Wearable strain sensors based on thin graphite films for human activity monitoring

NASA Astrophysics Data System (ADS)

Saito, Takanari; Kihara, Yusuke; Shirakashi, Jun-ichi

2017-12-01

Wearable health-monitoring devices have attracted increasing attention in disease diagnosis and health assessment. In many cases, such devices have been prepared by complicated multistep procedures which result in the waste of materials and require expensive facilities. In this study, we focused on pyrolytic graphite sheet (PGS), which is a low-cost, simple, and flexible material, used as wearable devices for monitoring human activity. We investigated wearable devices based on PGSs for the observation of elbow and finger motions. The thin graphite films were fabricated by cutting small films from PGSs. The wearable devices were then made from the thin graphite films assembled on a commercially available rubber glove. The human motions could be observed using the wearable devices. Therefore, these results suggested that the wearable devices based on thin graphite films may broaden their application in cost-effective wearable electronics for the observation of human activity.

Fabrication of novel coated pyrolytic graphite electrodes for the selective nano-level monitoring of Cd²⁺ ions in biological and environmental samples using polymeric membrane of newly synthesized macrocycle.

PubMed

Sahani, Manoj Kumar; Singh, A K; Jain, A K; Upadhyay, Anjali; Kumar, Amit; Singh, Udai P; Narang, Shikha

2015-02-20

Novel 5-amino-1,3,4-thiadiazole-2-thiol unit based macrocyclic ionophore 5,11,17-trithia-1,3,7,9,13,15,19,20,21-nonaazatetracyclo[14.2.1.1(4,7).1(10,13)]henicosa-4(20),10(21),16(19)-triene-6,12,18-trithione (M1), was synthesized and characterized. Preliminary studies on M1 have showed that it has more the affinity toward Cd(2+) ion. Thus, the macrocyclic ionophore (M1) was used as electroactive material in the fabrication of PVC-membrane electrodes such as polymeric membrane electrode (PME), coated graphite electrode (CGE) and coated pyrolytic graphite electrode (CPGE) were prepared and its performance characteristic were compared with. The electroanalytical studies performed on PME, CGE and CPGE revealed that CPGE having membrane composition M1:PVC:1-CN:NaTPB in the ratio of 7:37:54:2 exhibits the best potentiometric characteristics in terms of detection limit of 7.58×10(-9) mol L(-1), Nernstian slope of 29.6 mV decade(-1) of activity. The sensor was found to be independent of pH in the range 2.5-8.5. The sensor showed a fast response time of 10s and could be used over a period of 4 months without any significant divergence in its potentiometric characteristics. The sensor has been employed for monitoring of the Cd(2+) ion in real samples and also used as an indicator electrode in the potentiometric titration of Cd(2+) ion with EDTA. Copyright © 2014. Published by Elsevier B.V.

Producing graphite with desired properties

NASA Technical Reports Server (NTRS)

Dickinson, J. M.; Imprescia, R. J.; Reiswig, R. D.; Smith, M. C.

1971-01-01

Isotropic or anisotropic graphite is synthesized with precise control of particle size, distribution, and shape. The isotropic graphites are nearly perfectly isotropic, with thermal expansion coefficients two or three times those of ordinary graphites. The anisotropic graphites approach the anisotropy of pyrolytic graphite.

[Study on the determination of trace gallium in molybdenum-coated pyrolytic graphite tube by electrothermal absorption spectrometry].

PubMed

Huang, Yu-an; Zhou, Fang-qin; Long, Si-hua; Yang, Liu

2004-02-01

The effects on gallium atomization in the pyrolytic graphite tube imposed by different matrix modifiers and different coatings were discussed detailedly in this paper. In the presence of matrix modifier of Ni(NO3)2 the matrix interference was eliminated efficiently. The pyrolytic graphite tubes were coated differently with lanthanum, zirconium, and molybdenum to avoid producing gallium carbide. Results showed that the tube with molybdenum coating was the best. On this basis, the mechanism of gallium atomization in the molybdenum-coated pyrolytic graphite tube using Ni(NO3)2 as a matrix modifier was studied furthermore; in addition, the parameters of the operation were optimized. As a result, a new method improved in many aspects was developed to detect trace gallium in complicated sample of gangue. The outcomes of practical applications indicated that the method could satisfy the requests of analysis and that the manipulations were simple to achieve. The characteristic content, the detection limit, and the adding recoveries were 2.12 x 10(-11) g, 1.4 x 10(-10) g and 97.4%-102.7% respectively, and the relative standard deviation was less than or equal to 3.6% (n = 11).

Thermophysical properties of graphite HOPG and HAPG in the solid state and under melting (from 2000 K up to 5000 K)

NASA Astrophysics Data System (ADS)

Savvatimskiy, A. I.; Onufriev, S. V.; Konyukhov, S. A.

2017-11-01

Experiments with HOPG graphite grade showed that the melting temperature of graphite equals 4800-4900 K and that the melting of graphite is possible only at elevated pressures. The data were obtained for resistivity, specific heat and input (Joule) energy up to 5000 K. HAPG (Highly Annealing Pyrolytic Graphite) is a form of highly oriented pyrolytic graphite. HAPG specimens in the form of strips (thickness 30 microns) were placed in a cell (between two plates of glass-sapphire). The specimen temperature was measured by a high speed pyrometer. The heat of fusion for both graphite grades (heated in a confined volume) was less (and specific heat - higher) than for the case with nearly free expansion. A possible reason for the observed effects is discussed in the report.

Synthesis of gold nanoparticles on the surface of pyrolytic graphite using penicillin as a stabilizing reagent and the catalytic oxidation of α-naphthylamine

NASA Astrophysics Data System (ADS)

Song, Y. Z.; Song, Y.; Cheng, Z. P.; Zhou, J. F.; Wei, C.

2013-01-01

Electrochemical synthesis of gold nanoparticles on the surface of pyrolytic graphite using penicillin as a stabilizing reagent was proposed. The gold nanoparticles were characterized by scanning electron microscopy, cyclic voltammetry, IR spectra, UV spectra, and powder X-ray diffraction spectra. The electro-chemical catalysis of penicillin for α-naphthylamine was demonstrated.

Thermal Performance of an Annealed Pyrolytic Graphite Solar Collector

NASA Technical Reports Server (NTRS)

Jaworske, Donald A.; Hornacek, Jennifer

2002-01-01

A solar collector having the combined properties of high solar absorptance, low infrared emittance, and high thermal conductivity is needed for applications where solar energy is to be absorbed and transported for use in minisatellites. Such a solar collector may be used with a low temperature differential heat engine to provide power or with a thermal bus for thermal switching applications. One concept being considered for the solar collector is an Al2O3 cermet coating applied to a thermal conductivity enhanced polished aluminum substrate. The cermet coating provides high solar absorptance and the polished aluminum provides low infrared emittance. Annealed pyrolytic graphite embedded in the aluminum substrate provides enhanced thermal conductivity. The as-measured thermal performance of an annealed pyrolytic graphite thermal conductivity enhanced polished aluminum solar collector, coated with a cermet coating, will be presented.

Low-energy electron diffraction study of potassium adsorbed on single-crystal graphite and highly oriented pyrolytic graphite

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

Ferralis, N.; Diehl, R.D.; Pussi, K.

2004-12-15

Potassium adsorption on graphite has been a model system for the understanding of the interaction of alkali metals with surfaces. The geometries of the (2x2) structure of potassium on both single-crystal graphite (SCG) and highly oriented pyrolytic graphite (HOPG) were investigated for various preparation conditions for graphite temperatures between 55 and 140 K. In all cases, the geometry was found to consist of K atoms in the hollow sites on top of the surface. The K-graphite average perpendicular spacing is 2.79{+-}0.03 A , corresponding to an average C-K distance of 3.13{+-}0.03 A , and the spacing between graphite planes ismore » consistent with the bulk spacing of 3.35 A. No evidence was observed for a sublayer of potassium. The results of dynamical LEED studies for the clean SCG and HOPG surfaces indicate that the surface structures of both are consistent with the truncated bulk structure of graphite.« less

Surface Superstructure of Carbon Nanotubes on Highly Oriented Pyrolytic Graphite Annealed at Elevated Temperatures

NASA Astrophysics Data System (ADS)

An, Bai; Fukuyama, Seiji; Yokogawa, Kiyoshi; Yoshimura, Masamichi

1998-06-01

Carbon nanotubes deposited on highly oriented pyrolytic graphite (HOPG) are annealed in ultra high vacuum. The effect of annealing temperature on the surface morphology of the carbon nanotubes on HOPG is examined by scanning tunneling microscopy. The ring-like surface superstructure of (\\sqrt {3}× \\sqrt {3})R30° of graphite is found on the carbon nanotubes annealed above 1593 K. The tips of the carbon nanotubes are destroyed and the stacking misarrangement between the upper and the lower walls of the tube join with HOPG resulting in the superstructure.

Calibrated work function mapping by Kelvin probe force microscopy

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

AFM visualization at a single-molecule level of denaturated states of proteins on graphite.

PubMed

Barinov, Nikolay A; Prokhorov, Valery V; Dubrovin, Evgeniy V; Klinov, Dmitry V

2016-10-01

Different graphitic materials are either already used or believed to be advantageous in biomedical and biotechnological applications, e.g., as biomaterials or substrates for sensors. Most of these applications or associated important issues, such as biocompatibility, address the problem of adsorption of protein molecules and, in particular the conformational state of the adsorbed protein molecule on graphite. High-resolution AFM demonstrates highly oriented pyrolytic graphite (HOPG) induced denaturation of four proteins of blood plasma, such as ferritin, fibrinogen, human serum albumin (HSA) and immunoglobulin G (IgG), at a single molecule level. Protein denaturation is accompanied by the decrease of the heights of protein globules and spreading of the denatured protein fraction on the surface. In contrast, the modification of HOPG with the amphiphilic oligoglycine-hydrocarbon derivative monolayer preserves the native-like conformation and provides even more mild conditions for the protein adsorption than typically used mica. Protein unfolding on HOPG may have universal character for "soft" globular proteins. Copyright © 2016 Elsevier B.V. All rights reserved.

Coupling Graphene Sheets with Iron Oxide Nanoparticles for Energy Storage and Microelectronics

DTIC Science & Technology

2015-12-18

obtained from three different synthetic methods: (i) electrochemical exfoliation of highly oriented pyrolytic graphite ( HOPG ) [8], (ii) reduction of ...Fe2O3 -Graphene Sheets Graphene sheets are obtained from electrochemical exfoliation of highly oriented pyrolytic graphite ( HOPG ) flake. Two...fringes of ɤ-Fe2O3 nanoparticles in graphene sheet is shown. Typical X-ray diffraction ( XRD ) patterns of the HOPG , exfoliated graphene, PyDop1-ɤ-Fe2O3

Materials International Space Station Experiment-6 (MISSE-6) Atomic Oxygen Fluence Monitor Experiment

NASA Technical Reports Server (NTRS)

Banks, Bruce A.; Miller, Sharon K.; Waters, Deborah L.

2010-01-01

An atomic oxygen fluence monitor was flown as part of the Materials International Space Station Experiment-6 (MISSE-6). The monitor was designed to measure the accumulation of atomic oxygen fluence with time as it impinged upon the ram surface of the MISSE 6B Passive Experiment Container (PEC). This was an active experiment for which data was to be stored on a battery-powered data logger for post-flight retrieval and analysis. The atomic oxygen fluence measurement was accomplished by allowing atomic oxygen to erode two opposing wedges of pyrolytic graphite that partially covered a photodiode. As the wedges of pyrolytic graphite erode, the area of the photodiode that is illuminated by the Sun increases. The short circuit current, which is proportional to the area of illumination, was to be measured and recorded as a function of time. The short circuit current from a different photodiode, which was oriented in the same direction and had an unobstructed view of the Sun, was also to be recorded as a reference current. The ratio of the two separate recorded currents should bear a linear relationship with the accumulated atomic oxygen fluence and be independent of the intensity of solar illumination. Ground hyperthermal atomic oxygen exposure facilities were used to evaluate the linearity of the ratio of short circuit current to the atomic oxygen fluence. In flight, the current measurement circuitry failed to operate properly, thus the overall atomic oxygen mission fluence could only be estimated based on the physical erosion of the pyrolytic graphite wedges. The atomic oxygen fluence was calculated based on the knowledge of the space atomic oxygen erosion yield of pyrolytic graphite measured from samples on the MISSE 2. The atomic oxygen fluence monitor, the expected result and comparison of mission atomic oxygen fluence based on the erosion of the pyrolytic graphite and Kapton H atomic oxygen fluence witness samples are presented in this paper.

SIKA—the multiplexing cold-neutron triple-axis spectrometer at ANSTO

NASA Astrophysics Data System (ADS)

Wu, C.-M.; Deng, G.; Gardner, J. S.; Vorderwisch, P.; Li, W.-H.; Yano, S.; Peng, J.-C.; Imamovic, E.

2016-10-01

SIKA is a new cold-neutron triple-axis spectrometer receiving neutrons from the cold source CG4 of the 20MW Open Pool Australian Light-water reactor. As a state-of-the-art triple-axis spectrometer, SIKA is equipped with a large double-focusing pyrolytic graphite monochromator, a multiblade pyrolytic graphite analyser and a multi-detector system. In this paper, we present the design, functions, and capabilities of SIKA, and discuss commissioning experimental results from powder and single-crystal samples to demonstrate its performance.

Quenchable compressed graphite synthesized from neutron-irradiated highly oriented pyrolytic graphite in high pressure treatment at 1500 °C

NASA Astrophysics Data System (ADS)

Niwase, Keisuke; Terasawa, Mititaka; Honda, Shin-ichi; Niibe, Masahito; Hisakuni, Tomohiko; Iwata, Tadao; Higo, Yuji; Hirai, Takeshi; Shinmei, Toru; Ohfuji, Hiroaki; Irifune, Tetsuo

2018-04-01

The super hard material of "compressed graphite" (CG) has been reported to be formed under compression of graphite at room temperature. However, it returns to graphite under decompression. Neutron-irradiated graphite, on the other hand, is a unique material for the synthesis of a new carbon phase, as reported by the formation of an amorphous diamond by shock compression. Here, we investigate the change of structure of highly oriented pyrolytic graphite (HOPG) irradiated with neutrons to a fluence of 1.4 × 1024 n/m2 under static pressure. The neutron-irradiated HOPG sample was compressed to 15 GPa at room temperature and then the temperature was increased up to 1500 °C. X-ray diffraction, high-resolution transmission electron microscopy on the recovered sample clearly showed the formation of a significant amount of quenchable-CG with ordinary graphite. Formation of hexagonal and cubic diamonds was also confirmed. The effect of irradiation-induced defects on the synthesis of quenchable-CG under high pressure and high temperature treatment was discussed.

Transformation of shock-compressed graphite to hexagonal diamond in nanoseconds

PubMed Central

Turneaure, Stefan J.; Sharma, Surinder M.; Volz, Travis J.; Winey, J. M.; Gupta, Yogendra M.

2017-01-01

The graphite-to-diamond transformation under shock compression has been of broad scientific interest since 1961. The formation of hexagonal diamond (HD) is of particular interest because it is expected to be harder than cubic diamond and due to its use in terrestrial sciences as a marker at meteorite impact sites. However, the formation of diamond having a fully hexagonal structure continues to be questioned and remains unresolved. Using real-time (nanosecond), in situ x-ray diffraction measurements, we show unequivocally that highly oriented pyrolytic graphite, shock-compressed along the c axis to 50 GPa, transforms to highly oriented elastically strained HD with the (100)HD plane parallel to the graphite basal plane. These findings contradict recent molecular dynamics simulation results for the shock-induced graphite-to-diamond transformation and provide a benchmark for future theoretical simulations. Additionally, our results show that an earlier report of HD forming only above 170 GPa for shocked pyrolytic graphite may lead to incorrect interpretations of meteorite impact events. PMID:29098183

Transformation of shock-compressed graphite to hexagonal diamond in nanoseconds

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

Turneaure, Stefan J.; Sharma, Surinder M.; Volz, Travis J.

The graphite-to-diamond transformation under shock compression has been of broad scientific interest since 1961. The formation of hexagonal diamond (HD) is of particular interest because it is expected to be harder than cubic diamond and due to its use in terrestrial sciences as a marker at meteorite impact sites. However, the formation of diamond having a fully hexagonal structure continues to be questioned and remains unresolved. Using real-time (nanosecond), in situ x-ray diffraction measurements, we show unequivocally that highly oriented pyrolytic graphite, shock-compressed along the c axis to 50 GPa, transforms to highly oriented elastically strained HD with the (100)HDmore » plane parallel to the graphite basal plane. These findings contradict recent molecular dynamics simulation results for the shock-induced graphite-to-diamond transformation and provide a benchmark for future theoretical simulations. Additionally, our results show that an earlier report of HD forming only above 170 GPa for shocked pyrolytic graphite may lead to incorrect interpretations of meteorite impact events.« less

Transformation of shock-compressed graphite to hexagonal diamond in nanoseconds

DOE PAGES

Turneaure, Stefan J.; Sharma, Surinder M.; Volz, Travis J.; ...

2017-10-27

The graphite-to-diamond transformation under shock compression has been of broad scientific interest since 1961. The formation of hexagonal diamond (HD) is of particular interest because it is expected to be harder than cubic diamond and due to its use in terrestrial sciences as a marker at meteorite impact sites. However, the formation of diamond having a fully hexagonal structure continues to be questioned and remains unresolved. Using real-time (nanosecond), in situ x-ray diffraction measurements, we show unequivocally that highly oriented pyrolytic graphite, shock-compressed along the c axis to 50 GPa, transforms to highly oriented elastically strained HD with the (100)HDmore » plane parallel to the graphite basal plane. These findings contradict recent molecular dynamics simulation results for the shock-induced graphite-to-diamond transformation and provide a benchmark for future theoretical simulations. Additionally, our results show that an earlier report of HD forming only above 170 GPa for shocked pyrolytic graphite may lead to incorrect interpretations of meteorite impact events.« less

Structural Analysis of Pyrolytic Graphite Optics for the HiPEP Ion Thruster

NASA Technical Reports Server (NTRS)

Meckel, Nicole; Polaha, Jonathan; Juhlin, Nils

2006-01-01

The long lifetime requirements of interplanetary exploration missions is driving the need to develop long-life components for the electric propulsion thrusters that are being targeted for these missions. One of the primary life-limiting components of ion thrusters are the optics, which are continuously eroded during the operation of the thruster. Pyrolytic graphite optics are being considered for the High Power Electric Propulsion (HiPEP) ion thruster because of their very high resistance to erosion. This paper describes the structural analysis of the HiPEP pyrolytic graphite. A description of the development of the grid model, as well as the development of the effective properties and stress concentrations in the apertured area of the grids is included. An evaluation of the use of curved grids shows that the increased stiffness (compared to flat grids) prevents intergrid impact during launch, however, the residual stresses introduced by curving the grids pushes the resulting peak stresses beyond the critical stress. As a result, flat grids are recommended as the design solution. Thermally induced grid displacements during normal thruster operation are also presented.

Nitrogen: Unraveling the Secret to Stable Carbon-Supported Pt-Alloy Electrocatalysts

DTIC Science & Technology

2013-10-01

materials reveal broad N1s spectra, indicative of formation of multiple functionalities including but not limited to pyridinic, graphitic and pyrrolic ...network along with nitrogen substitutional defects, while high-dosage increases vacancy agglomerations and pyridinic and pyrrolic nitrogen defects...Article Online highly oriented pyrolytic graphite (HOPG) surface. Simulated defects included pyridinic (Npyridinic), pyrrolic (Npyrrolic), graphitic

Preparation of pyrolytic carbon coating on graphite for inhibiting liquid fluoride salt and Xe135 penetration for molten salt breeder reactor

NASA Astrophysics Data System (ADS)

Song, Jinliang; Zhao, Yanling; He, Xiujie; Zhang, Baoliang; Xu, Li; He, Zhoutong; Zhang, DongSheng; Gao, Lina; Xia, Huihao; Zhou, Xingtai; Huai, Ping; Bai, Shuo

2015-01-01

A fixed-bed deposition method was used to prepare rough laminar pyrolytic carbon coating (RLPyC) on graphite for inhibiting liquid fluoride salt and Xe135 penetration during use in molten salt breeder reactor. The RLPyC coating possessed a graphitization degree of 44% and had good contact with graphite substrate. A high-pressure reactor was constructed to evaluate the molten salt infiltration in the isostatic graphite (IG-110, TOYO TANSO CO., LTD.) and RLPyC coated graphite under 1.01, 1.52, 3.04, 5.07 and 10.13 × 105 Pa for 12 h. Mercury injection and molten-salt infiltration experiments indicated the porosity and the salt-infiltration amount of 18.4% and 13.5 wt% under 1.52 × 105 Pa of IG-110, which was much less than 1.2% and 0.06 wt% under 10.13 × 105 Pa of the RLPyC, respectively. A vacuum device was constructed to evaluate the Xe135 penetration in the graphite. The helium diffusion coefficient of RLPyC coated graphite was 2.16 × 10-12 m2/s, much less than 1.21 × 10-6 m2/s of the graphite. Thermal cycle experiment indicated the coatings possessed excellent thermal stability. The coated graphite could effectively inhibit the liquid fluoride salt and Xe135 penetration.

