among the NPs within the cluster and namely a clear dependence of the SERS-efficiency on both the cluster area (basically linear) and the number of stacked NPs layers. A cooperative action among the superimposed layers has been proved also by electromagnetic simulations performed on simplified nanostructures consisting of stacking planes of ordered Nps. Being clear the potentialities of these disordered self-assembled clusters, in terms of both easy fabrication and signal enhancement, we developed a specific nanofabrication protocol, based on electron beam lithography and molecular functionalization, that allowed for a fine control of the Np assemblies into designed shapes fixing their area and height. In particular, we fabricated 2D ordered arrays of disordered clusters choosing gold Nps owing to their high stability. AFM measurements confirmed the regularity in spacing and size (i.e. area and layer number) of the aggregates. Preliminary SERS measurements confirm the high signal enhancement and demonstrate a quite good reproducibility over large number of aggregates within 100×100 μm{sup 2} 2D super-structure. The availability of such a multisensor could allow a careful statistical analysis of the SERS response, thus leading to a reliable quantitative estimate of the presence of relevant molecular species even at ultra-low concentration.« less

Covalent Surface Modifications of Carbon Nanotubes.

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

Pavia Sanders, Adriana; O'Bryan, Greg

A report meant to document the chemistries investigated by the author for covalent surface modification of CNTs. Oxidation, cycloaddition, and radical reactions were explored to determine their success at covalently altering the CNT surface. Characterization through infrared spectroscopy, Raman spectroscopy, and thermo gravimetric analysis was performed in order to determine the success of the chemistries employed. This report is not exhaustive and was performed for CNT surface modification exploration as it pertains to the "Next Gen" project.

Disposable urea biosensor based on nanoporous ZnO film fabricated from omissible polymeric substrate.

PubMed

Rahmanian, Reza; Mozaffari, Sayed Ahmad; Abedi, Mohammad

2015-12-01

In the present study, a facile and simple fabrication method of a semiconductor based urea biosensor was reported via three steps: (i) producing a ZnO-PVA composite film by means of a polymer assisted electrodeposition of zinc oxide (ZnO) on the F-doped SnO2 conducting glass (FTO) using water soluble polyvinyl alcohol (PVA), (ii) obtaining a nanoporous ZnO film by PVA omission via a subsequent post-treatment by annealing of the ZnO-PVA film, and (iii) preparation of a FTO/ZnO/Urs biosensor by exploiting a nanoporous ZnO film as an efficient and excellent platform area for electrostatic immobilization of urease enzyme (Urs) which was forced by the difference in their isoelectric point (IEP). The characterization techniques focused on the analysis of the ZnO-PVA film surfaces before and after annealing, which had a prominent effect on the porosity of the prepared ZnO film. The surface characterization of the nanostructured ZnO film by a field emission-scanning electron microscopy (FE-SEM), exhibited a film surface area as an effective bio-sensing matrix for enzyme immobilization. The structural characterization and monitoring of the biosensor fabrication was performed using UV-Vis, Fourier Transform Infrared (FT-IR), Raman Spectroscopy, Thermogravimetric Analysis (TGA), Cyclic Voltammetry (CV), and Electrochemical Impedance Spectroscopy (EIS) techniques. The impedimetric results of the FTO/ZnO/Urs biosensor showed a high sensitivity for urea detection within 8.0-110.0mg dL(-1) with the limit of detection as 5.0mg dL(-1). Copyright © 2015 Elsevier B.V. All rights reserved.

Preparation of RuO2-TiO2/Nano-graphite composite anode for electrochemical degradation of ceftriaxone sodium.

PubMed

Li, Dong; Guo, Xiaolei; Song, Haoran; Sun, Tianyi; Wan, Jiafeng

2018-06-05

Graphite-like material is widely used for preparing various electrodes for wastewater treatment. To enhance the electrochemical degradation efficiency of Nano-graphite (Nano-G) anode, RuO 2 -TiO 2 /Nano-G composite anode was prepared through the sol-gel method and hot-press technology. RuO 2 -TiO 2 /Nano-G composite was characterized by X-ray diffraction, X-ray photoelectron spectroscopy, transmission electron microscopy and N 2 adsorption-desorption. Results showed that RuO 2 , TiO 2 and Nano-G were composited successfully, and RuO 2 and TiO 2 nanoparticles were distributed uniformly on the surface of Nano-G sheet. Specific surface area of RuO 2 -TiO 2 /Nano-G composite was higher than that of TiO 2 /Nano-G composite and Nano-G. Electrochemical performances of RuO 2 -TiO 2 /Nano-G anode were investigated by cyclic voltammetry, electrochemical impedance spectroscopy. RuO 2 -TiO 2 /Nano-G anode was applied to electrochemical degradation of ceftriaxone. The generation of hydroxyl radical (OH) was measured. Results demonstrated that RuO 2 -TiO 2 /Nano-G anode displayed enhanced electrochemical degradation efficiency towards ceftriaxone and yield of OH, which is derived from the synergetic effect between RuO 2 , TiO 2 and Nano-G, which enhance the specific surface area, improve the electrochemical oxidation activity and lower the charge transfer resistance. Besides, the possible degradation intermediates and pathways of ceftriaxone sodium were identified. This study may provide a viable and promising prospect for RuO 2 -TiO 2 /Nano-G anode towards effective electrochemical degradation of antibiotics from wastewater. Copyright © 2018 Elsevier B.V. All rights reserved.

Surface-segregated monolayers: a new type of ordered monolayer for surface modification of organic semiconductors.

PubMed

Wei, Qingshuo; Tajima, Keisuke; Tong, Yujin; Ye, Shen; Hashimoto, Kazuhito

2009-12-09

We report a new type of ordered monolayer for the surface modification of organic semiconductors. Fullerene derivatives with fluorocarbon chains ([6,6]-phenyl-C(61)-buryric acid 1H,1H-perfluoro-1-alkyl ester or FC(n)) spontaneously segregated as a monolayer on the surface of a [6,6]-phenyl-C(61)-butyric acid methyl ester (PCBM) film during a spin-coating process from the mixture solutions, as confirmed by X-ray photoelectron spectroscopy (XPS). Ultraviolet photoelectron spectroscopy (UPS) showed the shift of ionization potentials (IPs) depending on the fluorocarbon chain length, indicating the formation of surface dipole moments. Surface-sensitive vibrational spectroscopy, sum frequency generation (SFG) revealed the ordered molecular orientations of the C(60) moiety in the surface FC(n) layers. The intensity of the SFG signals from FC(n) on the surface showed a clear odd-even effect when the length of the fluorocarbon chain was changed. This new concept of the surface-segregated monolayer provides a facile and versatile approach to modifying the surface of organic semiconductors and is applicable to various organic optoelectronic devices.

Nitrogen nanoinclusions in milky diamonds from Juina area, Mato Grosso State, Brazil

NASA Astrophysics Data System (ADS)

Rudloff-Grund, J.; Brenker, F. E.; Marquardt, K.; Howell, D.; Schreiber, A.; O'Reilly, S. Y.; Griffin, W. L.; Kaminsky, F. V.

2016-11-01

A unique set of diamonds with a 'milky' optical appearance from the Rio Soriso placer deposit in the Juina area, Mato Grosso, Brazil was studied by combined transmission electron microscopy (TEM) and fourier transform infrared (FTIR) spectroscopy. The main characteristics of the studied samples are large numbers of randomly distributed {111}-faceted octahedral defect nanostructures. The dislocation densities of the focused ion beam (FIB) foils are generally low. Dislocation loops are observed only around larger inclusions. The inclusion size shows a bimodal distribution and spreads around values of 20 and 200 nm. Electron energy-loss spectroscopy (EELS) and energy-dispersive X-ray (EDX) spectroscopy mapping of both subsets yield high nitrogen contents for all sealed inclusions. In cases where the nanoinclusions touch the surface of the FIB section no nitrogen signal could be detected, indicating the loss of a fluid or gas phase as the carrier of nitrogen. FTIR mapping of the same regions showed a strong correlation between structurally bound nitrogen, hydrogen and the abundance of nanoinclusions. We propose that the most likely phase included in these nanoinclusions is NH3. These nanoinclusions could be the result of a high-temperature episode or of long residence times at shallower depths and lower temperatures. Thus they might represent the last stage of the nitrogen aggregation, or they may be syngenetic trapped NH-bearing source fluids.

X-ray photoelectron spectroscopy for characterization of wood surfaces in adhesion studies

Treesearch

James F. Beecher; Charles R. Frihart

2005-01-01

X-ray photoelectron spectroscopy (XPS) is one of a set of tools that have been used to characterize wood surfaces. Among the advantages of XPS are surface sensitivity, identification of nearly all elements, and frequently, discrimination of bonding states. For these reasons, XPS seemed to be an appropriate tool to help explain the differences in bond strength under wet...

UHV AFM based colloidal probe studies of adhesive properties of VAlN hard coatings

NASA Astrophysics Data System (ADS)

Wiesing, M.; de los Arcos, T.; Grundmeier, G.