Precision blackbody sources for radiometric standards.

PubMed

Sapritsky, V I; Khlevnoy, B B; Khromchenko, V B; Lisiansky, B E; Mekhontsev, S N; Melenevsky, U A; Morozova, S P; Prokhorov, A V; Samoilov, L N; Shapoval, V I; Sudarev, K A; Zelener, M F

1997-08-01

The precision blackbody sources developed at the All-Russian Institute for Optical and Physical Measurements (Moscow, Russia) and their characteristics are analyzed. The precision high-temperature graphite blackbody BB22p, large-area high-temperature pyrolytic graphite blackbody BB3200pg, middle-temperature graphite blackbody BB2000, low-temperature blackbody BB300, and gallium fixed-point blackbody BB29gl and their characteristics are described.

Carbon Materials Research

DTIC Science & Technology

2006-08-01

carbon would be highly oriented pyrolytic graphite ( HOPG ), which is formed by depositing one atom at a time on a surface utilizing the pyrolysis of a... of the crystallites, and baking to 2800 K produces a polycrystalline graphite part that has high strength and conductivity. To make isotropic...pitch fibers) or flexible (Graphoil®), as well as anisotropic ( HOPG ) or isotropic ( polycrystalline graphite ). In addition, porosity, lubricity

A high-performance ternary Si composite anode material with crystal graphite core and amorphous carbon shell

NASA Astrophysics Data System (ADS)

Sui, Dong; Xie, Yuqing; Zhao, Weimin; Zhang, Hongtao; Zhou, Ying; Qin, Xiting; Ma, Yanfeng; Yang, Yong; Chen, Yongsheng

2018-04-01

Si is a promising anode material for lithium-ion batteries, but suffers from sophisticated engineering structures and complex fabrication processes that pose challenges for commercial application. Herein, a ternary Si/graphite/pyrolytic carbon (SiGC) anode material with a structure of crystal core and amorphous shell using low-cost raw materials is developed. In this ternary SiGC composite, Si component exists as nanoparticles and is spread on the surface of the core graphite flakes while the sucrose-derived pyrolytic carbon further covers the graphite/Si components as the amorphous shell. With this structure, Si together with the graphite contributes to the high specific capacity of this Si ternary material. Also the graphite serves as the supporting and conducting matrix and the amorphous shell carbon could accommodate the volume change effect of Si, reinforces the integrity of the composite architecture, and prevents the graphite and Si from direct exposing to the electrolyte. The optimized ternary SiGC composite displays high reversible specific capacity of 818 mAh g-1 at 0.1 A g-1, initial Coulombic efficiency (CE) over 80%, and excellent cycling stability at 0.5 A g-1 with 83.6% capacity retention (∼610 mAh g-1) after 300 cycles.

Microrobot with passive diamagnetic levitation for microparticle manipulations

NASA Astrophysics Data System (ADS)

Feng, Lin; Zhang, Shengyuan; Jiang, Yonggang; Zhang, Deyuan; Arai, Fumihito

2017-12-01

In this paper, an innovative microrobot with passive diamagnetic levitation is presented. Based on theoretical analysis, finite element method simulation, and experiments, the shape of pyrolytic graphite is redesigned, which improves the stability of passive diamagnetic levitation significantly. Therefore, passive diamagnetic levitation is able to be applied for 3-D control of the microrobot. Compared with the traditional microrobots driven by permanent magnets in a microfluidic chip, the microrobot made of pyrolytic graphite and driven by magnetic force has two advantages, no friction and 3-D control, which is able to expand the scope of the microrobot applications. Finally, the microrobot with passive diamagnetic levitation was demonstrated by being encapsulated in a microfluidic chip for microparticle manipulations.

SPM observation of slow highly charged ion induced nanodots on highly orientated pyrolytic graphite

NASA Astrophysics Data System (ADS)

Mitsuda, Y.; Nakamura, B. E. O'Rourke1 N.; Kanai, Y.; Ohtani, S.; Yamazaki, Y.

2007-03-01

We have observed nanodots on a highly orientated pyrolytic graphite (HOPG) surface produced by highly charged ion impacts using a scanning tunneling microscope. Previous measurements have con.rmed the dominant role of the potential energy or the incident ion charge state on the size and height of the observed nanodots. The present results extend these previous measurements to much lower kinetic energy. It appears that there is no observable influence on the lateral size of the nanodots due to the incident ion kinetic energy down to approximately 200 eV. In contrast some slight reduction in the nanodot height was observed as the kinetic energy was reduced.

Structure-Property Relationships in Surface-Modified Ceramics. NATO advanced Science Institutes, Series E: Applied Sciences, Volume 170

DTIC Science & Technology

1989-01-01

channelling and scanning electron microscopy (SEM) of highly oriented pyrolytic graphite ( HOPG ), comparative scratch testing results and some ideas on...electrode graphite , HOPG and carbon fibers also show enhanced wear resistance followoing irradiation (6), the extent of which depends upon the initial...literature dealing with damage effects and physical property changes following neutron irradiation of graphite (single and polycrystalline ) in nuclear

Pyrolytic Carbon Nanosheets for Ultrafast and Ultrastable Sodium-Ion Storage.

PubMed

Cho, Se Youn; Kang, Minjee; Choi, Jaewon; Lee, Min Eui; Yoon, Hyeon Ji; Kim, Hae Jin; Leal, Cecilia; Lee, Sungho; Jin, Hyoung-Joon; Yun, Young Soo

2018-04-01

Na-ion cointercalation in the graphite host structure in a glyme-based electrolyte represents a new possibility for using carbon-based materials (CMs) as anodes for Na-ion storage. However, local microstructures and nanoscale morphological features in CMs affect their electrochemical performances; they require intensive studies to achieve high levels of Na-ion storage performances. Here, pyrolytic carbon nanosheets (PCNs) composed of multitudinous graphitic nanocrystals are prepared from renewable bioresources by heating. In particular, PCN-2800 prepared by heating at 2800 °C has a distinctive sp 2 carbon bonding nature, crystalline domain size of ≈44.2 Å, and high electrical conductivity of ≈320 S cm -1 , presenting significantly high rate capability at 600 C (60 A g -1 ) and stable cycling behaviors over 40 000 cycles as an anode for Na-ion storage. The results of this study show the unusual graphitization behaviors of a char-type carbon precursor and exceptionally high rate and cycling performances of the resulting graphitic material, PCN-2800, even surpassing those of supercapacitors. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Online time-differential perturbed angular correlation study with an 19O beam - Residence sites of oxygen atoms in highly oriented pyrolytic graphite

NASA Astrophysics Data System (ADS)

Sato, W.; Ueno, H.; Watanabe, H.; Miyoshi, H.; Yoshimi, A.; Kameda, D.; Ito, T.; Shimada, K.; Kaihara, J.; Suda, S.; Kobayashi, Y.; Shinohara, A.; Ohkubo, Y.; Asahi, K.

2008-01-01

The online time-differential perturbed angular correlation (TDPAC) method was applied to a study of the physical states of a probe 19F, the β- decay product of 19O (t1/2 = 26.9 s), implanted in highly oriented pyrolytic graphite. The observed magnitude of the electric field gradient at the probe nucleus, ∣Vzz∣ = 2.91(17) × 1022 V m-2, suggests that the incident 19O atoms are stabilized at an interlayer position with point group C3v. Exhibiting observed TDPAC spectra having a clear sample-to-detector configuration dependence, we demonstrate the applicability of the present online method with a short-lived radioactive 19O beam.

Observation of Persistent Currents in Finely Dispersed Pyrolytic Graphite

NASA Astrophysics Data System (ADS)

Saad, M.; Gilmutdinov, I. F.; Kiiamov, A. G.; Tayurskii, D. A.; Nikitin, S. I.; Yusupov, R. V.

2018-01-01

The trapped magnetic flux in the finely ground pyrolytic graphite sample annealed at 670 K in air has been observed. Flux trapping occurs on cooling of the sample from room temperature to 10 K in a magnetic field of 1 T. The magnitude and sign of the induced trapped moment remain unchanged when the applied magnetic field is varied within ±1 T at T K. The trapped magnetic flux is manifested in the displacement of the magnetization curve relative to that of the sample cooled in zero field. Displacement magnitude gradually decreases with the temperature increase up to 350 K, not reaching zero. The set of experimental observations probably reflects the presence in the sample of a granular high-temperature superconducting phase.

Neutron transmission measurements of poly and pyrolytic graphite crystals

NASA Astrophysics Data System (ADS)

Adib, M.; Abbas, Y.; Abdel-Kawy, A.; Ashry, A.; Kilany, M.; Kenawy, M. A.

The total neutron cross-section measurements of polycrystalline graphite have been carried out in a neutron wavelength from 0.04 to 0.78 nm. This work also presents the neutron transmission measurements of pyrolytic graphite (PG) crystal in a neutron wavelength band from 0.03 to 0.50 nm, at different orientations of the PG crystal with regard to the beam direction. The measurements were performed using three time-of-flight (TOF) spectrometers installed in front of three of the ET-RR-1 reactor horizontal channels. The average value of the coherent scattering amplitude for polycrystalline graphite was calculated and found to be bcoh = (6.61 ± 0.07) fm. The behaviour of neutron transmission through the PG crystal, while oriented at different angles with regard to the beam direction, shows dips at neutron wavelengths corresponding to the reflections from (hkl) planes of hexagonal graphite structure. The positions of the observed dips are found to be in good agreement with the calculated ones. It was also found that a 40 mm thick PG crystal is quite enough to reduce the second-order contamination of the neutron beam from 2.81 to 0.04, assuming that the incident neutrons have a Maxwell distribution with neutron gas temperature 330 K.

Stability of Nanobubbles Formed at the Interface between Cold Water and Hot Highly Oriented Pyrolytic Graphite.

PubMed

An, Hongjie; Tan, Beng Hau; Zeng, Qingyun; Ohl, Claus-Dieter

2016-11-01

For the wider application of nanobubbles, a simple and reproducible nucleation process is not readily available. Here we describe a method for nucleating nanobubbles using only the most basic of conditions: depositing cold water at 4 °C on heated highly oriented pyrolytic graphite substrates. This method thus avoids the need, as in previous studies, to use secondary liquids, salts, or electrolysis to nucleate the nanobubbles and provides a pure system in which the properties of nanobubbles can be studied. The nanobubbles generated with this method are observed to survive for at least 5 days, barely changing their contact angles or heights after the first few hours. The stability of the nanobubbles in our system is discussed within the framework of some recently published theories.

Multiferroic BiFeO3 thin films and nanodots grown on highly oriented pyrolytic graphite substrates

NASA Astrophysics Data System (ADS)

Shin, Hyun Wook; Son, Jong Yeog

2017-12-01

Multiferroic BiFeO3 (BFO) thin films and nanodots are deposited on highly oriented pyrolytic graphite (HOPG) substrates via a pulsed laser deposition technique, where the HOPG surface has a honeycomb lattice structure made of carbon atoms, similar to graphene. A graphene/BFO/HOPG capacitor exhibited multiferroic properties, namely ferroelectricity (a residual polarization of 26.8 μC/cm2) and ferromagnetism (a residual magnetization of 1.1 × 10-5 emu). The BFO thin film had high domain wall energies and demonstrated switching time of approximately 82 ns. An 8-nm BFO nanodot showed a typical piezoelectric hysteresis loop with an effective residual piezoelectric constant of approximately 110 pm/V and exhibited two clearly separated current curves depending on the ferroelectric polarization direction.

Direct graphene growth from highly ordered pyrolytic graphite using pulsed Nd: YAG laser on p-Si (100) substrate at 700°c

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

Kumar, Pramod, E-mail: kumarpramod.iitd@gmail.com; Lahiri, Indranil; Mitra, Anirban

Few layer graphene was deposited on p-type Si (100) substrates by pulsed laser deposition of highly ordered pyrolytic graphite (HOPG) target at a relatively low temperature of 700 °C, without any catalytic layer. Effect of laser energy on the ability to produce the crystalline graphene was studied. It was observed that a laser energy of 220 mJ/pulse lead to form few layer graphene while higher laser energy of 440 mJ/pulse was detrimental to precipitation process. The reasons behind this observation are also discussed. Graphene samples were analyzed using Raman spectroscopy and surface morphology of graphene samples was confirmed using fieldmore » emission scanning electron microscope (FE-SEM).« less

The electrophoretic deposition of ZnO on highly oriented pyrolytic graphite

NASA Astrophysics Data System (ADS)

Ghalamboran, Milad; Jahangiri, Mojtaba; Yousefiazari, Ehsan

2017-12-01

Intensive research has been conducted on ZnO thin and thick films in recent years. Such layers, used in different electronic devices, are deposited utilizing various methods, but electrophoretic deposition (EPD) has been chosen because of the advantages like low energy consumption, economical superiority, ecofriendliness, controllability, and high deposition rate. Here, we report electrophoretically depositing ZnO layers onto highly oriented pyrolytic graphite. Well-dispersed and stable ZnO suspensions are used for the deposition of continuous and even layers of ZnO on the substrate. ZnO powder is dispersed in acetone. The electric field applied is in the 250 V/cm to 2000 V/cm range. The morphology of the deposits are studied by SEM at the different stages of the deposition process.

Electrostatic force microscopy on oriented graphite surfaces: coexistence of insulating and conducting behaviors.

PubMed

Lu, Yonghua; Muñoz, M; Steplecaru, C S; Hao, Cheng; Bai, Ming; Garcia, N; Schindler, K; Esquinazi, P

2006-08-18

We present measurements of the electric potential fluctuations on the surface of highly oriented pyrolytic graphite using electrostatic force and atomic force microscopy. Micrometric domainlike potential distributions are observed even when the sample is grounded. Such potential distributions are unexpected given the good metallic conductivity of graphite because the surface should be an equipotential. Our results indicate the coexistence of regions with "metalliclike" and "insulatinglike" behaviors showing large potential fluctuations of the order of 0.25 V. In lower quality graphite, this effect is not observed. Experiments are performed in Ar and air atmospheres.

Window for radiation detectors and the like

DOEpatents

Sparks, C.J. Jr.; Ogle, J.C.

1975-10-28

An improved x- and gamma-radiation and particle transparent window for the environment-controlling enclosure of various types of radiation and particle detectors is provided by a special graphite foil of a thickness of from about 0.1 to 1 mil. The graphite must have very parallel hexagonal planes with a mosaic spread no greater than 5$sup 0$ to have the necessary strength in thin sections to support one atmosphere or more of pressure. Such graphite is formed by hot- pressing and annealing pyrolytically deposited graphite and thereafter stripping off layers of sufficient thickness to form the window.

Atomic resolution images of graphite in air

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

Grigg, D.A.; Shedd, G.M.; Griffis, D.

One sample used for proof of operation for atomic resolution in STM is highly oriented pyrolytic graphite (HOPG). This sample has been imaged with many different STM`s obtaining similar results. Atomic resolution images of HOPG have now been obtained using an STM designed and built at the Precision Engineering Center. This paper discusses the theoretical predictions and experimental results obtained in imaging of HOPG.

Covalent Modification of Highly Ordered Pyrolytic Graphite with a Stable Organic Free Radical by Using Diazonium Chemistry.

PubMed

Seber, Gonca; Rudnev, Alexander V; Droghetti, Andrea; Rungger, Ivan; Veciana, Jaume; Mas-Torrent, Marta; Rovira, Concepció; Crivillers, Núria

2017-01-26

A novel, persistent, electrochemically active perchlorinated triphenylmethyl (PTM) radical with a diazonium functionality has been covalently attached to highly ordered pyrolytic graphite (HOPG) by electrografting in a single-step process. Electrochemical scanning tunneling microscopy (EC-STM) and Raman spectroscopy measurements revealed that PTM molecules had a higher tendency to covalently react at the HOPG step edges. The cross-section profiles from EC-STM images showed that there was current enhancement at the functionalized areas, which could be explained by redox-mediated electron tunneling through surface-confined redox-active molecules. Cyclic voltammetry clearly demonstrated that the intrinsic properties of the organic radical were preserved upon grafting and DFT calculations also revealed that the magnetic character of the PTM radical was preserved. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Molecular orientation of copper phthalocyanine thin films on different monolayers of fullerene on SiO{sub 2} or highly oriented pyrolytic graphite

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

Wang, Chenggong; Wang, Congcong; Liu, Xiaoliang

2015-03-23

The interface electronic structures of copper phthalocyanine (CuPc) have been studied using ultraviolet photoemission spectroscopy as different monolayers of C{sub 60} were inserted between CuPc and a SiO{sub 2} or highly ordered pyrolytic graphite (HOPG) substrate. The results show that CuPc has standing up configuration with one monolayer of C{sub 60} insertion on SiO{sub 2} while lying down on HOPG, indicating that the insertion layer propagates the CuPc-substrate interaction. Meanwhile, CuPc on more than one monolayers of C{sub 60} on different substrates show that the substrate orientation effect quickly vanished. Our study elucidates intriguing molecular interactions that manipulate molecular orientationmore » and donor-acceptor energy level alignment.« less

Nuclear fuel elements and method of making same

DOEpatents

Schweitzer, Donald G.

1992-01-01

A nuclear fuel element for a high temperature gas nuclear reactor that has an average operating temperature in excess of 2000.degree. C., and a method of making such a fuel element. The fuel element is characterized by having fissionable fuel material localized and stabilized within pores of a carbon or graphite member by melting the fissionable material to cause it to chemically react with the carbon walls of the pores. The fissionable fuel material is further stabilized and localized within the pores of the graphite member by providing one or more coatings of pyrolytic carbon or diamond surrounding the porous graphite member so that each layer defines a successive barrier against migration of the fissionable fuel from the pores, and so that the outermost layer of pyrolytic carbon or diamond forms a barrier between the fissionable material and the moderating gases used in an associated high temperature gas reactor. The method of the invention provides for making such new elements either as generally spherically elements, or as flexible filaments, or as other relatively small-sized fuel elements that are particularly suited for use in high temperature gas reactors.

Scanning tunneling microscopy of the formation, transformation, and property of oligothiophene self-organizations on graphite and gold surfaces.

PubMed

Yang, Zhi-Yong; Zhang, Hui-Min; Yan, Cun-Ji; Li, Shan-Shan; Yan, Hui-Juan; Song, Wei-Guo; Wan, Li-Jun

2007-03-06

Two alkyl-substituted dual oligothiophenes, quarterthiophene (4T)-trimethylene (tm)-octithiophene (8T) and 4T-tm-4T, were used to fabricate molecular structures on highly oriented pyrolytic graphite and Au(111) surfaces. The resulted structures were investigated by scanning tunneling microscopy. The 4T-tm-8T and 4T-tm-4T molecules self-organize into long-range ordered structures with linear and/or quasi-hexagonal patterns on highly oriented pyrolytic graphite at ambient temperature. Thermal annealing induced a phase transformation from quasi-hexagonal to linear in 4T-tm-8T adlayer. The molecules adsorbed on Au(111) surface in randomly folded and linear conformation. Based on scanning tunneling microscopy results, the structural models for different self-organizations were proposed. Scanning tunneling spectroscopy measurement showed the electronic property of individual molecules in the patterns. These results are significant in understanding the chemistry of molecular structure, including its formation, transformation, and electronic properties. They also help to fabricate oligothiophene assemblies with desired structures for future molecular devices.