2018-01-01

The adhesion of polystyrene (PS) on V0.27Al0.29N0.44 and the related influence of the oxidation states of both surfaces was investigated using X-Ray Photoelectron Spectroscopy (XPS) and Colloidal Force Spectroscopy (CFS) in Ultra-High Vacuum (UHV). Complementary, the intimate relation between the adhesion force, the chemical structure and surface polarizability was investigated by XPS valence band spectroscopy and the calculation of non-retarded Hamaker coefficients using Lifshitz theory based on optical data as derived from Reflection Electron Energy Loss Spectroscopy (REELS) spectra. The combined electron and force spectroscopic analysis of the interaction forces disclosed quantitatively the separation of the adhesion force in van der Waals and Lewis acid-base contributions. Further, the surface polarizability of VAlN was shown to be unaffected by oxygen incorporation due to the formation of an only gradually oxidized surface comprising a range of vanadium oxidation states. In contrast, the adhesion force analysis revealed additional Lewis acid-base interactions between the oxidized and non-oxidized VAlN surfaces and carboxyl groups present in the surface of PS after an oxidative oxygen beam treatment.

Analysis of dispersive interactions at polymer/TiAlN interfaces by means of dynamic force spectroscopy.

PubMed

Wiesing, M; de Los Arcos, T; Gebhard, M; Devi, A; Grundmeier, G

2017-12-20

The structural and electronic origins of the interactions between polycarbonate and sputter deposited TiAlN were analysed using a combined electron and force spectroscopic approach. Interaction forces were measured by means of dynamic force spectroscopy and the surface polarizability was analysed by X-ray photoelectron valence band spectroscopy. It could be shown that the adhesive interactions between polycarbonate and TiAlN are governed by van der Waals forces. Different surface cleansing and oxidizing treatments were investigated and the effect of the surface chemistry on the force interactions was analysed. Intense surface oxidation resulted in a decreased adhesion force by a factor of two due to the formation of a 2 nm thick Ti 0.21 Al 0.45 O surface oxide layer. The origin of the residual adhesion forces caused by the mixed Ti 0.21 Al 0.45 O surface oxide was clarified by considering the non-retarded Hamaker coefficients as calculated by Lifshitz theory, based on optical data from Reflection Electron Energy Loss Spectroscopy. This disclosed increased dispersion forces of Ti 0.21 Al 0.45 O due to the presence of Ti(iv) ions and related Ti 3d band optical transitions.

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.

Emerging surface characterization techniques for carbon steel corrosion: a critical brief review.

PubMed

Dwivedi, D; Lepkova, K; Becker, T

2017-03-01

Carbon steel is a preferred construction material in many industrial and domestic applications, including oil and gas pipelines, where corrosion mitigation using film-forming corrosion inhibitor formulations is a widely accepted method. This review identifies surface analytical techniques that are considered suitable for analysis of thin films at metallic substrates, but are yet to be applied to analysis of carbon steel surfaces in corrosive media or treated with corrosion inhibitors. The reviewed methods include time of flight-secondary ion mass spectrometry, X-ray absorption spectroscopy methods, particle-induced X-ray emission, Rutherford backscatter spectroscopy, Auger electron spectroscopy, electron probe microanalysis, near-edge X-ray absorption fine structure spectroscopy, X-ray photoemission electron microscopy, low-energy electron diffraction, small-angle neutron scattering and neutron reflectometry, and conversion electron Moessbauer spectrometry. Advantages and limitations of the analytical methods in thin-film surface investigations are discussed. Technical parameters of nominated analytical methods are provided to assist in the selection of suitable methods for analysis of metallic substrates deposited with surface films. The challenges associated with the applications of the emerging analytical methods in corrosion science are also addressed.

Emerging surface characterization techniques for carbon steel corrosion: a critical brief review

NASA Astrophysics Data System (ADS)

Dwivedi, D.; Lepkova, K.; Becker, T.

2017-03-01

Carbon steel is a preferred construction material in many industrial and domestic applications, including oil and gas pipelines, where corrosion mitigation using film-forming corrosion inhibitor formulations is a widely accepted method. This review identifies surface analytical techniques that are considered suitable for analysis of thin films at metallic substrates, but are yet to be applied to analysis of carbon steel surfaces in corrosive media or treated with corrosion inhibitors. The reviewed methods include time of flight-secondary ion mass spectrometry, X-ray absorption spectroscopy methods, particle-induced X-ray emission, Rutherford backscatter spectroscopy, Auger electron spectroscopy, electron probe microanalysis, near-edge X-ray absorption fine structure spectroscopy, X-ray photoemission electron microscopy, low-energy electron diffraction, small-angle neutron scattering and neutron reflectometry, and conversion electron Moessbauer spectrometry. Advantages and limitations of the analytical methods in thin-film surface investigations are discussed. Technical parameters of nominated analytical methods are provided to assist in the selection of suitable methods for analysis of metallic substrates deposited with surface films. The challenges associated with the applications of the emerging analytical methods in corrosion science are also addressed.

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.

Emerging surface characterization techniques for carbon steel corrosion: a critical brief review

PubMed Central

Dwivedi, D.; Becker, T.

2017-01-01

Carbon steel is a preferred construction material in many industrial and domestic applications, including oil and gas pipelines, where corrosion mitigation using film-forming corrosion inhibitor formulations is a widely accepted method. This review identifies surface analytical techniques that are considered suitable for analysis of thin films at metallic substrates, but are yet to be applied to analysis of carbon steel surfaces in corrosive media or treated with corrosion inhibitors. The reviewed methods include time of flight-secondary ion mass spectrometry, X-ray absorption spectroscopy methods, particle-induced X-ray emission, Rutherford backscatter spectroscopy, Auger electron spectroscopy, electron probe microanalysis, near-edge X-ray absorption fine structure spectroscopy, X-ray photoemission electron microscopy, low-energy electron diffraction, small-angle neutron scattering and neutron reflectometry, and conversion electron Moessbauer spectrometry. Advantages and limitations of the analytical methods in thin-film surface investigations are discussed. Technical parameters of nominated analytical methods are provided to assist in the selection of suitable methods for analysis of metallic substrates deposited with surface films. The challenges associated with the applications of the emerging analytical methods in corrosion science are also addressed. PMID:28413351

Area-Selective Atomic Layer Deposition of SiO2 Using Acetylacetone as a Chemoselective Inhibitor in an ABC-Type Cycle

PubMed Central

2017-01-01

Area-selective atomic layer deposition (ALD) is rapidly gaining interest because of its potential application in self-aligned fabrication schemes for next-generation nanoelectronics. Here, we introduce an approach for area-selective ALD that relies on the use of chemoselective inhibitor molecules in a three-step (ABC-type) ALD cycle. A process for area-selective ALD of SiO2 was developed comprising acetylacetone inhibitor (step A), bis(diethylamino)silane precursor (step B), and O2 plasma reactant (step C) pulses. Our results show that this process allows for selective deposition of SiO2 on GeO2, SiNx, SiO2, and WO3, in the presence of Al2O3, TiO2, and HfO2 surfaces. In situ Fourier transform infrared spectroscopy experiments and density functional theory calculations underline that the selectivity of the approach stems from the chemoselective adsorption of the inhibitor. The selectivity between different oxide starting surfaces and the compatibility with plasma-assisted or ozone-based ALD are distinct features of this approach. Furthermore, the approach offers the opportunity of tuning the substrate-selectivity by proper selection of inhibitor molecules. PMID:28850774

Nanostructure and surface activation of mayenite (12CaO·7Al2O3) ceramics via femtosecond laser irradiation in solvents

NASA Astrophysics Data System (ADS)

Visbal, Heidy; Hirano, Minami; Omura, Takuya; Shimizu, Masahiro; Takaishi, Taigo; Hirao, Kazuyuki

2017-07-01

Mayenite (12CaO·7Al2O3) is a highly interesting functional material due to the wide variety of its possible future applications. In this study, we used femtosecond laser irradiation in several solvents with varying polarities to increase the specific surface area of 12CaO·7Al2O3 ceramics and reduce their particle size without any structural degradation or loss of crystallinity. We observed that when femtosecond laser irradiation was applied to solvents bearing hydroxyl groups, a smaller particle size was obtained with the particle size decreasing as the polarity of the solvent increased. Using infrared spectroscopy, we confirmed the presence of hydroxyl and carbonyl surface functional groups at the surface of 12CaO·7Al2O3 ceramics after femtosecond laser irradiation. This is attributed to the direct chemical bonds breaking of the solvent via multiphoton ionization and/or tunneling ionization, followed by the Coulomb explosion and the subsequent production of ions that are adsorbed on the surfaces of 12CaO·7Al2O3 ceramics. Femtosecond laser irradiation in polar solvents with hydroxyl groups can reduce the particle size and increase the specific surface area without degradation or loss of crystallinity of 12CaO·7Al2O3 ceramics. Additionally, this method can be used for the surface modification and introduction of functional groups on the 12CaO·7Al2O3 ceramics surface.