Comparison of DNA-Reactive Metabolites from Nitrosamine and Styrene Using Voltammetric DNA/Microsomes Sensors

PubMed Central

Krishnan, Sadagopan; Bajrami, Besnik; Mani, Vigneshwaran; Pan, Shenmin; Rusling, James F.

2012-01-01

Voltammetric sensors made with films of polyions, double-stranded DNA and liver microsomes adsorbed layer-by-layer onto pyrolytic graphite electrodes were evaluated for reactive metabolite screening. This approach features simple, inexpensive screening without enzyme purification for applications in drug or environmental chemical development. Cytochrome P450 enzymes (CYPs) in the liver microsomes were activated by an NADPH regenerating system or by electrolysis to metabolize model carcinogenic compounds nitrosamine and styrene. Reactive metabolites formed in the films were trapped as adducts with nucleobases on DNA. The DNA damage was detected by square-wave voltammetry (SWV) using Ru(bpy)32+ as a DNA-oxidation catalyst. These sensors showed a larger rate of increase in signal vs. reaction time for a highly toxic nitrosamine than for the moderately toxic styrene due to more rapid reactive metabolite-DNA adduct formation. Results were consistent with reported in vivo TD50 data for the formation of liver tumors in rats. Analogous polyion/ liver microsome films prepared on 500 nm silica nanoparticles (nanoreactors) and reacted with nitrosamine or styrene, provided LC-MS or GC analyses of metabolite formation rates that correlated well with sensor response. PMID:23100998

Determining the phonon energy of highly oriented pyrolytic graphite by scanning tunneling microscope light emission spectroscopy

NASA Astrophysics Data System (ADS)

Uehara, Yoichi; Michimata, Junichi; Watanabe, Shota; Katano, Satoshi; Inaoka, Takeshi

2018-03-01

We have investigated the scanning tunneling microscope (STM) light emission spectra of isolated single Ag nanoparticles lying on highly oriented pyrolytic graphite (HOPG). The STM light emission spectra exhibited two types of spectral structures (step-like and periodic). Comparisons of the observed structures and theoretical predictions indicate that the phonon energy of the ZO mode of HOPG [M. Mohr et al., Phys. Rev. B 76, 035439 (2007)] can be determined from the energy difference between the cutoff of STM light emission and the step in the former structure, and from the period of the latter structure. Since the role of the Ag nanoparticles does not depend on the substrate materials, this method will enable the phonon energies of various materials to be measured by STM light emission spectroscopy. The spatial resolution is comparable to the lateral size of the individual Ag nanoparticles (that is, a few nm).

Optical motion control of maglev graphite.

PubMed

Kobayashi, Masayuki; Abe, Jiro

2012-12-26

Graphite has been known as a typical diamagnetic material and can be levitated in the strong magnetic field. Here we show that the magnetically levitating pyrolytic graphite can be moved in the arbitrary place by simple photoirradiation. It is notable that the optical motion control system described in this paper requires only NdFeB permanent magnets and light source. The optical movement is driven by photothermally induced changes in the magnetic susceptibility of the graphite. Moreover, we demonstrate that light energy can be converted into rotational kinetic energy by means of the photothermal property. We find that the levitating graphite disk rotates at over 200 rpm under the sunlight, making it possible to develop a new class of light energy conversion system.

Cyclic fatigue-crack propagation, stress-corrosion, and fracture-toughness behavior in pyrolytic carbon-coated graphite for prosthetic heart valve applications.

PubMed

Ritchie, R O; Dauskardt, R H; Yu, W K; Brendzel, A M

1990-02-01

Fracture-mechanics tests were performed to characterize the cyclic fatigue, stress-corrosion cracking, and fracture-toughness behavior of a pyrolytic carbon-coated graphite composite material used in the manufacture of cardiac valve prostheses. Testing was carried out using compact tension C(T) samples containing "atomically" sharp precracks, both in room-temperature air and principally in a simulated physiological environment of 37 degrees C Ringer's lactate solution. Under sustained (monotonic) loads, the composite exhibited resistance-curve behavior, with a fracture toughness (KIc) between 1.1 and 1.9 MPa square root of m, and subcritical stress-corrosion crack velocities (da/dt) which were a function of the stress intensity K raised to the 74th power (over the range approximately 10(-9) to over 10(-5) m/s). More importantly, contrary to common perception, under cyclic loading conditions the composite was found to display true (cyclic) fatigue failure in both environments; fatigue-crack growth rates (da/dN) were seen to be a function of the 19th power of the stress-intensity range delta K (over the range approximately 10(-11) to over 10(-8) m/cycle). As subcritical crack velocities under cyclic loading were found to be many orders of magnitude faster than those measured under equivalent monotonic loads and to occur at typically 45% lower stress-intensity levels, cyclic fatigue in pyrolytic carbon-coated graphite is reasoned to be a vital consideration in the design and life-prediction procedures of prosthetic devices manufactured from this material.

Formation mechanism of graphite hexagonal pyramids by argon plasma etching of graphite substrates

NASA Astrophysics Data System (ADS)

Glad, X.; de Poucques, L.; Bougdira, J.

2015-12-01

A new graphite crystal morphology has been recently reported, namely the graphite hexagonal pyramids (GHPs). They are hexagonally-shaped crystals with diameters ranging from 50 to 800 nm and a constant apex angle of 40°. These nanostructures are formed from graphite substrates (flexible graphite and highly ordered pyrolytic graphite) in low pressure helicon coupling radiofrequency argon plasma at 25 eV ion energy and, purportedly, due to a physical etching process. In this paper, the occurrence of peculiar crystals is shown, presenting two hexagonal orientations obtained on both types of samples, which confirms such a formation mechanism. Moreover, by applying a pretreatment step with different time durations of inductive coupling radiofrequency argon plasma, for which the incident ion energy decreases at 12 eV, uniform coverage of the surface can be achieved with an influence on the density and size of the GHPs.

Magnetotransport in two dimensional electron systems under microwave excitation and in highly oriented pyrolytic graphite

NASA Astrophysics Data System (ADS)

Ramanayaka, Aruna N.

This thesis consists of two parts. The first part considers the effect of microwave radiation on magnetotransport in high quality GaAs/AlGaAs heterostructure two dimensional electron systems. The effect of microwave (MW) radiation on electron temperature was studied by investigating the amplitude of the Shubnikov de Haas (SdH) oscillations in a regime where the cyclotron frequency o c and the MW angular frequency o satisfy 2o ≤ o c ≤ 3.5o. The results indicate negligible electron heating under modest MW photoexcitation, in agreement with theoretical predictions. Next, the effect of the polarization direction of the linearly polarized MWs on the MW induced magnetoresistance oscillation amplitude was investigated. The results demonstrate the first indications of polarization dependence of MW induced magnetoresistance oscillations. In the second part, experiments on the magnetotransport of three dimensional highly oriented pyrolytic graphite (HOPG) reveal a non-zero Berry phase for HOPG. Furthermore, a novel phase relation between oscillatory magneto- and Hall- resistances was discovered from the studies of the HOPG specimen. INDEX WORDS: Two dimensional electron systems, Magnetoresistance, Microwave induced magnetoresistance oscillations, Graphite, Quantum Hall effect, Hall effect, Resistivity rule, Shubnikov de Haas effect, Shubnikov de Haas oscillation.

Feasibility of intercalated graphite railgun armatures

NASA Technical Reports Server (NTRS)

Gaier, James R.; Gooden, Clarence E.; Yashan, Doreen; Naud, Steven

1990-01-01

Graphite intercalation compounds may provide an excellent material for the fabrication of electro-magnetic railgun armatures. As a pulse of power is fed into the armature the intercalate could be excited into the plasma state around the edges of the armature, while the bulk of the current would be carried through the graphite block. Such an armature would have the desirable characteristics of both diffuse plasma armatures and bulk conduction armatures. In addition, the highly anisotropic nature of these materials could enable the electrical and thermal conductivity to be tailored to meet the specific requirements of electromagnetic railgun armatures. Preliminary investigations were performed in an attempt to determine the feasibility of using graphite intercalation compounds as railgun armatures. Issues of fabrication, resistivity, stability, and electrical current spreading are addressed for the case of highly oriented pyrolytic graphite.

Transformation of shock-compressed graphite to hexagonal diamond in nanoseconds

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

Turneaure, Stefan J.; Sharma, Surinder M.; Volz, Travis J.

2017-10-01

The graphite-to-diamond transformation under shock compression has been of broad scientific interest since 1961. The formation of hexagonal diamond (HD) is of particular interest because it is expected to be harder than cubic diamond and due to its use in terrestrial sciences as a marker at meteorite impact sites. However, the formation of diamond having a fully hexagonal structure continues to be questioned and remains unresolved. Using real-time (nanosecond), in situ x-ray diffraction measurements, we show unequivocally that highly oriented pyrolytic graphite, shock-compressed along the c axis to 50 GPa, transforms to highly oriented elastically strained HD with the (100)HDmore » plane parallel to the graphite basal plane.« less

Surface analysis of model systems: From a metal-graphite interface to an intermetallic catalyst

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

Kwolek, Emma J.

This thesis summarizes research completed on two different model systems. In the first system, we investigate the deposition of the elemental metal dysprosium on highly-oriented pyrolytic graphite (HOPG) and its resulting nucleation and growth. The goal of this research is to better understand the metal-carbon interactions that occur on HOPG and to apply those to an array of other carbon surfaces. This insight may prove beneficial to developing and using new materials for electronic applications, magnetic applications and catalysis.

Imaging graphite in air by scanning tunneling microscopy - Role of the tip

NASA Technical Reports Server (NTRS)

Colton, R. J.; Baker, S. M.; Driscoll, R. J.; Youngquist, M. G.; Baldeschwieler, J. D.; Kaiser, W. J.

1988-01-01

Atomically resolved images of highly oriented pyrolytic graphite (HOPG) in air at point contact have been obtained. Direct contact between tip and sample or contact through a contamination layer provides a conduction mechanism in addition to the exponential tunneling mechanism responsible for scanning tunneling microscopy (STM) imaging. Current-voltage (I-V) spectra were obtained while scanning in the current imaging mode with the feedback circuit interrupted in order to study the graphite imaging mechanism. Multiple tunneling tips are probably responsible for images without the expected hexagonal or trigonal symmetry. The observations indicate that the use of HOPG for testing and calibration of STM instrumentation may be misleading.

Semiconductor cooling apparatus

NASA Technical Reports Server (NTRS)

Banks, Bruce A. (Inventor); Gaier, James R. (Inventor)

1993-01-01

Gas derived graphite fibers generated by the decomposition of an organic gas are joined with a suitable binder. This produces a high thermal conductivity composite material which passively conducts heat from a source, such as a semiconductor, to a heat sink. The fibers may be intercalated. The intercalate can be halogen or halide salt, alkaline metal, or any other species which contributes to the electrical conductivity improvement of the graphite fiber. The fibers are bundled and joined with a suitable binder to form a high thermal conductivity composite material device. The heat transfer device may also be made of intercalated highly oriented pyrolytic graphite and machined, rather than made of fibers.

Atomization from a tantalum surface in graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Gregoire, D. C.; Chakrabarti, C. L.

The mechanism of atom formation of U, V, Mo, Ni, Mn, Cu and Mg atomized from pyrolytic graphite and tantalum metal surfaces has been studied. The mechanism of atom formation for U from a graphite tube atomizer is reported for the first time. The peak absorbance for U and Cu is increased by factors of 59.7 and 2.0, respectively, whereas that of V, Mo and Ni is reduced by several orders of magnitude when they are atomized from a tantalum metal surface. The peak absorbance of Mn and Mg is not appreciably affected by the material of the atomization surface. Interaction of Mn and Mg with the graphite surface and formation of their refractory carbides was found to be negligible. Uranium forms a refractory carbide when heated from a graphite surface.

Cyclic fatigue and fracture in pyrolytic carbon-coated graphite mechanical heart-valve prostheses: role of small cracks in life prediction.

PubMed

Dauskardt, R H; Ritchie, R O; Takemoto, J K; Brendzel, A M

1994-07-01

A fracture-mechanics based study has performed to characterize the fracture toughness and rates of cyclic fatigue-crack growth of incipient flaws in prosthetic heart-valve components made of pyrolytic carbon-coated graphite. Such data are required to predict the safe structural lifetime of mechanical heart-valve prostheses using damage-tolerant analysis. Unlike previous studies where fatigue-crack propagation data were obtained using through-thickness, long cracks (approximately 2-20 mm long), growing in conventional (e.g., compact-tension) samples, experiments were performed on physically small cracks (approximately 100-600 microns long), initiated on the surface of the pyrolytic-carbon coating to simulate reality. Small-crack toughness results were found to agree closely with those measured conventionally with long cracks. However, similar to well-known observations in metal fatigue, it was found that based on the usual computations of the applied (far-field) driving force in terms of the maximum stress intensity, Kmax, small fatigue cracks grew at rates that exceeded those of long cracks at the same applied stress intensity, and displayed a negative dependency on Kmax; moreover, they grew at applied stress intensities less than the fatigue threshold value, below which long cracks are presumed dormant. To resolve this apparent discrepancy, it is shown that long and small crack results can be normalized, provided growth rates are characterized in terms of the total (near-tip) stress intensity (incorporating, for example, the effect of residual stress); with this achieved, in principle, either form of data can be used for life prediction of implant devices. Inspection of the long and small crack results reveals extensive scatter inherent in both forms of growth-rate data for the pyrolytic-carbon material.

Auger mediated positron sticking on graphene and highly oriented pyrolytic graphite

NASA Astrophysics Data System (ADS)

Chirayath, V. A.; Chrysler, M.; McDonald, A.; Lim, Z.; Shastry, K.; Gladen, R.; Fairchild, A.; Koymen, A.; Weiss, A.

Positron annihilation induced Auger electron spectroscopy (PAES) measurements on 6-8 layers graphene grown on polycrystalline copper and the measurements on a highly oriented pyrolytic graphite (HOPG) sample have indicated the presence of a bound surface state for positrons. Measurements carried out with positrons of kinetic energies lower than the electron work function for graphene or HOPG have shown emission of low energy electrons possible only through the Auger mediated positron sticking (AMPS) process. In this process the positron makes a transition from a positive energy scattering state to a bound surface state. The transition energy is coupled to a valence electron which may then have enough energy to get ejected from the sample surface. The positrons which are bound to surface state are highly localized in a direction perpendicular to surface and delocalized parallel to it which makes this process highly surface sensitive and can thus be used for characterizing graphene or graphite surfaces for open volume defects and surface impurities. The measurements have also shown an extremely large low energy tail for the C KVV Auger transition at 263eV indicative of another physical process for low energy emission. This work was supported by NSF Grant No. DMR 1508719 and DMR 1338130.

Relationship between microstructure and tribological behavior of CFRC composites

NASA Astrophysics Data System (ADS)

de Souza, Maria Aparecida Miranda; Pardini, Luiz Claudio

2017-12-01

Carbon fiber reinforced carbon (CFRC) composites were initially introduced in spacecraft propulsion area and quickly started to be applied in aircraft braking systems, replacing conventional metallic systems, thanks to their excellent tribological properties. Each company develops their own CFRC composite production system, the information is unique to each manufacturer, and little is reported in the literature. In this work, tribological characterizations of three commercial CFRC composites are performed using a pin-on-disc tribometer. The results showed that the pairs assembled with pyrolytic matrix composites of rough or smooth laminar texture with graphitization index between 18 and 40% has an average COF between 0.15 and 0.25, while the pairs assembled with mixed pairs, pyrolytic matrix and glassy matrix, or pair of glassy matrix display average COF between 0.10 and 0.15. Wear which can reach a rate 9 times higher to the tribological pair of glassy composite when compared to a pyrolytic composite.

On the fractography of overload, stress corrosion, and cyclic fatigue failures in pyrolytic-carbon materials used in prosthetic heart-valve devices.

PubMed

Ritchie, R O; Dauskardt, R H; Pennisi, F J

1992-01-01

A scanning electron microscopy study is reported of the nature and morphology of fracture surfaces in pyrocarbons commonly used for the manufacture of mechanical heart-valve prostheses. Specifically, silicon-alloyed low-temperature-isotropic (LTI)-pyrolytic carbon is examined, both as a coating on graphite and as a monolithic material, following overload, stress corrosion (static fatigue), and cyclic fatigue failures in a simulated physiological environment of 37 degrees C Ringer's solution. It is found that, in contrast to most metallic materials yet in keeping with many ceramics, there are no distinct fracture morphologies in pyro-carbons which are characteristic of a specific mode of loading; fracture surfaces appear to be identical for both catastrophic and subcritical crack growth under either sustained or cyclic loading. We conclude that caution should be used in assigning the likely cause of failure of pyrolytic carbon heart-valve components using fractographic examination.

Huyen Dinh | NREL

Science.gov Websites

.; Dinh, H.N. T. Gennett and R. O' (2013). "Nitrogen: unraveling the secret to stable carbon .; Gennett, (2011). "Tuning carbon-based fuel cell catalyst support structures via nitrogen pyrolytic graphite doped with nitrogen." J Phys Chem (C 2011 115:28); pp. 13676-13684. Dinh, H.N.; Ren

Ordered water structure at hydrophobic graphite interfaces observed by 4D, ultrafast electron crystallography

PubMed Central

Yang, Ding-Shyue; Zewail, Ahmed H.

2009-01-01

Interfacial water has unique properties in various functions. Here, using 4-dimensional (4D), ultrafast electron crystallography with atomic-scale spatial and temporal resolution, we report study of structure and dynamics of interfacial water assembly on a hydrophobic surface. Structurally, vertically stacked bilayers on highly oriented pyrolytic graphite surface were determined to be ordered, contrary to the expectation that the strong hydrogen bonding of water on hydrophobic surfaces would dominate with suppressed interfacial order. Because of its terrace morphology, graphite plays the role of a template. The dynamics is also surprising. After the excitation of graphite by an ultrafast infrared pulse, the interfacial ice structure undergoes nonequilibrium “phase transformation” identified in the hydrogen-bond network through the observation of structural isosbestic point. We provide the time scales involved, the nature of ice-graphite structural dynamics, and relevance to properties related to confined water. PMID:19246378

ICP-MS measurement of silver diffusion coefficient in graphite IG-110 between 1048K and 1284K

NASA Astrophysics Data System (ADS)

Carter, L. M.; Seelig, J. D.; Brockman, J. D.; Robertson, J. D.; Loyalka, S. K.

2018-01-01

Silver-110m has been shown to permeate intact silicon carbide and pyrolytic carbon coating layers of the TRISO fuel particles during normal High Temperature Gas-Cooled Reactor (HTGR) operational conditions. The diffusion coefficients for silver in graphite IG-110 measured using a release method designed to simulate HTGR conditions of high temperature and flowing helium in the temperature range 1048-1253 K are reported. The measurements were made using spheres milled from IG-110 graphite that were infused with silver using a pressure vessel technique. The Ag diffusion was measured using a time release technique with an ICP-MS instrument for detection. The results of this work are:

Integrated Thermal Modules for Cooling Silicon and Silicon Carbide Power Modules

DTIC Science & Technology

2007-06-11

analyses, bench tests, and motor tests comprise the program. The ITMs, in place of standard heatsinks, use a highly conductive pyrolytic graphite to...passively cool power modules. Initial results show that even simple ITMs can lower chip temperatures by 20 deg. C and 10 deg. C with engine oil and

Diffraction of real and virtual photons in a pyrolytic graphite crystal as source of intensive quasimonochromatic X-ray beam

NASA Astrophysics Data System (ADS)

Bogomazova, E. A.; Kalinin, B. N.; Naumenko, G. A.; Padalko, D. V.; Potylitsyn, A. P.; Sharafutdinov, A. F.; Vnukov, I. E.