Characterization of iron surface modified by 2-mercaptobenzothiazole self-assembled monolayers

NASA Astrophysics Data System (ADS)

Feng, Yuanyuan; Chen, Shenhao; Zhang, Honglin; Li, Ping; Wu, Ling; Guo, Wenjuan

2006-12-01

A self-assembled monolayer of 2-mercaptobenzothiazole (MBT) adsorbed on the iron surface was prepared. The films were characterized by electrochemical impedance spectroscopy (EIS), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared reflection spectroscopy (FT-IR) and scanning electron microscopy (SEM). Besides, the microcalorimetry method was utilized to study the self-assembled process on iron surface and the adsorption mechanism was discussed from the power-time curve. The results indicated that MBT was able to form a film spontaneously on iron surface and the presence of it could protect iron from corrosion effectively. However, the assembling time and the concentration influence the protection efficiency. Quantum chemical calculations, according to which adsorption mechanism was discussed, could explain the experimental results to some extent.

Interfaces of electrical contacts in organic semiconductor devices

NASA Astrophysics Data System (ADS)

Demirkan, Korhan

Progress in organic semiconductor devices relies on better understanding of interfaces as well as material development. The engineering of interfaces that exhibit low resistance, low operating voltage and long-term stability to minimize device degradation is one of the crucial requirements. Photoelectron spectroscopy is a powerful technique to study the metal-semiconductor interfaces, allowing: (i) elucidation of the energy levels of the semiconductor and the contacts that determine Schottky barrier height, (ii) inspection of electrical interactions (such as charge transfer, dipole formation, formation of induced density of states or formation of polaron/bi-polaron states) that effect the energy level alignment, (iii) determination of interfacial chemistry, and (iv) estimation of interface morphology. In this thesis, we have used photoelectron spectroscopy extensively for detailed analysis of the metal organic semiconductor interfaces. In this study, we demonstrate the use of photoelectron spectroscopy for construction of energy level diagrams and display some results related to chemical tailoring of materials for engineering interfaces with lowered Schottky barriers. Following our work on the energy level alignment of poly(p-phenyene vinylene) based organic semiconductors on various substrates [Au, indium tin oxide, Si (with native oxide) and Al (with native oxide)], we tested controlling the energy level alignment by using polar self assembled molecules (SAMs). Photoelectron spectroscopy showed that, by introducing SAMs on the Au surface, we successfully changed the effective work function of Au surface. We found that in this case, the change in the effective work function of the metal surface was not reflected as a shift in the energy levels of the organic semiconductor, as opposed to the results achieved with different substrate materials. To investigate the chemical interactions at the metal/organic interface, we studied the metallization of poly(2-methoxy-5,2'-ethyl-hexyloxy-phenylene vinylene) (MEH-PPV), polystyrene (PS) and ozone treated polystyrene (PS-O3) surfaces by thermal deposition of aluminum. Photoelectron spectroscopy showed the degree of chemical interaction between Al and each polymer, for MEH-PPV, the chemical interactions were mainly through the C-O present in the side chain of the polymer structure. The chemical interaction of Al with polystyrene was less significant, but it showed a dramatic increase after ozone treatment of the polystyrene surface (due to the formation of exposed oxygen sites). Formation of metal oxide and metal-organic compound is detected during the Al metallization of MEH-PPV and ozone-treated PS surfaces. Our results showed that the condensation of Al on polymer surfaces is highly dependent on surface reactivity. Enormous differences were observed for the condensation coefficient of Al on PS and PS-O3 surfaces. For the inert PS surface, results showed that Al atoms poorly wet the polymer surface and form distributed clusters at the surface. Results on reactive polymer surfaces suggest morphology reminiscent of a Stranski-Krastanov-type growth and high contact area. Many studies have shown that the insertion of a thin interlayer of the oxide or fluoride of alkali or alkaline metals between the low work function electrode and the organic semiconductor layers dramatically lowers the onset voltage and increases the efficiency compared to identical devices without the insulating layer. Various modes have been suggested for the mechanism of device performance enhancement. We have investigated the chemical and electrical interaction of (i) LiF with MEH-PPV, (ii) Al with MEH-PPV in the presence of a thin LiF layer at the interface, and finally (iii) the interaction of Al with LiF. AFM and XPS data showed that LiF forms island on the surface. Our data in agreement with various existing models suggested the (i) alteration in the electronic properties under applied bias, (ii) doping of the organic semiconductor, (iii) formation of metal alloy (Au-Li). In addition to the possible electrical modifications at the interface suggested previously, our data also suggest a change in the film growth on LiF modified surfaces.