2003-01-01

A series of experiments on the parametric X-rays radiation (PXR) generation and radiation soft component diffraction of relativistic electrons in pyrolytic graphite (PG) crystals have been carried out at the Tomsk synchrotron. It is shown that the experimental results with PG crystals are explained by the kinematic PXR theory if we take into account a contribution of the real photons diffraction (transition radiation, bremsstrahlung and PXR photons as well). The measurements of the emission spectrum of channeled electrons in the photon energy range much smaller than the characteristic energy of channeling radiation have been performed with a crystal-diffraction spectrometer. For electrons incident along the <1 1 0> axis of a silicon crystal, the radiation intensity in the energy range 30⩽ ω⩽360 keV exceeds the bremsstrahlung one almost by an order of magnitude. Different possibilities to create an effective source of the monochromatic X-ray beam based on the real and virtual photons diffraction in the PG crystals have been considered.

Voltammetric studies of hemoglobin-coated polystyrene latex bead films on pyrolytic graphite electrodes.

PubMed

Sun, Hong; Hu, Naifei

2004-08-01

A novel hemoglobin (Hb)-coated polystyrene (PS) latex bead film was deposited on pyrolytic graphite (PG) electrode surface. In the first step, positively charged Hb molecules in pH 5.0 buffers were adsorbed on the surface of negatively charged, 500 nm diameter PS latex beads bearing sulfate groups by electrostatic interaction. The aqueous dispersion of Hb-coated PS particles was then deposited on the surface of PG electrodes and, after evaporation of the solvent, Hb-PS films were formed. The Hb-PS film electrodes exhibited a pair of well-defined, quasi-reversible cyclic voltammetric (CV) peaks at about -0.36 V vs. SCE in pH 7.0 buffers, characteristic of Hb heme Fe(III)/Fe(II) redox couples. Positions of Soret absorption band of Hb-PS films suggest that Hb retains its near-native structure in the films in its dry form and in solution at medium pH. The Hb in PS films was also acted as a catalyst to catalyze electrochemical reduction of various substrates such as trichloroacetic acid (TCA), nitrite, oxygen and hydrogen peroxide.

Electrodeposition of platinum on highly oriented pyrolytic graphite. Part I: electrochemical characterization.

PubMed

Lu, Guojin; Zangari, Giovanni

2005-04-28

The electrochemical deposition of Pt on highly oriented pyrolytic graphite (HOPG) from H2PtCl6 solutions was investigated by cyclic voltammetry and chronoamperometry. The effects of deposition overpotential, H2PtCl6 concentration, supporting electrolyte, and anion additions on the deposition process were evaluated. Addition of chloride inhibits Pt deposition due to adsorption on the substrate and blocking of reduction sites, while SO4(2-) and ClO4- slightly promote Pt reduction. By comparing potentiostatic current-time transients with the Scharifker-Hills model, a transition from progressive to instantaneous nucleation was observed when increasing the deposition overpotential. Following addition of chloride anions the fit of experimental transients with the instantaneous nucleation mode improves, while the addition of SO4(2-) induces only small changes. Chloride anions strongly inhibit the reduction process, which is shifted in the cathodic direction. The above results indicate that the most appropriate conditions for growing Pt nanoparticles on HOPG with narrow size distribution are to use an H2PtCl6 solution with HCl as supporting electrolyte and to apply a high cathodic overpotential.

Electrochemical formation and characterization of Au nanostructures on a highly ordered pyrolytic graphite surface

NASA Astrophysics Data System (ADS)

Gómez, José J. Arroyo; Zubieta, Carolina; Ferullo, Ricardo M.; García, Silvana G.

2016-02-01

The electrochemical formation of Au nanoparticles on a highly ordered pyrolytic graphite (HOPG) substrate using conventional electrochemical techniques and ex-situ AFM is reported. From the potentiostatic current transients studies, the Au electrodeposition process on HOPG surfaces was described, within the potential range considered, by a model involving instantaneous nucleation and diffusion controlled 3D growth, which was corroborated by the microscopic analysis. Initially, three-dimensional (3D) hemispherical nanoparticles distributed on surface defects (step edges) of the substrate were observed, with increasing particle size at more negative potentials. The double potential pulse technique allowed the formation of rounded deposits at low deposition potentials, which tend to form lines of nuclei aligned in defined directions leading to 3D ordered structures. By choosing suitable nucleation and growth pulses, one-dimensional (1D) deposits were possible, preferentially located on step edges of the HOPG substrate. Quantum-mechanical calculations confirmed the tendency of Au atoms to join selectively on surface defects, such as the HOPG step edges, at the early stages of Au electrodeposition.

Formation of Nanocones on Highly Oriented Pyrolytic Graphite by Oxygen Plasma

PubMed Central

Vesel, Alenka; Eleršič, Kristina; Modic, Martina; Junkar, Ita; Mozetič, Miran

2014-01-01

Improvement in hemocompatibility of highly oriented pyrolytic graphite (HOPG) by formation of nanostructured surface by oxygen plasma treatment is reported. We have showed that by appropriate fine tuning of plasma and discharge parameters we are able to create nanostructured surface which is densely covered with nanocones. The size of the nanocones strongly depended on treatment time. The optimal results in terms of material hemocompatibility were obtained after treatment with oxygen plasma for 15 s, when both the nanotopography and wettability were the most favorable, since marked reduction in adhesion and activation of platelets was observed on this surface. At prolonged treatment times, the rich surface topography was lost and thus also its antithrombogenic properties. Chemical composition of the surface was always more or less the same, regardless of its morphology and height of the nanocones. Namely, on all plasma treated samples, only a few atomic percent of oxygen was found, meaning that plasma caused mostly etching, leading to changes in the surface morphology. This indicates that the main preventing mechanism against platelets adhesion was the right surface morphology. PMID:28788553

Highly sensitive protein detection by combination of atomic force microscopy fishing with charge generation and mass spectrometry analysis.

PubMed

Ivanov, Yuri D; Pleshakova, Tatyana; Malsagova, Krystina; Kozlov, Andrey; Kaysheva, Anna; Kopylov, Arthur; Izotov, Alexander; Andreeva, Elena; Kanashenko, Sergey; Usanov, Sergey; Archakov, Alexander

2014-10-01

An approach combining atomic force microscopy (AFM) fishing and mass spectrometry (MS) analysis to detect proteins at ultra-low concentrations is proposed. Fishing out protein molecules onto a highly oriented pyrolytic graphite surface coated with polytetrafluoroethylene film was carried out with and without application of an external electric field. After that they were visualized by AFM and identified by MS. It was found that injection of solution leads to charge generation in the solution, and an electric potential within the measuring cell is induced. It was demonstrated that without an external electric field in the rapid injection input of diluted protein solution the fishing is efficient, as opposed to slow fluid input. The high sensitivity of this method was demonstrated by detection of human serum albumin and human cytochrome b5 in 10(-17) -10(-18) m water solutions. It was shown that an external negative voltage applied to highly oriented pyrolytic graphite hinders the protein fishing. The efficiency of fishing with an external positive voltage was similar to that obtained without applying any voltage. © 2014 FEBS.

Ultra-thin passivating film induced by vinylene carbonate on highly oriented pyrolytic graphite negative electrode in lithium-ion cell

NASA Astrophysics Data System (ADS)

Matsuoka, O.; Hiwara, A.; Omi, T.; Toriida, M.; Hayashi, T.; Tanaka, C.; Saito, Y.; Ishida, T.; Tan, H.; Ono, S. S.; Yamamoto, S.

We investigated the influence of vinylene carbonate, as an additive molecule, on the decomposition phenomena of electrolyte solution [ethylene carbonate (EC)—ethyl methyl carbonate (EMC) (1:2 by volume) containing 1 M LiPF 6] on a highly oriented pyrolytic graphite (HOPG) negative electrode by using cyclic voltammetry (CV) and atomic force microscopy (AFM). Vinylene carbonate deactivated reactive sites (e.g. radicals and oxides at the defects and the edge of carbon layer) on the cleaved surface of the HOPG negative electrode, and prevented further decomposition of the other solvents there. Further, vinylene carbonate induced an ultra-thin film (less than 1.0 nm in thickness) on the terrace of the basal plane of the HOPG negative electrode, and this film suppressed the decomposition of electrolyte solution on the terraces of the basal plane. We consider that this ultra-thin passivating film is composed of a reduction product of vinylene carbonate (VC), and might have a polymer structure. These induced effects might explain how VC improves the life performance of lithium-ion cells.

Self-assembled monolayers of shape-persistent macrocycles on graphite: interior design and conformational polymorphism.

PubMed

Vollmeyer, Joscha; Eberhagen, Friederike; Höger, Sigurd; Jester, Stefan-S

2014-01-01

Three shape-persistent naphthylene-phenylene-acetylene macrocycles of identical backbone structures and extraannular substitution patterns but different (empty, apolar, polar) nanopore fillings are self-assembled at the solid/liquid interface of highly oriented pyrolytic graphite and 1,2,4-trichlorobenzene. Submolecularly resolved images of the resulting two-dimensional (2D) crystalline monolayer patterns are obtained by in situ scanning tunneling microscopy. A concentration-dependent conformational polymorphism is found, and open and more dense packing motifs are observed. For all three compounds alike lattice parameters are found, therefore the intermolecular macrocycle distances are mainly determined by their size and symmetry. This is an excellent example that the graphite acts as a template for the macrocycle organization independent from their specific interior.

Ion sputter textured graphite electrode plates

NASA Technical Reports Server (NTRS)

Curren, A. N.; Forman, R.; Sovey, J. S.; Wintucky, E. G. (Inventor)

1983-01-01

A specially textured surface of pyrolytic graphite exhibits extremely low yields of secondary electrons and reduced numbers of reflected primary electrons after impingement of high energy primary electrons. Electrode plates of this material are used in multistage depressed collectors. An ion flux having an energy between 500 iV and 1000 iV and a current density between 1.0 mA/sq cm and 6.0 mA/sq cm produces surface roughening or texturing which is in the form of needles or spires. Such textured surfaces are especially useful as anode collector plates in high tube devices.

Room temperature stable single molecule rectifiers with graphite electrodes

NASA Astrophysics Data System (ADS)

Rungger, Ivan; Kaliginedi, V.; Droghetti, A.; Ozawa, H.; Kuzume, A.; Haga, M.; Broekmann, P.; Rudnev, A. V.

In this combined theoretical and experimental study we present new molecular electronics device characteristics of unprecedented stability at room temperature by using electrodes based on highly oriented pyrolytic graphite with covalently attached molecules. To this aim, we explore the effect of the anchoring group chemistry on the charge transport properties of graphite/molecule contacts by means of the scanning tunneling microscopy break-junction technique and ab initio simulations. The theoretical approach to evaluate the conductance is based on density functional theory calculations combined with the non-equilibrium Greens function technique, as implemented in the Smeagol electron transport code. We also demonstrate a strong bias dependence and rectification of the single molecule conductance induced by the anchoring chemistry in combination with the very low density of states of graphite around the Fermi energy. We show that the direction of tunneling current rectification can be tuned by anchoring group chemistry.

On the thermodynamic path enabling a room-temperature, laser-assisted graphite to nanodiamond transformation

NASA Astrophysics Data System (ADS)

Gorrini, F.; Cazzanelli, M.; Bazzanella, N.; Edla, R.; Gemmi, M.; Cappello, V.; David, J.; Dorigoni, C.; Bifone, A.; Miotello, A.

2016-10-01

Nanodiamonds are the subject of active research for their potential applications in nano-magnetometry, quantum optics, bioimaging and water cleaning processes. Here, we present a novel thermodynamic model that describes a graphite-liquid-diamond route for the synthesis of nanodiamonds. Its robustness is proved via the production of nanodiamonds powders at room-temperature and standard atmospheric pressure by pulsed laser ablation of pyrolytic graphite in water. The aqueous environment provides a confinement mechanism that promotes diamond nucleation and growth, and a biologically compatible medium for suspension of nanodiamonds. Moreover, we introduce a facile physico-chemical method that does not require harsh chemical or temperature conditions to remove the graphitic byproducts of the laser ablation process. A full characterization of the nanodiamonds by electron and Raman spectroscopies is reported. Our model is also corroborated by comparison with experimental data from the literature.

Phonon-assisted indirect transitions in angle-resolved photoemission spectra of graphite and graphene

NASA Astrophysics Data System (ADS)

Ayria, Pourya; Tanaka, Shin-ichiro; Nugraha, Ahmad R. T.; Dresselhaus, Mildred S.; Saito, Riichiro

2016-08-01

Indirect transitions of electrons in graphene and graphite are investigated by means of angle-resolved photoemission spectroscopy (ARPES) with several different incident photon energies and light polarizations. The theoretical calculations of the indirect transition for graphene and for a single crystal of graphite are compared with the experimental measurements for highly-oriented pyrolytic graphite and a single crystal of graphite. The dispersion relations for the transverse optical (TO) and the out-of-plane longitudinal acoustic (ZA) phonon modes of graphite and the TO phonon mode of graphene can be extracted from the inelastic ARPES intensity. We find that the TO phonon mode for k points along the Γ -K and K -M -K' directions in the Brillouin zone can be observed in the ARPES spectra of graphite and graphene by using a photon energy ≈11.1 eV. The relevant mechanism in the ARPES process for this case is the resonant indirect transition. On the other hand, the ZA phonon mode of graphite can be observed by using a photon energy ≈6.3 eV through a nonresonant indirect transition, while the ZA phonon mode of graphene within the same mechanism should not be observed.

Thermally stable laminating resins

NASA Technical Reports Server (NTRS)

Jones, R. J.; Vaughan, R. W.; Burns, E. A.

1972-01-01

Improved thermally stable laminating resins were developed based on the addition-type pyrolytic polymerization. Detailed monomer and polymer synthesis and characterization studies identified formulations which facilitate press molding processing and autoclave fabrication of glass and graphite fiber reinforced composites. A specific resin formulation, termed P10P was utilized to prepare a Courtaulds HMS reinforced simulated airfoil demonstration part by an autoclave molding process.

Fabrication and Vibration Results of 30-cm Pyrolytic Graphite Ion Optics

NASA Technical Reports Server (NTRS)

DePano, Michael K.; Hart, Stephen L.; Hanna, Andrew A.; Schneider, Analyn C.

2004-01-01

Boeing Electron Dynamic Devices, Inc. is currently developing pyrolytic graphite (PG) grids designed to operate on 30-cm NSTAR-type thrusters for the Carbon Based Ion Optics (CBIO) program. The PG technology effort of the CBIO program aims to research PG as a flightworthy material for use in dished ion optics by designing, fabricating, and performance testing 30-cm PG grids. As such, PG grid fabrication results will be discussed as will PG design considerations and how they must differ from the NSTAR molybdenum grid design. Surface characteristics and surface processing of PG will be explored relative to effects on voltage breakdown. Part of the CBIO program objectives is to understand the erosion of PG due to Xenon ion bombardment. Discussion of PG and CC sputter yields will be presented relative to molybdenum. These sputter yields will be utilized in the life modeling of carbon-based grids. Finally, vibration results of 30-cm PG grids will be presented and compared to a first-order model generated at Boeing EDD. Performance testing results of the PG grids will not be discussed in this paper as it has yet to be completed.

A scanning tunneling microscope study on an ordered mixed monolayer of bis(4,5-dihydronaphtho[1,2-d])-tetrathiafulvalene and n-tetradecane on highly oriented pyrolytic graphite.

PubMed

Zhao, Miao; Jiang, Peng; Deng, Ke; Jiang, Chao

2010-11-01

Tetrathiafulvalene (TTF) and its derivatives (TTFs) have been successfully used as building blocks to form charge transfer salts and organic semiconductors because of their special structures and rich electron nature. We report the formation of ordered mixed binary-component monolayer consisting of Bis(4,5-dihydronaphtho[1,2-d])tetrathiafulvalene (DH-TTF) and n-tetradecane (n-C14H30) molecules on highly oriented pyrolytic graphite (HOPG) surface. Scanning tunneling microscope (STM) imaging reveals that the two different kinds of molecules can spontaneously form ordered periodic phase separation structures on the substrate, in which ordered DH-TTF double- (or single-) lamella structures are periodically tuned by ordered n-C14H30 double- (or single-) lamella structures. Furthermore, scanning tunneling spectrum (STS) measurements by addressing the individual DH-TTF and n-C14H30 molecules in the ordered monolayer show that the two different kinds of molecules exhibit completely different I(V) characters on the HOPG substrate. The modulated arrangement of the TTF derivative by insulating molecules opens a possible route to construct organic conducting molecule ribbons for potential application in nanodevices.

Atomic Oxygen Erosion Yield Predictive Tool for Spacecraft Polymers in Low Earth Orbit

NASA Technical Reports Server (NTRS)

Bank, Bruce A.; de Groh, Kim K.; Backus, Jane A.

2008-01-01

A predictive tool was developed to estimate the low Earth orbit (LEO) atomic oxygen erosion yield of polymers based on the results of the Polymer Erosion and Contamination Experiment (PEACE) Polymers experiment flown as part of the Materials International Space Station Experiment 2 (MISSE 2). The MISSE 2 PEACE experiment accurately measured the erosion yield of a wide variety of polymers and pyrolytic graphite. The 40 different materials tested were selected specifically to represent a variety of polymers used in space as well as a wide variety of polymer chemical structures. The resulting erosion yield data was used to develop a predictive tool which utilizes chemical structure and physical properties of polymers that can be measured in ground laboratory testing to predict the in-space atomic oxygen erosion yield of a polymer. The properties include chemical structure, bonding information, density and ash content. The resulting predictive tool has a correlation coefficient of 0.914 when compared with actual MISSE 2 space data for 38 polymers and pyrolytic graphite. The intent of the predictive tool is to be able to make estimates of atomic oxygen erosion yields for new polymers without requiring expensive and time consumptive in-space testing.

Nanoscale electrochemical patterning reveals the active sites for catechol oxidation at graphite surfaces.

PubMed

Patel, Anisha N; McKelvey, Kim; Unwin, Patrick R

2012-12-19

Graphite-based electrodes (graphite, graphene, and nanotubes) are used widely in electrochemistry, and there is a long-standing view that graphite step edges are needed to catalyze many reactions, with the basal surface considered to be inert. In the present work, this model was tested directly for the first time using scanning electrochemical cell microscopy reactive patterning and shown to be incorrect. For the electro-oxidation of dopamine as a model process, the reaction rate was measured at high spatial resolution across a surface of highly oriented pyrolytic graphite. Oxidation products left behind in a pattern defined by the scanned electrochemical cell served as surface-site markers, allowing the electrochemical activity to be correlated directly with the graphite structure on the nanoscale. This process produced tens of thousands of electrochemical measurements at different locations across the basal surface, unambiguously revealing it to be highly electrochemically active, with step edges providing no enhanced activity. This new model of graphite electrodes has significant implications for the design of carbon-based biosensors, and the results are additionally important for understanding electrochemical processes on related sp(2)-hybridized materials such as pristine graphene and nanotubes.

Pyrolytic Carbon Coatings on Aligned Carbon Nanotube Assemblies and Fabrication of Advanced Carbon Nanotube/Carbon Composites

NASA Astrophysics Data System (ADS)

Faraji, Shaghayegh

Chemical vapor deposition (CVD) is a technique used to create a pyrolytic carbon (PyC) matrix around fibrous preforms in carbon/carbon (C/C) composites. Due to difficulties in producing three-dimensional carbon nanotube (CNT) assemblies, use of nanotubes in CVD fabricated CNT/C composites is limited. This dissertation describes efforts to: 1) Study the microstructure of PyC deposited on CNTs in order to understand the effect of microstructure and morphology of carbon coatings on graphitization behavior of CNT/PyC composites. This understanding helped to suggest a new approach for controlled radial growth of CNTs. 2) Evaluate the properties of CNT/PyC structures as a novel form of CNT assemblies with resilient, anisotropic and tunable properties. PyC was deposited on aligned sheets of nanotubes, drawn from spinnable CNT arras, using CVD of acetylene gas. At longer deposition times, the microstructure of PyC changed from laminar turbostratic carbon to a disordered carbon. For samples with short PyC deposition times (up to 30 minutes), deposited carbon layer rearranged during graphitization treatment and resulted in a crystalline structure where the coating and original tube walls could not be easily differentiated. In contrast, in samples with longer carbon deposition durations, carbon layers close to the surface of the coating remained disordered even after graphitization thermal treatment. Understanding the effect of PyC microstructure transition on graphitization behavior of CNT/PyC composites was used to develop a new method for controlled radial growth of CNTs. Carbon coated aligned CNT sheets were graphitized after each short (20 minutes) carbon deposition cycle. This prevented development of disorder carbon during subsequent PyC deposition cycles. Using cyclic-graphitization method, thick PyC coating layers were successfully graphitized into a crystalline structure that could not be differentiated from the original nanotube walls. This resulted into radial growth of CNTs, from 40 to 100 nm. Infiltration of PyC into stacked layered sheets of aligned CNTs produced resilient foam-like materials that exhibited complete recovery from 90% compressive strain. PyC coated the junctions between nanotubes and also increased their surface roughness. These changes were assumed to be responsible for the resiliency of the, once inelastic, assembly of nanotubes. While nanotubes' alignment resulted in anisotropic properties of the foams, variation in PyC infiltration duration was used to tune the foams' properties. Further investigation into properties of these foams showed promising results for their application as pressure/strain sensor and selective liquid absorbers for oil spill clean ups. Finally, CNT foams were used as novel substrates for growth of secondary nanotube assemblies. In order to achieve that, foams were first coated with alumina buffer layers using atomic layer deposition (ALD) method. New nanotubes were further grown inside the foams by CVD of acetylene over iron nano-particles. Super low density and highly porous structure of the foams allowed for diffusion of catalyst along with growth gasses into their bulk, which resulted in growth of secondary nanotubes throughout the thickness of the foams. The thickness of the alumina buffer layer was shown to influence CNT nucleation density and growth uniformity across the thickness of the foams. Compressive mechanical testing of the foams showed an order of magnitude increase in compression strength after secondary CNT growth.

Mono- and multilayers of molecular spoked carbazole wheels on graphite

PubMed Central

Aggarwal, A Vikas; Kalle, Daniel; Höger, Sigurd

2014-01-01

Summary Self-assembled monolayers of a molecular spoked wheel (a shape-persistent macrocycle with an intraannular spoke/hub system) and its synthetic precursor are investigated by scanning tunneling microscopy (STM) at the liquid/solid interface of 1-octanoic acid and highly oriented pyrolytic graphite. The submolecularly resolved STM images reveal that the molecules indeed behave as more or less rigid objects of certain sizes and shapes – depending on their chemical structures. In addition, the images provide insight into the multilayer growth of the molecular spoked wheels (MSWs), where the first adlayer acts as a template for the commensurate adsorption of molecules in the second layer. PMID:25550744

Mono- and multilayers of molecular spoked carbazole wheels on graphite.

PubMed

Jester, Stefan-S; Aggarwal, A Vikas; Kalle, Daniel; Höger, Sigurd

2014-01-01

Self-assembled monolayers of a molecular spoked wheel (a shape-persistent macrocycle with an intraannular spoke/hub system) and its synthetic precursor are investigated by scanning tunneling microscopy (STM) at the liquid/solid interface of 1-octanoic acid and highly oriented pyrolytic graphite. The submolecularly resolved STM images reveal that the molecules indeed behave as more or less rigid objects of certain sizes and shapes - depending on their chemical structures. In addition, the images provide insight into the multilayer growth of the molecular spoked wheels (MSWs), where the first adlayer acts as a template for the commensurate adsorption of molecules in the second layer.

Vacuum-compatible, ultra-low material budget Micro-Vertex Detector of the compressed baryonic matter experiment at FAIR

NASA Astrophysics Data System (ADS)

Koziel, Michal; Amar-Youcef, Samir; Bialas, Norbert; Deveaux, Michael; Fröhlich, Ingo; Klaus, Philipp; Michel, Jan; Milanović, Borislav; Müntz, Christian; Stroth, Joachim; Tischler, Tobias; Weirich, Roland; Wiebusch, Michael

2017-02-01

The Compressed Baryonic Matter (CBM) Experiment is one of the core experiments of the future FAIR facility near Darmstadt (Germany). The fixed-target experiment will explore the phase diagram of strongly interacting matter in the regime of high net baryon densities with numerous probes, among them open charm mesons. The Micro Vertex Detector (MVD) will provide the secondary vertex resolution of ∼ 50 μm along the beam axis, contribute to the background rejection in dielectron spectroscopy, and to the reconstruction of weak decays. The detector comprises four stations placed at 5, 10, 15, and 20 cm downstream the target and inside the target vacuum. The stations will be populated with highly granular CMOS Monolithic Active Pixel Sensors, which will feature a spatial resolution of < 5 μm, a non-ionizing radiation tolerance of >1013neq /cm2, an ionizing radiation tolerance of ∼ 3 Mrad, and a readout speed of a few 10 μs/frame. This work introduces the MVD-PRESTO project, which aims at integrating a precursor of the second station of the CBM-MVD meeting the following requirements: material budget of x /X0 < 0.5 %, vacuum compatibility, double-sided sensor integration on a Thermal Pyrolytic Graphite (TPG) carrier, and heat evacuation of about 350 mW/cm2/sensor with a temperature gradient of a few K/cm.

The Erosion of Diamond and Highly Oriented Pyrolytic Graphite After 1.5 Years of Space Exposure

NASA Technical Reports Server (NTRS)

De Groh, Kim K.; Banks, Bruce A.

2018-01-01

Polymers and other oxidizable materials on the exterior of spacecraft in the low Earth orbit (LEO) space environment can be eroded due to reaction with atomic oxygen (AO). Therefore, in order to design durable spacecraft, it is important to know the LEO AO erosion yield (Ey, volume loss per incident oxygen atom) of materials susceptible to AO reaction. The Polymers Experiment was developed to determine the AO Ey of various polymers and other materials flown in ram and wake orientations in LEO. The experiment was flown as part of the Materials International Space Station Experiment 7 (MISSE 7) mission for 1.5 years on the exterior of the International Space Station (ISS). As part of the experiment, a sample containing Class 2A diamond (100 plane) and highly oriented pyrolytic graphite (HOPG, basal and edge planes) was exposed to ram AO and characterized for erosion. The materials were salt-sprayed prior to flight to provide isolated sites of AO protection. The Ey of the samples was determined through post-flight electron microscopy recession depth measurements. The experiment also included a Kapton H witness sample for AO fluence determination. This paper provides an overview of the MISSE 7 mission, a description of the flight experiment, the characterization techniques used, the mission AO fluence, and the LEO Ey results for diamond and HOPG (basal and edge planes). The data is compared to the Ey of pyrolytic graphite exposed to four years of space exposure as part of the MISSE 2 mission. The results indicate that diamond erodes, but with a very low Ey of 1.58 +/- 0.04 x 10(exp -26) cm(exp 3)/atom. The different HOPG planes displayed significantly different amounts of erosion from each other. The HOPG basal plane had an Ey of 1.05 +/- 0.08 x 10(exp -24) cm(exp 3)/atom while the edge plane had a lower Ey of only 5.38 +/- 0.90 x 10(exp -25) -cm(exp 3)/atom. The Ey data from this ISS spaceflight experiment provides valuable information for understanding of chemistry and chemical structure dependent modeling of AO erosion.

Understanding the Growth Mechanism of GaN Epitaxial Layers on Mechanically Exfoliated Graphite

NASA Astrophysics Data System (ADS)

Li, Tianbao; Liu, Chenyang; Zhang, Zhe; Yu, Bin; Dong, Hailiang; Jia, Wei; Jia, Zhigang; Yu, Chunyan; Gan, Lin; Xu, Bingshe; Jiang, Haiwei

2018-04-01

The growth mechanism of GaN epitaxial layers on mechanically exfoliated graphite is explained in detail based on classic nucleation theory. The number of defects on the graphite surface can be increased via O-plasma treatment, leading to increased nucleation density on the graphite surface. The addition of elemental Al can effectively improve the nucleation rate, which can promote the formation of dense nucleation layers and the lateral growth of GaN epitaxial layers. The surface morphologies of the nucleation layers, annealed layers and epitaxial layers were characterized by field-emission scanning electron microscopy, where the evolution of the surface morphology coincided with a 3D-to-2D growth mechanism. High-resolution transmission electron microscopy was used to characterize the microstructure of GaN. Fast Fourier transform diffraction patterns showed that cubic phase (zinc-blend structure) GaN grains were obtained using conventional GaN nucleation layers, while the hexagonal phase (wurtzite structure) GaN films were formed using AlGaN nucleation layers. Our work opens new avenues for using highly oriented pyrolytic graphite as a substrate to fabricate transferable optoelectronic devices.

Understanding the Growth Mechanism of GaN Epitaxial Layers on Mechanically Exfoliated Graphite.

PubMed

Li, Tianbao; Liu, Chenyang; Zhang, Zhe; Yu, Bin; Dong, Hailiang; Jia, Wei; Jia, Zhigang; Yu, Chunyan; Gan, Lin; Xu, Bingshe; Jiang, Haiwei

2018-04-27

The growth mechanism of GaN epitaxial layers on mechanically exfoliated graphite is explained in detail based on classic nucleation theory. The number of defects on the graphite surface can be increased via O-plasma treatment, leading to increased nucleation density on the graphite surface. The addition of elemental Al can effectively improve the nucleation rate, which can promote the formation of dense nucleation layers and the lateral growth of GaN epitaxial layers. The surface morphologies of the nucleation layers, annealed layers and epitaxial layers were characterized by field-emission scanning electron microscopy, where the evolution of the surface morphology coincided with a 3D-to-2D growth mechanism. High-resolution transmission electron microscopy was used to characterize the microstructure of GaN. Fast Fourier transform diffraction patterns showed that cubic phase (zinc-blend structure) GaN grains were obtained using conventional GaN nucleation layers, while the hexagonal phase (wurtzite structure) GaN films were formed using AlGaN nucleation layers. Our work opens new avenues for using highly oriented pyrolytic graphite as a substrate to fabricate transferable optoelectronic devices.

Alternate electrode materials for the SP100 reactor

NASA Astrophysics Data System (ADS)

Randich, E.

1992-05-01

This work was performed in response to a request by the Astro-Space Division of the General Electric Co. to develop alternate electrodes materials for the electrodes of the PD2 modules to be used in the SP100 thermoelectric power conversion system. Initially, the project consisted of four tasks: (1) development of a ZrB2 (C) CVD coating on SiMo substrates; (2) development of a ZrB2 (C) CVD coating on SiGe substrates; (3) development of CVI W for porous graphite electrodes; and (4) technology transfer of pertinent developed processes. The project evolved initially into developing only ZrB2 coatings on SiGe and graphite substrates, and later into developing ZrB2 coatings only on graphite substrates. Several sizes of graphite and pyrolytic carbon-coated graphite substrates were coated with ZrB2 during the project. For budgetary reasons, the project was terminated after half the allotted time had passed. Apart from the production of coated specimens for evaluation, the major accomplishment of the project was the development of the CVD processing to produce the desired coatings.

In-situ observation of the chemical erosion of graphite in the scrape-off-layer of TEXTOR

NASA Astrophysics Data System (ADS)

Philipps, V.; Vietzke, E.; Erdweg, M.

1989-04-01

A sniffer probe system has been used to investigate the chemical erosion during interaction of the TEXTOR scrape-off plasma with a pyrolytic graphite plate at temperatures up to 1400 °C. Floating potential conditions as well as 200 V bias has been applied at plasma ion fluxes of about 10 18ions/cm 2 sec.Methane formation was found to be 8 × 10 -3 CH 4/H and 1.5 × 10 -2 CD 4/D + for room temperature graphite and floating potential increasing by a factor of two at temperature around 500 °C. Biasing the graphite decreases the methane yield at room temperature and increase it in the maximum temperature range. CO formation due to chemical interaction of oxygen ions with the graphite reaches ratios between 3 and 6 × 10 -2 CO/D(H) near the limiter edge under normal TEXTOR scrape-off conditions and exceeds the chemical hydro-(deu-tero-carbon formation significantly. The results are discussed in view of the present status of hydro-(deutero-)carbon formation on graphite and carbon impurity observations made in fusion experiments.

A new oxidation based technique for artifact free TEM specimen preparation of nuclear graphite

NASA Astrophysics Data System (ADS)

Johns, Steve; Shin, Wontak; Kane, Joshua J.; Windes, William E.; Ubic, Rick; Karthik, Chinnathambi

2018-07-01

Graphite is a key component in designs of current and future nuclear reactors whose in-service lifetimes are dependent upon the mechanical performance of the graphite. Irradiation damage from fast neutrons creates lattice defects which have a dynamic effect on the microstructure and mechanical properties of graphite. Transmission electron microscopy (TEM) can offer real-time monitoring of the dynamic atomic-level response of graphite subjected to irradiation; however, conventional TEM specimen-preparation techniques, such as argon ion milling itself, damage the graphite specimen and introduce lattice defects. It is impossible to distinguish these defects from the ones created by electron or neutron irradiation. To ensure that TEM specimens are artifact-free, a new oxidation-based technique has been developed. Bulk nuclear grades of graphite (IG-110 and NBG-18) and highly oriented pyrolytic graphite (HOPG) were initially mechanically thinned to ∼60 μm. Discs 3 mm in diameter were then oxidized at temperatures between 575 °C and 625 °C in oxidizing gasses using a new jet-polisher-like set-up in order to achieve optimal oxidation conditions to create self-supporting electron-transparent TEM specimens. The quality of these oxidized specimens were established using optical and electron microscopy. Samples oxidized at 575 °C exhibited large areas of electron transparency and the corresponding lattice imaging showed no apparent damage to the graphite lattice.

A new oxidation based technique for artifact free TEM specimen preparation of nuclear graphite

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

Johns, Steve; Shin, Wontak; Kane, Joshua J.

Graphite is a key component in designs of current and future nuclear reactors whose in-service lifetimes are dependent upon the mechanical performance of the graphite. Irradiation damage from fast neutrons creates lattice defects which have a dynamic effect on the microstructure and mechanical properties of graphite. Transmission electron microscopy (TEM) can offer real-time monitoring of the dynamic atomic-level response of graphite subjected to irradiation; however, conventional TEM specimen-preparation techniques, such as argon ion milling itself, damage the graphite specimen and introduce lattice defects. It is impossible to distinguish these defects from the ones created by electron or neutron irradiation. Thus,tomore » ensure that TEM specimens are artifact-free, a new oxidation-based technique has been developed. Bulk nuclear grades of graphite (IG-110 and NBG-18) and highly oriented pyrolytic graphite (HOPG) were initially mechanically thinned to ~60μm. Discs 3mm in diameter were then oxidized at temperatures between 575°C and 625°C in oxidizing gasses using a new jet-polisher-like set-up in order to achieve optimal oxidation conditions to create self-supporting electron-transparent TEM specimens. The quality of these oxidized specimens were established using optical and electron microscopy. Samples oxidized at 575°C exhibited large areas of electron transparency and the corresponding lattice imaging showed no apparent damage to the graphite lattice.« less

A new oxidation based technique for artifact free TEM specimen preparation of nuclear graphite

DOE PAGES

Johns, Steve; Shin, Wontak; Kane, Joshua J.; ...

2018-04-03

Graphite is a key component in designs of current and future nuclear reactors whose in-service lifetimes are dependent upon the mechanical performance of the graphite. Irradiation damage from fast neutrons creates lattice defects which have a dynamic effect on the microstructure and mechanical properties of graphite. Transmission electron microscopy (TEM) can offer real-time monitoring of the dynamic atomic-level response of graphite subjected to irradiation; however, conventional TEM specimen-preparation techniques, such as argon ion milling itself, damage the graphite specimen and introduce lattice defects. It is impossible to distinguish these defects from the ones created by electron or neutron irradiation. Thus,tomore » ensure that TEM specimens are artifact-free, a new oxidation-based technique has been developed. Bulk nuclear grades of graphite (IG-110 and NBG-18) and highly oriented pyrolytic graphite (HOPG) were initially mechanically thinned to ~60μm. Discs 3mm in diameter were then oxidized at temperatures between 575°C and 625°C in oxidizing gasses using a new jet-polisher-like set-up in order to achieve optimal oxidation conditions to create self-supporting electron-transparent TEM specimens. The quality of these oxidized specimens were established using optical and electron microscopy. Samples oxidized at 575°C exhibited large areas of electron transparency and the corresponding lattice imaging showed no apparent damage to the graphite lattice.« less

Ultrafast compression of graphite observed with sub-ps time resolution diffraction on LCLS

NASA Astrophysics Data System (ADS)

Armstrong, Michael; Goncharov, A.; Crowhurst, J.; Zaug, J.; Radousky, H.; Grivickas, P.; Bastea, S.; Goldman, N.; Stavrou, E.; Belof, J.; Gleason, A.; Lee, H. J.; Nagler, R.; Holtgrewe, N.; Walter, P.; Pakaprenka, V.; Nam, I.; Granados, E.; Presher, C.; Koroglu, B.

2017-06-01

We will present ps time resolution pulsed x-ray diffraction measurements of rapidly compressed highly oriented pyrolytic graphite along its basal plane at the Materials under Extreme Conditions (MEC) sector of the Linac Coherent Light Source (LCLS). These experiments explore the possibility of rapid (<100 ps time scale) material transformations occurring under very highly anisotropic compression conditions. Under such conditions, non-equilibrium mechanisms may play a role in the transformation process. We will present experimental results and simulations which explore this possibility. This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Security, LLC under Contract DE-AC52-07NA27344.

Surface induced selective deposition of Dysprosium Polyoxometalate on HOPG surface studied by STM and STS

NASA Astrophysics Data System (ADS)

Costa Milan, David; Pinilla Cienfuegos, Elena; Cardona Serra, Salvador; Coronado Miralles, Eugenio; Untiedt Lecuona, Carlos

2013-03-01

Scanning Tunneling Microscope (STM) and scanning Tunnelling spectroscopy (STS) techniques have been used to study the Preyssler type Polyoxometalate K12[DyP5W30O110] molecules deposited on Highly Oriented Pyrolytic Graphite surface (HOPG). Chainlike arrangements of clusters containing two or three molecules, as well as different cluster sizes are observed. As many structural artifacts are present on the graphite surface, like Moiré patterns, that could look like the molecular deposits, we have studied their STS and size to ensure the presence of the POM molecules on the surface. This article shows the possibility of addressing POMs on a flat surface to obtain their electronic properties through STS.

Stretchable and flexible high-strain sensors made using carbon nanotubes and graphite films on natural rubber.

PubMed

Tadakaluru, Sreenivasulu; Thongsuwan, Wiradej; Singjai, Pisith

2014-01-06

Conventional metallic strain sensors are flexible, but they can sustain maximum strains of only ~5%, so there is a need for sensors that can bear high strains for multifunctional applications. In this study, we report stretchable and flexible high-strain sensors that consist of entangled and randomly distributed multiwall carbon nanotubes or graphite flakes on a natural rubber substrate. Carbon nanotubes/graphite flakes were sandwiched in natural rubber to produce these high-strain sensors. Using field emission scanning electron microscopy, the morphology of the films for both the carbon nanotube and graphite sensors were assessed under different strain conditions (0% and 400% strain). As the strain was increased, the films fractured, resulting in an increase in the electrical resistance of the sensor; this change was reversible. Strains of up to 246% (graphite sensor) and 620% (carbon nanotube sensor) were measured; these values are respectively ~50 and ~120 times greater than those of conventional metallic strain sensors.

Stretchable and Flexible High-Strain Sensors Made Using Carbon Nanotubes and Graphite Films on Natural Rubber

PubMed Central

Tadakaluru, Sreenivasulu; Thongsuwan, Wiradej; Singjai, Pisith

2014-01-01

Conventional metallic strain sensors are flexible, but they can sustain maximum strains of only ∼5%, so there is a need for sensors that can bear high strains for multifunctional applications. In this study, we report stretchable and flexible high-strain sensors that consist of entangled and randomly distributed multiwall carbon nanotubes or graphite flakes on a natural rubber substrate. Carbon nanotubes/graphite flakes were sandwiched in natural rubber to produce these high-strain sensors. Using field emission scanning electron microscopy, the morphology of the films for both the carbon nanotube and graphite sensors were assessed under different strain conditions (0% and 400% strain). As the strain was increased, the films fractured, resulting in an increase in the electrical resistance of the sensor; this change was reversible. Strains of up to 246% (graphite sensor) and 620% (carbon nanotube sensor) were measured; these values are respectively ∼50 and ∼120 times greater than those of conventional metallic strain sensors. PMID:24399158

One-step formation of straight nanostripes from a mammal lipid-oleamide directly on highly oriented pyrolytic graphite.