Chemical splitting of multiwalled carbon nanotubes to enhance electrochemical capacitance for supercapacitors

NASA Astrophysics Data System (ADS)

Li, Xinlu; Li, Tongtao; Zhang, Xinlin; Zhong, Qineng; Li, Hongyi; Huang, Jiamu

2014-06-01

Multiwalled carbon nanotubes (MWCNTs) were chemically split and self-assembled to a flexible porous paper made of graphene oxide nanoribbons (GONRs). The morphology and microstructure of the pristine MWCNTs and GONRs were analyzed by transmission electron microscopy, scanning electron microscopy, X-ray diffraction, Raman spectroscopy and Fourier transform infrared spectroscopy. And the specific surface area and porosity structure were measured by N2 adsorption-desorption. The longitudinally split MWCNTs show an enhancement in specific capacitance from 21 F g-1 to 156 F g-1 compared with the pristine counterpart at 0.1 A g-1 in a 6 M KOH aqueous electrolytes. The electrochemical experiments prove that the chemical splitting of MWCNTs will make inner carbon layers opened and exposed to electrochemical double layers, which can effectively improve the electrochemical capacitance for supercapacitors.

Water hyacinth cellulose-based membrane for adsorption of liquid waste dyes and chromium

NASA Astrophysics Data System (ADS)

Agtasia Putri, Cintia; Yulianti, Ian; Desianna, Ika; Sholihah, Anisa; Sujarwata

2018-04-01

Water hyacinth (Eichornia crassipes) is a weed in aquatic area whose trunk contains a lot of cellulose. Cellulose contained can be used as dyes adsorbent in a form of composite membrane. This study aims to investigate the capacity of water hyacinth cellulose-based membrane to adsorb dye and Chromium (Cr) contained in liquid. The process of membrane fabrication begins with isolation of water hyacinth cellulose. The isolated cellulose powder was used to make the membrane by mixing it with polyvinyl alcohol-polyethylene glycol (PVA-PEG) with various compositions. The morphology of membrane surface was analyzed using CCD microscope. The analysis using Ultraviolet Visible Spectroscopy (UV-Vis) and Atomic Absorption Spectroscopy (AAS) indicate that the membrane with composition ratio of cellulose: PVA: PEG of 6.5: 2.5: 1 adsorb Cr up to 38.75%.

Pt monolayer shell on nitrided alloy core — A path to highly stable oxygen reduction catalyst

DOE PAGES

Hu, Jue; Kuttiyiel, Kurian A.; Sasaki, Kotaro; ...

2015-07-22

The inadequate activity and stability of Pt as a cathode catalyst under the severe operation conditions are the critical problems facing the application of the proton exchange membrane fuel cell (PEMFC). Here we report on a novel route to synthesize highly active and stable oxygen reduction catalysts by depositing Pt monolayer on a nitrided alloy core. The prepared Pt MLPdNiN/C catalyst retains 89% of the initial electrochemical surface area after 50,000 cycles between potentials 0.6 and 1.0 V. By correlating electron energy-loss spectroscopy and X-ray absorption spectroscopy analyses with electrochemical measurements, we found that the significant improvement of stability ofmore » the Pt MLPdNiN/C catalyst is caused by nitrogen doping while reducing the total precious metal loading.« less

Water Interfaces, Solvation, and Spectroscopy

NASA Astrophysics Data System (ADS)

Geissler, Phillip L.

2013-04-01

Liquid water consistently expands our appreciation of the rich statistical mechanics that can emerge from simple molecular constituents. Here I review several interrelated areas of recent work on aqueous systems that aim to explore and explain this richness by revealing molecular arrangements, their thermodynamic origins, and the timescales on which they change. Vibrational spectroscopy of OH stretching features prominently in these discussions, with an emphasis on efforts to establish connections between spectroscopic signals and statistics of intermolecular structure. For bulk solutions, the results of these efforts largely verify and enrich existing physical pictures of hydrogen-bond network connectivity, dynamics, and response. For water at interfaces, such pictures are still emerging. As an important example I discuss the solvation of small ions at the air-water interface, whose surface propensities challenge a basic understanding of how aqueous fluctuations accommodate solutes in heterogeneous environments.