PubMed

Zhang, Renjie; Möhwald, Helmuth; Kurth, Dirk G

2009-02-17

Hierarchical nanostructures are obtained directly on highly oriented pyrolytic graphite (HOPG) by spin coating of dilute chloroform solution of 9-Z-octadecenamide (oleamide), a natural lipid with cis-CdC- conformation, existing in the cerebrospinal fluid of mammal animals and being an additive for medical use and food packaging. Straight separated nanostripes with a length of 70-300 nm exist in the topmost layer and compact nanostripes in the bottom layer contacting HOPG. Compact nanostripes have a periodicity spacing of 3.8 nm, indicating H-bonding between two rows of oleamide molecules. The orientation of the hierarchical nanostructures differs by n60 degrees+/-8 degrees (n=1 or 2), reflecting the epitaxial ordering along theHOPGsubstrate. The nanostripes are stable against annealing.Amolecular packing scheme for the nanostructures is proposed, where the -C=C bond angle in oleamide is 120 degrees and the plane of the carbon skeleton lies parallel to the HOPG substrate. Nanostripes in the topmost layer are formed from separated rows of oleamide molecules, due to the short-range surface potential of the substrate. The scheme involves direct influence ofHOPGon the orientation of oleamide molecules to form nanostripes without any purposely added saturated alkanes and H-bonds between amide groups in adjacent two rows of oleamide molecules.

Reflection of Low Energy Positrons from the Surface of Highly Oriented Pyrolytic Graphite and Single Layer Graphene.

NASA Astrophysics Data System (ADS)

Imam, S. K.; Chirayath, V. A.; Chrysler, M. D.; Fairchild, A. J.; Gladen, R. W.; Koymen, A. R.; Weiss, A. H.; UT Arlington Positron Surface Laboratory Team

A time of flight positron annihilation induced Auger electron spectrometer (TOF-PAES) was utilized to measure the reflection of positrons as a function of incident positron energy (0 to 10 eV) from the surface of highly oriented pyrolytic graphite (HOPG) and from a single layer graphene (SLG) on a Cu foil. A NaI scintillation detector was used to measure the annihilation gamma from the reflected positrons as a function of incident positron kinetic energy. The annihilation of the positrons on HOPG and SLG were simultaneously measured using another NaI detector near the sample. The Auger electrons emitted as a result of the annihilation of positrons from the surface of the sample were also measured concurrently. As the positron kinetic energy was increased, the number of reflected positrons calculated from the intensity under the annihilation gamma peak showed a steady decrease. The positronium formation measured at the sample using the gamma spectrum showed a peak at 6 eV. The intensity of the carbon KVV Auger peak showed a dip at the same energy. The correlation of the three signals, intensity of reflected positrons, positrons annihilating at the sample and the Auger intensity are discussed for both samples. This work was supported by NSF Grant No. DMR 1508719 and DMR 1338130.

Magneto-transport properties of As-implanted highly oriented pyrolytic graphite

NASA Astrophysics Data System (ADS)

de Jesus, R. F.; Camargo, B. C.; da Silva, R. R.; Kopelevich, Y.; Behar, M.; Gusmão, M. A.; Pureur, P.

2016-11-01

We report on magneto-transport experiments in a high-quality sample of highly-oriented pyrolytic graphite (HOPG). Magneto-resistance and Hall resistivity measurements were carried out in magnetic inductions up to B = 9 T applied parallel to the c-axis at fixed temperatures between T=2 K and T=12 K. The sample was submitted to three subsequent irradiations with As ions. The implanted As contents were 2.5, 5 and 10 at% at the maximum of the distribution profile. Experiments were performed after each implantation stage. Shubnikov-de Haas (SdH) oscillations were observed in both the magneto-resistance and Hall-effect measurements. Analyses of these results with fast Fourier transform (FFT) lead to fundamental frequencies and effective masses for electrons and holes that are independent of the implantation fluences. The Hall resistivity at low temperatures shows a sign reversal as a function of the field in all implanted states. We interpret the obtained results with basis on a qualitative model that supposes the existence of an extrinsic hole density associated to the defect structure of our sample. We conclude that the As implantation does not produce a semiconductor-type doping in our HOPG sample. Instead, an increase in the extrinsic hole density is likely to occur as a consequence of disorder induced by implantation.

Graphene Nanobubbles Produced by Water Splitting.

PubMed

An, Hongjie; Tan, Beng Hau; Moo, James Guo Sheng; Liu, Sheng; Pumera, Martin; Ohl, Claus-Dieter

2017-05-10

Graphene nanobubbles are of significant interest due to their ability to trap mesoscopic volumes of gas for various applications in nanoscale engineering. However, conventional protocols to produce such bubbles are relatively elaborate and require specialized equipment to subject graphite samples to high temperatures or pressures. Here, we demonstrate the formation of graphene nanobubbles between layers of highly oriented pyrolytic graphite (HOPG) with electrolysis. Although this process can also lead to the formation of gaseous surface nanobubbles on top of the substrate, the two types of bubbles can easily be distinguished using atomic force microscopy. We estimated the Young's modulus, internal pressure, and the thickness of the top membrane of the graphene nanobubbles. The hydrogen storage capacity can reach ∼5 wt % for a graphene nanobubble with a membrane that is four layers thick. The simplicity of our protocol paves the way for such graphitic nanobubbles to be utilized for energy storage and industrial applications on a wide scale.

Graphite, graphene and the flat band superconductivity

NASA Astrophysics Data System (ADS)

Volovik, G. E.

2018-04-01

Superconductivity has been observed in bilayer graphene [1,2]. The main factor, which determines the mechanism of the formation of this superconductivity is the "magic angle" of twist of two graphene layers, at which the electronic band structure becomes nearly flat. The specific role played by twist and by the band flattening, has been earlier suggested for explanations of the signatures of room-temperature superconductivity observed in the highly oriented pyrolytic graphite (HOPG), when the quasi two-dimensional interfaces between the twisted domains are present. The interface contains the periodic array of misfit dislocations (analogs of the boundaries of the unit cell of the Moire superlattice in bilayer graphene), which provide the possible source of the flat band. This demonstrates that it is high time for combination of the theoretical and experimental efforts in order to reach the reproducible room-temperature superconductivity in graphite or in similar real or artificial materials.

3-Dimensional atomic scale structure of the ionic liquid-graphite interface elucidated by AM-AFM and quantum chemical simulations

NASA Astrophysics Data System (ADS)

Page, Alister J.; Elbourne, Aaron; Stefanovic, Ryan; Addicoat, Matthew A.; Warr, Gregory G.; Voïtchovsky, Kislon; Atkin, Rob

2014-06-01

In situ amplitude modulated atomic force microscopy (AM-AFM) and quantum chemical simulations are used to resolve the structure of the highly ordered pyrolytic graphite (HOPG)-bulk propylammonium nitrate (PAN) interface with resolution comparable with that achieved for frozen ionic liquid (IL) monolayers using STM. This is the first time that (a) molecular resolution images of bulk IL-solid interfaces have been achieved, (b) the lateral structure of the IL graphite interface has been imaged for any IL, (c) AM-AFM has elucidated molecular level structure immersed in a viscous liquid and (d) it has been demonstrated that the IL structure at solid surfaces is a consequence of both thermodynamic and kinetic effects. The lateral structure of the PAN-graphite interface is highly ordered and consists of remarkably well-defined domains of a rhomboidal superstructure composed of propylammonium cations preferentially aligned along two of the three directions in the underlying graphite lattice. The nanostructure is primarily determined by the cation. Van der Waals interactions between the propylammonium chains and the surface mean that the cation is enriched in the surface layer, and is much less mobile than the anion. The presence of a heterogeneous lateral structure at an ionic liquid-solid interface has wide ranging ramifications for ionic liquid applications, including lubrication, capacitive charge storage and electrodeposition.In situ amplitude modulated atomic force microscopy (AM-AFM) and quantum chemical simulations are used to resolve the structure of the highly ordered pyrolytic graphite (HOPG)-bulk propylammonium nitrate (PAN) interface with resolution comparable with that achieved for frozen ionic liquid (IL) monolayers using STM. This is the first time that (a) molecular resolution images of bulk IL-solid interfaces have been achieved, (b) the lateral structure of the IL graphite interface has been imaged for any IL, (c) AM-AFM has elucidated molecular level structure immersed in a viscous liquid and (d) it has been demonstrated that the IL structure at solid surfaces is a consequence of both thermodynamic and kinetic effects. The lateral structure of the PAN-graphite interface is highly ordered and consists of remarkably well-defined domains of a rhomboidal superstructure composed of propylammonium cations preferentially aligned along two of the three directions in the underlying graphite lattice. The nanostructure is primarily determined by the cation. Van der Waals interactions between the propylammonium chains and the surface mean that the cation is enriched in the surface layer, and is much less mobile than the anion. The presence of a heterogeneous lateral structure at an ionic liquid-solid interface has wide ranging ramifications for ionic liquid applications, including lubrication, capacitive charge storage and electrodeposition. Electronic supplementary information (ESI) available. See DOI: 10.1039/c4nr01219d

Aqueous alteration of VHTR fuels particles under simulated geological conditions

NASA Astrophysics Data System (ADS)

Ait Chaou, Abdelouahed; Abdelouas, Abdesselam; Karakurt, Gökhan; Grambow, Bernd

2014-05-01

Very High Temperature Reactor (VHTR) fuels consist of the bistructural-isotropic (BISO) or tristructural-isotropic (TRISO)-coated particles embedded in a graphite matrix. Management of the spent fuel generated during VHTR operation would most likely be through deep geological disposal. In this framework we investigated the alteration of BISO (with pyrolytic carbon) and TRISO (with SiC) particles under geological conditions simulated by temperatures of 50 and 90 °C and in the presence of synthetic groundwater. Solid state (scanning electron microscopy (SEM), micro-Raman spectroscopy, electron probe microanalyses (EPMA) and X-ray photoelectron spectroscopy (XPS)) and solution analyses (ICP-MS, ionique chromatography (IC)) showed oxidation of both pyrolytic carbon and SiC at 90 °C. Under air this led to the formation of SiO2 and a clay-like Mg-silicate, while under reducing conditions (H2/N2 atmosphere) SiC and pyrolytic carbon were highly stable after a few months of alteration. At 50 °C, in the presence and absence of air, the alteration of the coatings was minor. In conclusion, due to their high stability in reducing conditions, HTR fuel disposal in reducing deep geological environments may constitute a viable solution for their long-term management.

Magnetic Surfaces, Thin Films, and Multilayers

DTIC Science & Technology

1992-01-01

investigations %as the cleaved ((00)I) face of highly oriented pyrolytic graphite ( HOPG ). This surface is inert in air and is easily imaged with the STM[83-86...Parkin IBM Almaden Research Center, San Jose, California, U.S.A. Herbert Hopster University of California -Irvine, Irvine, California, U.S.A. Jean...magnetic fields (typically 10 to 100 kOe). For polycrystalline samples and at normal temperatures more modest increases, typically of a factor of 2 to 10

Finite Element and Molecular Dynamics Modeling and Simulation of Thermal Properties

DTIC Science & Technology

2007-06-01

dots represent the experimental results of the normalized conductivity data ke/kf (ke is κ of the composite, kf is κ of the fluid) CNT in oil ...individual Single Walled Nanotube to four centimeters in length. [4] 6 Carbon based materials, in-plane pyrolytic graphite and diamonds, have the...conductivity of nanocomposites has not yet been achieved. A 2001 experiment studied the thermal conductivity of oil with CNT in suspension. The results

Impact of corrosion test container material in molten fluorides

DOE PAGES

Olson, Luke C.; Fuentes, Roderick E.; Martinez-Rodriguez, Michael J.; ...

2015-10-15

The effects of crucible material choice on alloy corrosion rates in immersion tests in molten LiF–NaF–KF (46.5–11.5-42 mol. %) salt held at 850 °C for 500 hrs are described. Four crucible materials were studied. Molten salt exposures of Incoloy-800H in graphite, Ni, Incoloy-800H, and pyrolytic boron nitride (PyBN) crucibles all led to weight-loss in the Incoloy-800H coupons. Alloy weight loss was ~30 times higher in the graphite and Ni crucibles in comparison to the Incoloy-800H and PyBN crucibles. It is hypothesized galvanic coupling between the alloy coupons and crucible materials contributed to the higher corrosion rates. Alloy salt immersion inmore » graphite and Ni crucibles had similar weight-loss hypothesized to occur due to the rate limiting out diffusion of Cr in the alloys to the surface where it reacts with and dissolves into the molten salt, followed by the reduction of Cr from solution at the molten salt and graphite/Ni interfaces. As a result, both the graphite and the Ni crucibles provided sinks for the Cr, in the formation of a Ni–Cr alloy in the case of the Ni crucible, and Cr carbide in the case of the graphite crucible.« less

A study of Kapton degradation under simulated shuttle environment

NASA Technical Reports Server (NTRS)

Eck, T. G.; Hoffman, R. W.

1986-01-01

A system was developed which employs a source of low energy oxygen ion to simulate the shuttle low Earth orbit environment. This source, together with diagnostic tools including surface analysis ans mass spectroscopic capability, was used to measure the dependence of ion energy of the oxygen induced CO signals from pyrolytic graphite and Kapton. For graphite the CO signal was examined at energies ranging form 4.5 to 465 eV and for Kapton from 4.5 to 188 eV. While the relative quantum yields inferred from the data are reasonably precise, there are large uncertainties in the absolute yields because of the assumptions necessary to covert the measured signal strengths to quantum yields. These assumptions are discussed in detail.

Molecular beam epitaxy growth of SrO buffer layers on graphite and graphene for the integration of complex oxides

DOE PAGES

Ahmed, Adam S.; Wen, Hua; Ohta, Taisuke; ...

2016-04-27

Here, we report the successful growth of high-quality SrO films on highly-ordered pyrolytic graphite (HOPG) and single-layer graphene by molecular beam epitaxy. The SrO layers have (001) orientation as confirmed by X-ray diffraction (XRD) while atomic force microscopy measurements show continuous pinhole-free films having rms surface roughness of <1.5 Å. Moreover, transport measurements of exfoliated graphene, after SrO deposition, show a strong dependence between the Dirac point and Sr oxidation. As a result, the SrO is leveraged as a buffer layer for more complex oxide integration via the demonstration of (001) oriented SrTiO3 grown atop a SrO/HOPG stack.

Molecular beam epitaxy growth of SrO buffer layers on graphite and graphene for the integration of complex oxides

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

Ahmed, Adam S.; Wen, Hua; Ohta, Taisuke

Here, we report the successful growth of high-quality SrO films on highly-ordered pyrolytic graphite (HOPG) and single-layer graphene by molecular beam epitaxy. The SrO layers have (001) orientation as confirmed by X-ray diffraction (XRD) while atomic force microscopy measurements show continuous pinhole-free films having rms surface roughness of <1.5 Å. Moreover, transport measurements of exfoliated graphene, after SrO deposition, show a strong dependence between the Dirac point and Sr oxidation. As a result, the SrO is leveraged as a buffer layer for more complex oxide integration via the demonstration of (001) oriented SrTiO3 grown atop a SrO/HOPG stack.

Stacked graphene nanofibers for electrochemical oxidation of DNA bases.

PubMed

Ambrosi, Adriano; Pumera, Martin

2010-08-21

In this article, we show that stacked graphene nanofibers (SGNFs) demonstrate superior electrochemical performance for oxidation of DNA bases over carbon nanotubes (CNTs). This is due to an exceptionally high number of accessible graphene sheet edges on the surface of the nanofibers when compared to carbon nanotubes, as shown by transmission electron microscopy and Raman spectroscopy. The oxidation signals of adenine, guanine, cytosine, and thymine exhibit two to four times higher currents than on CNT-based electrodes. SGNFs also exhibit higher sensitivity than do edge-plane pyrolytic graphite, glassy carbon, or graphite microparticle-based electrodes. We also demonstrate that influenza A(H1N1)-related strands can be sensitively oxidized on SGNF-based electrodes, which could therefore be applied to label-free DNA analysis.

Investigating the Co-Adsorption Behavior of Nucleic-Acid Base (Thymine and Cytosine) and Melamine at Liquid/Solid Interface

NASA Astrophysics Data System (ADS)

Zhao, Huiling; Li, Yinli; Chen, Dong; Liu, Bo

2016-12-01

The co-adsorption behavior of nucleic-acid base (thymine; cytosine) and melamine was investigated by scanning tunneling microscopy (STM) technique at liquid/solid (1-octanol/graphite) interface. STM characterization results indicate that phase separation happened after dropping the mixed solution of thymine-melamine onto highly oriented pyrolytic graphite (HOPG) surface, while the hetero-component cluster-like structure was observed when cytosine-melamine binary assembly system is used. From the viewpoints of non-covalent interactions calculated by using density functional theory (DFT) method, the formation mechanisms of these assembled structures were explored in detail. This work will supply a methodology to design the supramolecular assembled structures and the hetero-component materials composed by biological and chemical compound.

Voltammetric pH sensing using carbon electrodes: glassy carbon behaves similarly to EPPG.

PubMed

Lu, Min; Compton, Richard G

2014-09-21

Developing and building on recent work based on a simple sensor for pH determination using unmodified edge plane pyrolytic graphite (EPPG) electrodes, we present a voltammetric method for pH determination using a bare unmodified glassy carbon (GC) electrode. By exploiting the pH sensitive nature of quinones present on carbon edge-plane like sites within the GC, we show how GC electrodes can be used to measure pH. The electro-reduction of surface quinone groups on the glassy carbon electrode was characterised using cyclic voltammetry (CV) and optimised with square-wave voltammetry (SWV) at 298 K and 310 K. At both temperatures, a linear correlation was observed, corresponding to a 2 electron, 2 proton Nernstian response over the aqueous pH range 1.0 to 13.1. As such, unmodified glassy carbon electrodes are seen to be pH dependent, and the Nernstian response suggests its facile use for pH sensing. Given the widespread use of glassy carbon electrodes in electroanalysis, the approach offers a method for the near-simultaneous measurement and monitoring of pH during such analyses.

Bactericidal activity of self-assembled palmitic and stearic fatty acid crystals on highly ordered pyrolytic graphite.

PubMed

Ivanova, Elena P; Nguyen, Song Ha; Guo, Yachong; Baulin, Vladimir A; Webb, Hayden K; Truong, Vi Khanh; Wandiyanto, Jason V; Garvey, Christopher J; Mahon, Peter J; Mainwaring, David E; Crawford, Russell J

2017-09-01

The wings of insects such as cicadas and dragonflies have been found to possess nanostructure arrays that are assembled from fatty acids. These arrays can physically interact with the bacterial cell membranes, leading to the death of the cell. Such mechanobactericidal surfaces are of significant interest, as they can kill bacteria without the need for antibacterial chemicals. Here, we report on the bactericidal effect of two of the main lipid components of the insect wing epicuticle, palmitic (C16) and stearic (C18) fatty acids. Films of these fatty acids were re-crystallised on the surface of highly ordered pyrolytic graphite. It appeared that the presence of two additional CH 2 groups in the alkyl chain resulted in the formation of different surface structures. Scanning electron microscopy and atomic force microscopy showed that the palmitic acid microcrystallites were more asymmetric than those of the stearic acid, where the palmitic acid microcrystallites were observed to be an angular abutment in the scanning electron micrographs. The principal differences between the two types of long-chain saturated fatty acid crystallites were the larger density of peaks in the upper contact plane of the palmitic acid crystallites, as well as their greater proportion of asymmetrical shapes, in comparison to that of the stearic acid film. These two parameters might contribute to higher bactericidal activity on surfaces derived from palmitic acid. Both the palmitic and stearic acid crystallite surfaces displayed activity against Gram-negative, rod-shaped Pseudomonas aeruginosa and Gram-positive, spherical Staphylococcus aureus cells. These microcrystallite interfaces might be a useful tool in the fabrication of effective bactericidal nanocoatings. Nanostructured cicada and dragonfly wing surfaces have been discovered to be able physically kill bacterial cells. Here, we report on the successful fabrication of bactericidal three-dimensional structures of two main lipid components of the epicuticle of insect wings, palmitic (C16) and stearic (C18) acids. After crystallisation onto highly ordered pyrolytic graphite, both the palmitic and stearic acid films displayed bactericidal activity against both Gram-negative Pseudomonas aeruginosa and Gram-positive Staphylococcus aureus cells. The simplicity of the production of these microcrystallite interfaces suggests that a fabrication technique, based on solution deposition, could be an effective technique for the application of bactericidal nanocoatings. Copyright © 2017 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Coupling Graphene Sheets with Magnetic Nanoparticles for Energy Storage and Microelectronics

DTIC Science & Technology

2015-08-13

sheets obtained from three different synthetic methods: (i) electrochemical exfoliation of highly oriented pyrolytic graphite ( HOPG ) [8], (ii...Figure 8d, the characteristic lattice fringes of ɤ-Fe2O3 nanoparticles in graphene sheet is shown. Typical X-ray diffraction ( XRD ) patterns of the HOPG ...pattern in honey comb crystal lattice, (c) TEM (d) HRTEM image of graphene- PyDop1-MNP hybrid, (e) XRD pattern of the HOPG , exfoliated graphene, PyDop1

Characterization of ultralow thermal conductivity in anisotropic pyrolytic carbon coating for thermal management applications

DOE PAGES

Wang, Yuzhou; Hurley, David H.; Luther, Erik Paul; ...