Optical pumping and xenon NMR

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

Raftery, M. Daniel

1991-11-01

Nuclear Magnetic Resonance (NMR) spectroscopy of xenon has become an important tool for investigating a wide variety of materials, especially those with high surface area. The sensitivity of its chemical shift to environment, and its chemical inertness and adsorption properties make xenon a particularly useful NMR probe. This work discusses the application of optical pumping to enhance the sensitivity of xenon NMR experiments, thereby allowing them to be used in the study of systems with lower surface area. A novel method of optically-pumping 129Xe in low magnetic field below an NMR spectrometer and subsequent transfer of the gas to highmore » magnetic field is described. NMR studies of the highly polarized gas adsorbed onto powdered samples with low to moderate surface areas are now possible. For instance, NMR studies of optically-pumped xenon adsorbed onto polyacrylic acid show that xenon has a large interaction with the surface. By modeling the low temperature data in terms of a sticking probability and the gas phase xenon-xenon interaction, the diffusion coefficient for xenon at the surface of the polymer is determined. The sensitivity enhancement afforded by optical pumping also allows the NMR observation of xenon thin films frozen onto the inner surfaces of different sample cells. The geometry of the thin films results in interesting line shapes that are due to the bulk magnetic susceptibility of xenon. Experiments are also described that combine optical pumping with optical detection for high sensitivity in low magnetic field to observe the quadrupoler evolution of 131 Xe spins at the surface of the pumping cells. In cells with macroscopic asymmetry, a residual quadrupolar interaction causes a splitting in the 131Xe NMR frequencies in bare Pyrex glass cells and cells with added hydrogen.« less

Optical pumping and xenon NMR

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

Raftery, M.D.

1991-11-01

Nuclear Magnetic Resonance (NMR) spectroscopy of xenon has become an important tool for investigating a wide variety of materials, especially those with high surface area. The sensitivity of its chemical shift to environment, and its chemical inertness and adsorption properties make xenon a particularly useful NMR probe. This work discusses the application of optical pumping to enhance the sensitivity of xenon NMR experiments, thereby allowing them to be used in the study of systems with lower surface area. A novel method of optically-pumping [sup 129]Xe in low magnetic field below an NMR spectrometer and subsequent transfer of the gas tomore » high magnetic field is described. NMR studies of the highly polarized gas adsorbed onto powdered samples with low to moderate surface areas are now possible. For instance, NMR studies of optically-pumped xenon adsorbed onto polyacrylic acid show that xenon has a large interaction with the surface. By modeling the low temperature data in terms of a sticking probability and the gas phase xenon-xenon interaction, the diffusion coefficient for xenon at the surface of the polymer is determined. The sensitivity enhancement afforded by optical pumping also allows the NMR observation of xenon thin films frozen onto the inner surfaces of different sample cells. The geometry of the thin films results in interesting line shapes that are due to the bulk magnetic susceptibility of xenon. Experiments are also described that combine optical pumping with optical detection for high sensitivity in low magnetic field to observe the quadrupoler evolution of 131 Xe spins at the surface of the pumping cells. In cells with macroscopic asymmetry, a residual quadrupolar interaction causes a splitting in the [sup 131]Xe NMR frequencies in bare Pyrex glass cells and cells with added hydrogen.« less

Heavy-metal contamination on training ranges at the Grafenwoehr Training Area, Germany

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

Zellmer, S.D.; Schneider, J.F.

1993-05-01

Large quantities of lead and other heavy metals are deposited in the environment of weapons ranges during training exercises. This study was conducted to determine the type, degree, and extent of heavy-metal contamination on selected handgun, rifle, and hand-grenade ranges at Grafenwoehr Training Area, Germany. Soil, vegetation, and surface-water samples were collected and analyzed using the inductively-coupled plasma atomic-emission spectroscopy (ICP-AES) method and the toxic characterization leaching procedure (TCLP). The ICP-AES results show that above-normal levels of lead and copper are in the surface soil at the handgun range, high concentrations of lead and copper are in the berm andmore » soil surface at the rifle range, and elevated levels of cadmium and above-normal concentrations of arsenic, copper, and zinc are present in the surface soil at the hand-grenade range. The TCLP results show that surface soils can be considered hazardous waste because of lead content at the rifle range and because of cadmium concentration at the hand-grenade range. Vegetation at the handgun and rifle ranges has above-normal concentrations of lead. At the hand-grenade range, both vegetation and surface water have high levels of cadmium. A hand-held X-ray fluorescence (XRF) spectrum analyzer was used to measure lead concentrations in soils in a field test of the method. Comparison of XRF readings with ICP-AES results for lead indicate that the accuracy and precision of the hand-held XRF unit must improve before the unit can be used as more than a screening tool. Results of this study show that heavy-metal contamination at all three ranges is limited to the surface soil; heavy metals are not being leached into the soil profile or transported into adjacent areas.« less

A hydroxyapatite coating covalently linked onto a silicone implant material.