2017-12-11

Pyrolytic carbon (PyC) is an important material used in many applications including thermal management of electronic devices and structural stability of ceramic composites. Accurate measurement of physical properties of structures containing textured PyC layers with few-micrometer thickness poses new challenges. Here a laser-based thermoreflectance technique is used to measure thermal conductivity in a 30-μm-thick textured PyC layer deposited using chemical vapor deposition on the surface of spherical zirconia particles. Raman spectroscopy is used to confirm the graphitic nature and characterize microstructure of the deposited layer. Room temperature radial and circumferential thermal conductivities are found to be 0.28 W m –1more » K –1 and 11.5 W m –1 K –1, corresponding to cross-plane and in-plane conductivities of graphite. While the anisotropic ratio of the in-plane to cross-plane conductivities is smaller than previous results, the magnitude of the smallest conductivity is noticeably smaller than previously reported values for carbon materials and offers opportunities in thermal management applications. Very low in-plane and cross-plane thermal conductivities are attributed to strong grain boundary scattering, high defect concentration, and small inter-laminar porosity. Lastly, experimental results agree with the prediction of thermal transport model informed by the microstructure information revealed by Raman spectroscopy.« less

Electrochemical detection of DNA damage induced by acrylamide and its metabolite at the graphene-ionic liquid-Nafion modified pyrolytic graphite electrode.

PubMed

Qiu, Yanyan; Qu, Xiangjin; Dong, Jing; Ai, Shiyun; Han, Ruixia

2011-06-15

A new electrochemical biosensor for directly detecting DNA damage induced by acrylamide (AA) and its metabolite was presented in this work. The graphene-ionic liquid-Nafion modified pyrolytic graphite electrode (PGE) was prepared, and then horseradish peroxidase (HRP) and natural double-stranded DNA were alternately assembled on the modified electrode by the layer-by-layer method. The PGE/graphene-ionic liquid-Nafion and the construction of the (HRP/DNA)(n) film were characterized by electrochemical impedance spectroscopy. With the guanine signal in DNA as an indicator, the damage of DNA was detected by differential pulse voltammetry after PGE/graphene-ionic liquid-Nafion/(HRP/DNA)(n) was incubated in AA solution or AA+H(2)O(2) solution at 37°C. This method provides a new model to mimic and directly detect DNA damage induced by chemical pollutants and their metabolites in vitro. The results indicated that, in the presence of H(2)O(2), HRP was activated and catalyzed the transformation of AA to glycidamide, which could form DNA adducts and induce more serious damage of DNA than AA. In order to further verify these results, UV-vis spectrophotometry was also used to investigate DNA damage induced by AA and its metabolites in solution and the similar results were obtained. Copyright © 2011 Elsevier B.V. All rights reserved.

Characterization of ultralow thermal conductivity in anisotropic pyrolytic carbon coating for thermal management applications

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

Wang, Yuzhou; Hurley, David H.; Luther, Erik Paul

Pyrolytic carbon (PyC) is an important material used in many applications including thermal management of electronic devices and structural stability of ceramic composites. Accurate measurement of physical properties of structures containing textured PyC layers with few-micrometer thickness poses new challenges. Here a laser-based thermoreflectance technique is used to measure thermal conductivity in a 30-μm-thick textured PyC layer deposited using chemical vapor deposition on the surface of spherical zirconia particles. Raman spectroscopy is used to confirm the graphitic nature and characterize microstructure of the deposited layer. Room temperature radial and circumferential thermal conductivities are found to be 0.28 W m –1more » K –1 and 11.5 W m –1 K –1, corresponding to cross-plane and in-plane conductivities of graphite. While the anisotropic ratio of the in-plane to cross-plane conductivities is smaller than previous results, the magnitude of the smallest conductivity is noticeably smaller than previously reported values for carbon materials and offers opportunities in thermal management applications. Very low in-plane and cross-plane thermal conductivities are attributed to strong grain boundary scattering, high defect concentration, and small inter-laminar porosity. Lastly, experimental results agree with the prediction of thermal transport model informed by the microstructure information revealed by Raman spectroscopy.« less

The theory of cyclic voltammetry of electrochemically heterogeneous surfaces: comparison of different models for surface geometry and applications to highly ordered pyrolytic graphite.

PubMed

Ward, Kristopher R; Lawrence, Nathan S; Hartshorne, R Seth; Compton, Richard G

2012-05-28

The cyclic voltammetry at electrodes composed of multiple electroactive materials, where zones of one highly active material are distributed over a substrate of a second, less active material, is investigated by simulation. The two materials are assumed to differ in terms of their electrochemical rate constants towards any given redox couple. For a one-electron oxidation or reduction, the effect on voltammetry of the size and relative surface coverages of the zones as well as the rate constant of the slower zone are considered for systems where it is much slower than the rate constant of the faster zones. The occurrence of split peak cyclic voltammetry where two peaks are observed in the forward sweep, is studied in terms of the diffusional effects present in the system. A number of surface geometries are compared: specifically the more active zones are modelled as long, thin bands, as steps in the surface, as discs, and as rings (similar to a partially blocked electrode). Similar voltammetry for the band, step and ring models is seen but the disc geometry shows significant differences. Finally, the simulation technique is applied to the modelling of highly-ordered pyrolytic graphite (HOPG) surface and experimental conditions under which it may be possible to observe split peak voltammetry are predicted.

Time-resolved investigations of the non-thermal ablation process of graphite induced by femtosecond laser pulses

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

Kalupka, C., E-mail: christian.kalupka@llt.rwth-aachen.de; Finger, J.; Reininghaus, M.

2016-04-21

We report on the in-situ analysis of the ablation dynamics of the, so-called, laser induced non-thermal ablation process of graphite. A highly oriented pyrolytic graphite is excited by femtosecond laser pulses with fluences below the classic thermal ablation threshold. The ablation dynamics are investigated by axial pump-probe reflection measurements, transversal pump-probe shadowgraphy, and time-resolved transversal emission photography. The combination of the applied analysis methods allows for a continuous and detailed time-resolved observation of the non-thermal ablation dynamics from several picoseconds up to 180 ns. Formation of large, μm-sized particles takes place within the first 3.5 ns after irradiation. The following propagation ofmore » ablation products and the shock wave front are tracked by transversal shadowgraphy up to 16 ns. The comparison of ablation dynamics of different fluences by emission photography reveals thermal ablation products even for non-thermal fluences.« less

Direct determination of Pb in raw milk by graphite furnace atomic absorption spectrometry (GF AAS) with electrothermal atomization sampling from slurries.

PubMed

de Oliveira, Tatiane Milão; Augusto Peres, Jayme; Lurdes Felsner, Maria; Cristiane Justi, Karin

2017-08-15

Milk is an important food in the human diet due to its physico-chemical composition; therefore, it is necessary to monitor contamination by toxic metals such as Pb. Milk sample slurries were prepared using Triton X-100 and nitric acid for direct analysis of Pb using graphite furnace atomic absorption spectrometry - GF AAS. After dilution of the slurries, 10.00µl were directly introduced into the pyrolytic graphite tube without use of a chemical modifier, which acts as an advantage considering this type of matrix. The limits of detection and quantification were 0.64 and 2.14µgl -1 , respectively. The figures of merit studied showed that the proposed methodology without pretreatment of the raw milk sample and using external standard calibration is suitable. The methodology was applied in milk samples from the Guarapuava region, in Paraná State (Brazil) and Pb concentrations ranged from 2.12 to 37.36µgl -1 . Copyright © 2017 Elsevier Ltd. All rights reserved.

Atomic intercalation to measure adhesion of graphene on graphite

PubMed Central

Wang, Jun; Sorescu, Dan C.; Jeon, Seokmin; Belianinov, Alexei; Kalinin, Sergei V.; Baddorf, Arthur P.; Maksymovych, Petro

2016-01-01

The interest in mechanical properties of two-dimensional materials has emerged in light of new device concepts taking advantage of flexing, adhesion and friction. Here we demonstrate an effective method to measure adhesion of graphene atop highly ordered pyrolytic graphite, utilizing atomic-scale ‘blisters' created in the top layer by neon atom intercalates. Detailed analysis of scanning tunnelling microscopy images is used to reconstruct atomic positions and the strain map within the deformed graphene layer, and demonstrate the tip-induced subsurface translation of neon atoms. We invoke an analytical model, originally devised for graphene macroscopic deformations, to determine the graphite adhesion energy of 0.221±0.011 J m−2. This value is in excellent agreement with reported macroscopic values and our atomistic simulations. This implies mechanical properties of graphene scale down to a few-nanometre length. The simplicity of our method provides a unique opportunity to investigate the local variability of nanomechanical properties in layered materials. PMID:27796294

The Physics and Chemistry of carbides, Nitrides and Borides. Volume 185

DTIC Science & Technology

1990-01-01

and C-B-C chains [15,17]. Clearly, the use of boron-rich solids as electronic materials will place new demands on the quality of materials. In this...first heated in a pyrolytic boron nitride (PBN) crucible ( Union Carbide Corp.) under high vacuum (< 50 mTorr) to 1900°C. This removed surface...contamination of the sample. The powders were loaded into a graphite die with a high-purity BN die liner ( Union Carbide Grade HBC) with inner diameter of 3/8

SPM observation of nano-dots induced by slow highly charged ions

NASA Astrophysics Data System (ADS)

Nakamura, Nobuyuki; Terada, Masashi; Nakai, Yoichi; Kanai, Yasuyuki; Ohtani, Shunsuke; Komaki, Ken-ichiro; Yamazaki, Yasunori

2005-05-01

We have observed nano-dots on a highly oriented pyrolytic graphite (HOPG) surface produced by highly charged ion impacts with a scanning probe microscope. In order to clarify the role of potential and kinetic energies in surface modification, we have measured the kinetic energy and incident ion charge dependences of the dot size. The results showed that the potential energy or the incident ion charge has strong influence on the surface modification rather than the kinetic energy.

Highly selective dopamine electrochemical sensor based on electrochemically pretreated graphite and nafion composite modified screen printed carbon electrode.

PubMed

Ku, Shuhao; Palanisamy, Selvakumar; Chen, Shen-Ming

2013-12-01

Herein, we report a highly selective dopamine electrochemical sensor based on electrochemically pretreated graphite/nafion composite modified screen printed carbon (SPC) electrode. Electrochemically activated graphite/nafion composite was prepared by using a simple electrochemical method. Scanning electron microscope (SEM) used to characterize the surface morphology of the fabricated composite electrode. The SEM result clearly indicates that the graphitic basal planes were totally disturbed and leads to the formation of graphite nanosheets. The composite modified electrode showed an enhanced electrocatalytic activity toward the oxidation of DA when compared with either electrochemical pretreated graphite or nafion SPC electrodes. The fabricated composite electrode exhibits a good electrocatalytic oxidation toward DA in the linear response range from 0.5 to 70 μM with the detection limit of 0.023 μM. The proposed sensor also exhibits very good selectivity and stability, with the appreciable sensitivity. In addition, the proposed sensor showed satisfactory recovery results toward the commercial pharmaceutical DA samples. Copyright © 2013 Elsevier Inc. All rights reserved.

Electron reflection and secondary emission characteristics of sputter-textured pyrolytic graphite surfaces

NASA Technical Reports Server (NTRS)

Wintucky, E. G.; Curren, A. N.; Sovey, J. S.

1981-01-01

Measurements are presented of secondary electron emission and reflected primary electron characteristics of sputter-textured pyrolitic graphite surfaces with microstructures of various sizes and densities, made with an Auger cylindrical mirror analyzer in a high-vacuum chamber at pressures below 1.33 x 10 to the -7th N/sq m (10 to the -9th torr). A dense, tall, thin, spire-like microstructure, obtained at ion energies of 1000 eV and ion current densities of 5 mA/sq cm, is the most effective. The secondary electron emission from such a surface is lower than that of soot, whose secondary emission is among the lowest of any material. At a primary electron energy of 1000 eV, the secondary electron emission yield of smooth CU is about 350% greater than the lowest value obtained for sputter-textured pyrolitic graphite. The reflected primary electron index of smooth Cu is a factor of 80 greater. If the secondary electron emission yield is reduced to 0.3, which is possible with sputter-textured pyrolitic graphite, the traveling wave tube collector efficiency could be improved by as much as 4% over that for smooth copper.

Electrochemical modification of a pyrolytic graphite sheet for improved negative electrode performance in the vanadium redox flow battery

NASA Astrophysics Data System (ADS)

Kabir, Humayun; Gyan, Isaiah O.; Francis Cheng, I.

2017-02-01

The vanadium redox flow battery is a promising technology for buffering renewable energies. It is recognized that negative electrode is the limitation in this device where there are problems of slow heterogeneous electron transfer (HET) of V3+/2+ and parasitic H2 evolution. Any methods aimed at addressing one of these barriers must assess the effects on the other. We examine electrochemical enhancement of a common commercially available material. Treatment of Panasonic pyrolytic graphite sheets is through oxidation at 2.1 V vs. Ag/AgCl for 1 min in 1 M H2SO4. This increases the standard HET rate for V3+/2+ from 3.2 × 10-7 to 1 × 10-3 cm/s, one of the highest in literature and shifts voltammetric reductive peak potential from -1.0 V to -0.65 V in 50 mM V3+ in 1 M H2SO4. Infrared analysis of the surfaces indicates formation of Csbnd OH, Cdbnd O, and Csbnd O functionalities. These groups catalyze HET with V3+/2+ as hypothesized by Skyllas-Kasacos. Also of significance is that electrode modification decreases the fraction of the current directed towards H2 evolution. This proportion decreases by two orders of a magnitude from 12% to 0.1% as measured at the respective voltammetric peak potentials of -1.0 V (pristine) and -0.65 V (modified).

Preliminary Results of Field Emission Cathode Tests

NASA Technical Reports Server (NTRS)

Sovey, James S.; Kovaleski, Scott D.

2001-01-01

Preliminary screening tests of field emission cathodes such as chemical vapor deposited (CVD) diamond, textured pyrolytic graphite, and textured copper were conducted at background pressures typical of electric thruster test facilities to assess cathode performance and stability. Very low power electric thrusters which provide tens to hundreds micronewtons of thrust may need field emission neutralizers that have a capability of tens to hundreds of microamperes. From current voltage characteristics, it was found that the CVD diamond and textured metals cathodes clearly satisfied the Fowler-Nordheim emission relation. The CVD diamond and a textured copper cathode had average current densities of 270 and 380 mA/sq cm, respectively, at the beginning-of-life. After a few hours of operation the cathode emission currents degraded by 40 to 75% at background pressures in the 10(exp -5) Pa to 10(exp -4) Pa range. The textured pyrolytic graphite had a modest current density at beginning-of-life of 84 mA/sq cm, but this cathode was the most stable of all. Extended testing of the most promising cathodes is warranted to determine if current degradation is a burn-in effect or whether it is a long-term degradation process. Preliminary experiments with ferroelectric emission cathodes, which are ceramics with spontaneous electric polarization, were conducted. Peak current densities of 30 to 120 mA/sq cm were obtained for pulse durations of about 500 ns in the 10(exp -4) Pa pressure range.

Soft X-Ray Absorption Spectroscopy of High-Abrasion-Furnace Carbon Black

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

Muramatsu, Yasuji; Harada, Ryusuke; Gullikson, Eric M.

2007-02-02

The soft x-ray absorption spectra of high-abrasion-furnace carbon black were measured to obtain local-structure/chemical-states information of the primary particles and/or crystallites. The soft x-ray absorption spectral features of carbon black represent broader {pi}* and {sigma}* peak structures compared to highly oriented pyrolytic graphite (HOPG). The subtracted spectra between the carbon black and HOPG, (carbon black) - (HOPG), show double-peak structures on both sides of the {pi}* peak. The lower-energy peak, denoted as the 'pre-peak', in the subtracted spectra and the {pi}*/{sigma}* peak intensity ratio in the absorption spectra clearly depend on the specific surface area by nitrogen adsorption (NSA). Therefore,more » it is concluded that the pre-peak intensity and the {pi}*/{sigma}* ratio reflect the local graphitic structure of carbon black.« less

Internal and external atomic steps in graphite exhibit dramatically different physical and chemical properties.

PubMed

Lee, Hyunsoo; Lee, Han-Bo-Ram; Kwon, Sangku; Salmeron, Miquel; Park, Jeong Young

2015-04-28

We report on the physical and chemical properties of atomic steps on the surface of highly oriented pyrolytic graphite (HOPG) investigated using atomic force microscopy. Two types of step edges are identified: internal (formed during crystal growth) and external (formed by mechanical cleavage of bulk HOPG). The external steps exhibit higher friction than the internal steps due to the broken bonds of the exposed edge C atoms, while carbon atoms in the internal steps are not exposed. The reactivity of the atomic steps is manifested in a variety of ways, including the preferential attachment of Pt nanoparticles deposited on HOPG when using atomic layer deposition and KOH clusters formed during drop casting from aqueous solutions. These phenomena imply that only external atomic steps can be used for selective electrodeposition for nanoscale electronic devices.

Investigation of Pristine Graphite Oxide as Room-Temperature Chemiresistive Ammonia Gas Sensing Material.

PubMed

Bannov, Alexander G; Prášek, Jan; Jašek, Ondřej; Zajíčková, Lenka

2017-02-09

Graphite oxide has been investigated as a possible room-temperature chemiresistive sensor of ammonia in a gas phase. Graphite oxide was synthesized from high purity graphite using the modified Hummers method. The graphite oxide sample was investigated using scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray diffraction, thermogravimetry and differential scanning calorimetry. Sensing properties were tested in a wide range of ammonia concentrations in air (10-1000 ppm) and under different relative humidity levels (3%-65%). It was concluded that the graphite oxide-based sensor possessed a good response to NH₃ in dry synthetic air (ΔR/R₀ ranged from 2.5% to 7.4% for concentrations of 100-500 ppm and 3% relative humidity) with negligible cross-sensitivity towards H₂ and CH₄. It was determined that the sensor recovery rate was improved with ammonia concentration growth. Increasing the ambient relative humidity led to an increase of the sensor response. The highest response of 22.2% for 100 ppm of ammonia was achieved at a 65% relative humidity level.