PubMed

Furuzono, T; Sonoda, K; Tanaka, J

2001-07-01

A novel composite consisting of hydroxyapatite (HAp) microparticles covalently coupled onto a silicone sheet was developed. Initially, an acrylic acid (AAc) -grafted silicone sheet with a 16.7 microg/cm(2) surface graft density was prepared by corona-discharge treatment. The surface of sintered, spherical, carbonated HAp particles with an average diameter of 2.0 microm was subsequently modified with amino groups. The amino group surface density of the HAp particles was calculated to be approximately one amino molecule per 1.0 nm(2) of particle surface area. These samples were characterized with Fourier transform infrared spectrometry and X-ray photoelectron spectroscopy. After the formation of ammonium ionic bonds between both samples under aqueous conditions, they were reacted at 180 degrees C for 6 h in vacuo to form covalent bonds through a solid-phase condensation. The HAp particles were coupled to the AAc-grafted silicone surface by a covalent linkage. Further improvements in the adhesive and bioactive properties of the HAp-coated silicone material are expected.

Detachment strength of human osteoblasts cultured on hydroxyapatite with various surface roughness. Contribution of integrin subunits.

PubMed

Kokkinos, Petros A; Koutsoukos, Petros G; Deligianni, Despina D

2012-06-01

Hydroxyapatite (HA) has been widely used as a bone substitute in dental, maxillofacial and orthopaedic surgery and as osteoconductive bone substitute or precoating of pedicle screws and cages in spine surgery. The aim of the present study was to investigate the osteoblastic adhesion strength on HA substrata with different surface topography and biochemistry (pre-adsorption of fibronectin) after blocking of specific integrin subunits with monoclonal antibodies. Stoichiometric HA was prepared by precipitation followed by ageing and characterized by SEM, EDX, powder XRD, Raman spectroscopy, TGA, and specific surface area analysis. Human bone marrow derived osteoblasts were cultured on HA disc-shaped substrata which were sintered and polished resulting in two surface roughness grades. For attachment evaluation, cells were incubated with monoclonal antibodies and seeded for 2 h on the substrata. Cell detachment strength was determined using a rotating disc device. Cell detachment strength was surface roughness, fibronectin preadsorption and intergin subunit sensitive.

Permeable reactive barrier of surface hydrophobic granular activated carbon coupled with elemental iron for the removal of 2,4-dichlorophenol in water.

PubMed

Yang, Ji; Cao, Limei; Guo, Rui; Jia, Jinping

2010-12-15

Granular activated carbon was modified with dimethyl dichlorosilane to improve its surface hydrophobicity, and therefore to improve the performance of permeable reactive barrier constructed with the modified granular activated carbon and elemental iron. X-ray photoelectron spectroscopy shows that the surface silicon concentration of the modified granular activated carbon is higher than that of the original one, leading to the increased surface hydrophobicity. Although the specific surface area decreased from 895 to 835 m(2)g(-1), the modified granular activated carbon could adsorb 20% more 2,4-dichlorophenol than the original one did in water. It is also proven that the permeable reactive barrier with the modified granular activated carbon is more efficient at 2,4-dichlorophenol dechlorination, in which process 2,4-dichlorophenol is transformed to 2-chlorophenol or 4-chlorophenol then to phenol, or to phenol directly. Copyright © 2010 Elsevier B.V. All rights reserved.

Ultralow surface recombination velocity in InP nanowires probed by terahertz spectroscopy.

PubMed

Joyce, Hannah J; Wong-Leung, Jennifer; Yong, Chaw-Keong; Docherty, Callum J; Paiman, Suriati; Gao, Qiang; Tan, H Hoe; Jagadish, Chennupati; Lloyd-Hughes, James; Herz, Laura M; Johnston, Michael B

2012-10-10

Using transient terahertz photoconductivity measurements, we have made noncontact, room temperature measurements of the ultrafast charge carrier dynamics in InP nanowires. InP nanowires exhibited a very long photoconductivity lifetime of over 1 ns, and carrier lifetimes were remarkably insensitive to surface states despite the large nanowire surface area-to-volume ratio. An exceptionally low surface recombination velocity (170 cm/s) was recorded at room temperature. These results suggest that InP nanowires are prime candidates for optoelectronic devices, particularly photovoltaic devices, without the need for surface passivation. We found that the carrier mobility is not limited by nanowire diameter but is strongly limited by the presence of planar crystallographic defects such as stacking faults in these predominantly wurtzite nanowires. These findings show the great potential of very narrow InP nanowires for electronic devices but indicate that improvements in the crystallographic uniformity of InP nanowires will be critical for future nanowire device engineering.