The defect level and ideal thermal conductivity of graphene uncovered by residual thermal reffusivity at the 0 K limit

NASA Astrophysics Data System (ADS)

Xie, Yangsu; Xu, Zaoli; Xu, Shen; Cheng, Zhe; Hashemi, Nastaran; Deng, Cheng; Wang, Xinwei

2015-05-01

Due to its intriguing thermal and electrical properties, graphene has been widely studied for potential applications in sensor and energy devices. However, the reported value for its thermal conductivity spans from dozens to thousands of W m-1 K-1 due to different levels of alternations and defects in graphene samples. In this work, the thermal diffusivity of suspended four-layered graphene foam (GF) is characterized from room temperature (RT) down to 17 K. For the first time, we identify the defect level in graphene by evaluating the inverse of thermal diffusivity (termed ``thermal reffusivity'': Θ) at the 0 K limit. By using the Debye model of Θ = Θ0 + C × e-θ/2T and fitting the Θ-T curve to the point of T = 0 K, we identify the defect level (Θ0) and determine the Debye temperature of graphene. Θ0 is found to be 1878 s m-2 for the studied GF and 43-112 s m-2 for three highly crystalline graphite materials. This uncovers a 16-43-fold higher defect level in GF than that in pyrolytic graphite. In GF, the phonon mean free path solely induced by defects and boundary scattering is determined as 166 nm. The Debye temperature of graphene is determined to be 1813 K, which is very close to the average theoretical Debye temperature (1911 K) of the three acoustic phonon modes in graphene. By subtracting the defect effect, we report the ideal thermal diffusivity and conductivity (κideal) of graphene presented in the 3D foam structure in the range of 33-299 K. Detailed physics based on chemical composition and structure analysis are given to explain the κideal-T profile by comparing with those reported for suspended graphene.Due to its intriguing thermal and electrical properties, graphene has been widely studied for potential applications in sensor and energy devices. However, the reported value for its thermal conductivity spans from dozens to thousands of W m-1 K-1 due to different levels of alternations and defects in graphene samples. In this work, the thermal diffusivity of suspended four-layered graphene foam (GF) is characterized from room temperature (RT) down to 17 K. For the first time, we identify the defect level in graphene by evaluating the inverse of thermal diffusivity (termed ``thermal reffusivity'': Θ) at the 0 K limit. By using the Debye model of Θ = Θ0 + C × e-θ/2T and fitting the Θ-T curve to the point of T = 0 K, we identify the defect level (Θ0) and determine the Debye temperature of graphene. Θ0 is found to be 1878 s m-2 for the studied GF and 43-112 s m-2 for three highly crystalline graphite materials. This uncovers a 16-43-fold higher defect level in GF than that in pyrolytic graphite. In GF, the phonon mean free path solely induced by defects and boundary scattering is determined as 166 nm. The Debye temperature of graphene is determined to be 1813 K, which is very close to the average theoretical Debye temperature (1911 K) of the three acoustic phonon modes in graphene. By subtracting the defect effect, we report the ideal thermal diffusivity and conductivity (κideal) of graphene presented in the 3D foam structure in the range of 33-299 K. Detailed physics based on chemical composition and structure analysis are given to explain the κideal-T profile by comparing with those reported for suspended graphene. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr02012c

From Graphite to Graphene via Scanning Tunneling Microscopy

NASA Astrophysics Data System (ADS)

Qi, Dejun

The primary objective of this dissertation is to study both graphene on graphite and pristine freestanding grapheme using scanning tunneling microscopy (STM) and density functional theory (DFT) simulation technique. In the experiment part, good quality tungsten metalic tips for experiment were fabricated using our newly developed tip making setup. Then a series of measurements using a technique called electrostatic-manipulation scanning tunneling microscopy (EM-STM) of our own development were performed on a highly oriented pyrolytic graphite (HOPG) surface. The electrostatic interaction between the STM tip and the sample can be tuned to produce both reversible and irreversible large-scale movement of the graphite surface. Under this influence, atomic-resolution STM images reveal that a continuous electronic transition between two distinct patterns can be systematically controlled. DFT calculations reveal that this transition can be related to vertical displacements of the top layer of graphite relative to the bulk. Evidence for horizontal shifts in the top layer of graphite is also presented. Excellent agreement is found between experimental STM images and those simulated using DFT. In addition, the EM-STM technique was also used to controllably and reversibly pull freestanding graphene membranes up to 35 nm from their equilibrium height. Atomic-scale corrugation amplitudes 20 times larger than the STM electronic corrugation for graphene on a substrate were observed. The freestanding graphene membrane responds to a local attractive force created at the STM tip as a highly conductive yet flexible grounding plane with an elastic restoring force.

SUMMARY OF THE SEVENTH MEETING OF THE REFRACTORY COMPOSITES WORKING GROUP

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

Gibeaut, W.A.; Ogden, H.R.

1963-05-30

Information on refractory composites for use above 2500 deg F is summarized. Reports are concerned with protective coatings, insulating ceramics, materials for rocket thrust chambers, dispersion strengthening of metals, joining of refractory materials, and testing techniques. The problem of accelerated failure of silicide coatings under conditions of very low air pressure at high temperatures is studied. Although the maximum temperature capability of most silicide coatings is reduced about 50 theta deg at low air pressures, several coatings can protect molybdenum for 1/2 hr at 2800 to 3000 deg F under these conditions. The tin-aluminum coating also is susceptible to earlymore » failure at reduced pressure. An evaluation of the mechanical properties of 6-mil foils of D- 36, B-68, and TZM coated with commercial coatings demonstrated that some coatings seriously degrade substrate mechanical properties. Research on thermal- protection systems for re-entry vehicles whose surface temperatures reach from 3300 to 5500 deg F has resulted in agreement upon oxide coatings and thick metal- reinforced oxide composites. Simple plasmaarc-sprayed oxide coatings have demonstrated adequate oxidation resistance, but their structural stability in cyclic thermal exposure is inferior to metal-reinforced oxide. Thin unreinforced oxide coatings tend to spall in tests involving cyclic heating. A metal- reinforced oxide composite (reinforcement welded to substrate) has survived cyclic tests such as five 3-minute exposures at 4500 deg F without failing. A new carbon material called glassy carbon has demonstrnted better oxidation resistance than pyrolytic graphite at very high temperatures. The erosion resistance of pyrolytic graphite coatings on regular graphite in rocket firing tests using solid propellants is encouraging. There is considerable interest in fabricating small radiation-cooled rocket thrust chambers by plasma arc spraying. The design concept of internal reinforcement of sprayed-metal rocket chambers with wrought ductile wife appears impractical because of poor bonding and porosity around the wire. (auth)« less

Two-dimensional network stability of nucleobases and amino acids on graphite under ambient conditions: adenine, L-serine and L-tyrosine.

PubMed

Bald, Ilko; Weigelt, Sigrid; Ma, Xiaojing; Xie, Pengyang; Subramani, Ramesh; Dong, Mingdong; Wang, Chen; Mamdouh, Wael; Wang, Jianguo; Besenbacher, Flemming

2010-04-14

We have investigated the stability of two-dimensional self-assembled molecular networks formed upon co-adsorption of the DNA base, adenine, with each of the amino acids, L-serine and L-tyrosine, on a highly oriented pyrolytic graphite (HOPG) surface by drop-casting from a water solution. L-serine and L-tyrosine were chosen as model systems due to their different interaction with the solvent molecules and the graphite substrate, which is reflected in a high and low solubility in water, respectively, compared with adenine. Combined scanning tunneling microscopy (STM) measurements and density functional theory (DFT) calculations show that the self-assembly process is mainly driven by the formation of strong adenine-adenine hydrogen bonds. We find that pure adenine networks are energetically more stable than networks built up of either pure L-serine, pure L-tyrosine or combinations of adenine with L-serine or L-tyrosine, and that only pure adenine networks are stable enough to be observable by STM under ambient conditions.

Magnetotransport in Two Dimensional Electron Systems Under Microwave Excitation and in Highly Oriented Pyrolytic Graphite

DTIC Science & Technology

2012-01-01

Phys. Rev. Lett. 82, 2147 (1999). [89] Y. Zhang, Y. Tan, H. L. Stormer and P. Kim, Nature 438, 10 (2005). [90] J. W. McClure, Phys. Rev. 108, 612 (1957...Phys. 2, 595 (2006). [97] H. L. Stormer , J. P. Eisenstein, A. C. Gossard, W. Wiegmann, and K. Baldwin, Phys. Rev. Lett. 56, 85 (1985). [98] B. A...Sadowski, J. M. Schneider, and M. Potemski, J. Phys.: Cond. Matter 20, 454223 (2008). [108] W. Pan, J. S. Xia, H. L. Stormer , D. C. Tsui, C. L

Coupling Graphene Sheets with Iron Oxide Nanoparticles for Energy Storage and Microelectronics

DTIC Science & Technology

2015-08-13

of highly oriented pyrolytic graphite ( HOPG ) flake. Two electrode system containing platinum as counter electrode and HOPG as working electrode is... XRD ) patterns of the HOPG , exfoliated graphene, PyDop1-ɤ-Fe2O3 and PyDop1-ɤ-Fe2O3-graphene are given in Figure 1e. HOPG show a very sharp diffraction...atoms arranged in hexagonal pattern in honey comb crystal lattice, (c) TEM (d) HRTEM image of graphene- PyDop1-MNP hybrid, (e) XRD pattern of the HOPG

Spectroscopic and electrochemical behavior of the novel tetra-2-methyl-pyrazinoporphyrazines

NASA Astrophysics Data System (ADS)

Pişkin, Mehmet; Öztürk, Naciye; Durmuş, Mahmut

2017-12-01

This study presents the synthesis and characterization of novel metal-free (H2Pc) and metallo porphyrazines (magnesium(II) (MgPz), copper(II) (CuPz), iron(II) (FePz), manganese(II) (MnPz) and nickel(II) (NiPz)) substituted with four 2-methylpyrazine groups on the peripheral positions. The spectroscopic properties of newly synthesized porphyrazines were investigated. The electrochemical behaviors of these porphyrazines were also determined in DMSO solution by cyclic voltammetry (CV) and square wave voltammetry (SWV) methods on edge plane pyrolytic graphite electrode (EPPG) electrode.

Ultralight anisotropic foams from layered aligned carbon nanotube sheets

NASA Astrophysics Data System (ADS)

Faraji, Shaghayegh; L. Stano, Kelly; Yildiz, Ozkan; Li, Ang; Zhu, Yuntian; Bradford, Philip D.

2015-10-01

In this work, we present large scale, ultralight aligned carbon nanotube (CNT) structures which have densities an order of magnitude lower than CNT arrays, have tunable properties and exhibit resiliency after compression. By stacking aligned sheets of carbon nanotubes and then infiltrating with a pyrolytic carbon (PyC), resilient foam-like materials were produced that exhibited complete recovery from 90% compressive strain. With density as low as 3.8 mg cm-3, the foam structure is over 500 times less dense than bulk graphite. Microscopy revealed that PyC coated the junctions among CNTs, and also increased CNT surface roughness. These changes in the morphology explain the transition from inelastic behavior to foam-like recovery of the layered CNT sheet structure. Mechanical and thermal properties of the foams were tuned for different applications through variation of PyC deposition duration while dynamic mechanical analysis showed no change in mechanical properties over a large temperature range. Observation of a large and linear electrical resistance change during compression of the aligned CNT/carbon (ACNT/C) foams makes strain/pressure sensors a relevant application. The foams have high oil absorption capacities, up to 275 times their own weight, which suggests they may be useful in water treatment and oil spill cleanup. Finally, the ACNT/C foam's high porosity, surface area and stability allow for demonstration of the foams as catalyst support structures.In this work, we present large scale, ultralight aligned carbon nanotube (CNT) structures which have densities an order of magnitude lower than CNT arrays, have tunable properties and exhibit resiliency after compression. By stacking aligned sheets of carbon nanotubes and then infiltrating with a pyrolytic carbon (PyC), resilient foam-like materials were produced that exhibited complete recovery from 90% compressive strain. With density as low as 3.8 mg cm-3, the foam structure is over 500 times less dense than bulk graphite. Microscopy revealed that PyC coated the junctions among CNTs, and also increased CNT surface roughness. These changes in the morphology explain the transition from inelastic behavior to foam-like recovery of the layered CNT sheet structure. Mechanical and thermal properties of the foams were tuned for different applications through variation of PyC deposition duration while dynamic mechanical analysis showed no change in mechanical properties over a large temperature range. Observation of a large and linear electrical resistance change during compression of the aligned CNT/carbon (ACNT/C) foams makes strain/pressure sensors a relevant application. The foams have high oil absorption capacities, up to 275 times their own weight, which suggests they may be useful in water treatment and oil spill cleanup. Finally, the ACNT/C foam's high porosity, surface area and stability allow for demonstration of the foams as catalyst support structures. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr03899e

Effects of chemical states of carbon on deuterium retention in carbon-containing materials

NASA Astrophysics Data System (ADS)

Oyaidzu, Makoto; Kimura, Hiromi; Nakahata, Toshihiko; Nishikawa, Yusuke; Tokitani, Masayuki; Oya, Yasuhisa; Iwakiri, Hirotomo; Yoshida, Naoaki; Okuno, Kenji

2007-08-01

Deuterium retention behavior in highly oriented pyrolytic graphite (HOPG), poly-crystalline diamond, poly-crystalline SiC, sintered WC, and converted B 4C were investigated to reveal tritium behavior in re-deposition and co-deposition layers. Such layers would contain carbon, when the first wall and/or divertor were made of graphite or carbon-containing materials. Furthermore, the employment of other materials such as tungsten, and first wall conditioning such as boronization would complicate the layers. No different deuterium trapping sites due to carbon from those in HOPG were found in all the samples, where two deuterium trapping processes were observed: hot atom chemical trapping of energetic deuterium by a dangling bond of carbon and thermochemical trapping of thermalized deuterium in a constituent atom vacancy surrounded by carbons. Additionally, the latter reaction could be easily counteracted by or competed with the other deuterium trapping reactions by constituent atoms.

Femtosecond laser ablation of highly oriented pyrolytic graphite: a green route for large-scale production of porous graphene and graphene quantum dots.

PubMed

Russo, Paola; Hu, Anming; Compagnini, Giuseppe; Duley, Walter W; Zhou, Norman Y

2014-02-21

Porous graphene (PG) and graphene quantum dots (GQDs) are attracting attention due to their potential applications in photovoltaics, catalysis, and bio-related fields. We present a novel way for mass production of these promising materials. The femtosecond laser ablation of highly oriented pyrolytic graphite (HOPG) is employed for their synthesis. Porous graphene (PG) layers were found to float at the water-air interface, while graphene quantum dots (GQDs) were dispersed in the solution. The sheets consist of one to six stacked layers of spongy graphene, which form an irregular 3D porous structure that displays pores with an average size of 15-20 nm. Several characterization techniques have confirmed the porous nature of the collected layers. The analyses of the aqueous solution confirmed the presence of GQDs with dimensions of about 2-5 nm. It is found that the formation of both PG and GQDs depends on the fs-laser ablation energy. At laser fluences less than 12 J cm(-2), no evidence of either PG or GQDs is detected. However, polyynes with six and eight carbon atoms per chain are found in the solution. For laser energies in the 20-30 J cm(-2) range, these polyynes disappeared, while PG and GQDs were found at the water-air interface and in the solution, respectively. The origin of these materials can be explained based on the mechanisms for water breakdown and coal gasification. The absence of PG and GQDs, after the laser ablation of HOPG in liquid nitrogen, confirms the proposed mechanisms.

The defect level and ideal thermal conductivity of graphene uncovered by residual thermal reffusivity at the 0 K limit.

PubMed

Xie, Yangsu; Xu, Zaoli; Xu, Shen; Cheng, Zhe; Hashemi, Nastaran; Deng, Cheng; Wang, Xinwei

2015-06-14

Due to its intriguing thermal and electrical properties, graphene has been widely studied for potential applications in sensor and energy devices. However, the reported value for its thermal conductivity spans from dozens to thousands of W m(-1) K(-1) due to different levels of alternations and defects in graphene samples. In this work, the thermal diffusivity of suspended four-layered graphene foam (GF) is characterized from room temperature (RT) down to 17 K. For the first time, we identify the defect level in graphene by evaluating the inverse of thermal diffusivity (termed "thermal reffusivity": Θ) at the 0 K limit. By using the Debye model of Θ = Θ0 + C× e(-θ/2T) and fitting the Θ-T curve to the point of T = 0 K, we identify the defect level (Θ0) and determine the Debye temperature of graphene. Θ0 is found to be 1878 s m(-2) for the studied GF and 43-112 s m(-2) for three highly crystalline graphite materials. This uncovers a 16-43-fold higher defect level in GF than that in pyrolytic graphite. In GF, the phonon mean free path solely induced by defects and boundary scattering is determined as 166 nm. The Debye temperature of graphene is determined to be 1813 K, which is very close to the average theoretical Debye temperature (1911 K) of the three acoustic phonon modes in graphene. By subtracting the defect effect, we report the ideal thermal diffusivity and conductivity (κideal) of graphene presented in the 3D foam structure in the range of 33-299 K. Detailed physics based on chemical composition and structure analysis are given to explain the κideal-T profile by comparing with those reported for suspended graphene.

High temperature blackbody BB2000/40 for calibration of radiation thermometers and thermocouple

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

Ogarev, S. A.; Khlevnoy, B. B.; Samoylov, M. L.

2013-09-11

The cavity-type high temperature blackbody (HTBB) models of BB3200/3500 series are the most spread among metrological institutes worldwide as sources for radiometry and radiation thermometry, due to their ultra high working temperatures, high emissivity and stability. The materials of radiating cavities are graphite, pyrolytic graphite (PG) and their combination. The paper describes BB2000/40 blackbody with graphite-tube cavity that was developed for calibration of radiation thermometers at SCEI (Singapore). The peculiarity of BB2000/40 is a possibility to use it, besides calibration of pyrometers, as an instrument for thermocouples calibration. Operating within the temperature range from 900 °C to 2000 °C, themore » blackbody has a wide cavity opening of 40 mm. Emissivity of the cavity, with PG heater rings replaced partly by graphite elements, was estimated as 0.998 ± 0.0015 in the spectral range from 350 nm to 2000 nm. The uniformity along the cavity axis, accounting for 10 °C, was measured using a B-type thermocouple at 1500 °C. The BB2000/40, if necessary, can be easily modified, by replacing the graphite radiator with a set of PG rings, to be able to reach temperatures as high as 3200 °C. The HTBB utilizes an optical feedback system which allows temperature stabilization within 0.1 °C. This rear-view feedback allows the whole HTBB aperture to be used for measurements.« less

Pyrolytic carbon-coated stainless steel felt as a high-performance anode for bioelectrochemical systems.

PubMed

Guo, Kun; Hidalgo, Diana; Tommasi, Tonia; Rabaey, Korneel

2016-07-01

Scale up of bioelectrochemical systems (BESs) requires highly conductive, biocompatible and stable electrodes. Here we present pyrolytic carbon-coated stainless steel felt (C-SS felt) as a high-performance and scalable anode. The electrode is created by generating a carbon layer on stainless steel felt (SS felt) via a multi-step deposition process involving α-d-glucose impregnation, caramelization, and pyrolysis. Physicochemical characterizations of the surface elucidate that a thin (20±5μm) and homogenous layer of polycrystalline graphitic carbon was obtained on SS felt surface after modification. The carbon coating significantly increases the biocompatibility, enabling robust electroactive biofilm formation. The C-SS felt electrodes reach current densities (jmax) of 3.65±0.14mA/cm(2) within 7days of operation, which is 11 times higher than plain SS felt electrodes (0.30±0.04mA/cm(2)). The excellent biocompatibility, high specific surface area, high conductivity, good mechanical strength, and low cost make C-SS felt a promising electrode for BESs. Copyright © 2016 Elsevier Ltd. All rights reserved.

Mechanisms of ultrafast laser-induced deep-subwavelength gratings on graphite and diamond

NASA Astrophysics Data System (ADS)

Huang, Min; Zhao, Fuli; Cheng, Ya; Xu, Ningsheg; Xu, Zhizhan

2009-03-01

Deep-subwavelength gratings with periodicities of 170, 120, and 70 nm can be observed on highly oriented pyrolytic graphite irradiated by a femtosecond (fs) laser at 800 nm. Under picosecond laser irradiation, such gratings likewise can be produced. Interestingly, the 170-nm grating is also observed on single-crystal diamond irradiated by the 800-nm fs laser. In our opinion, the optical properties of the high-excited state of material surface play a key role for the formation of the deep-subwavelength gratings. The numerical simulations of the graphite deep-subwavelength grating at normal and high-excited states confirm that in the groove the light intensity can be extraordinarily enhanced via cavity-mode excitation in the condition of transverse-magnetic wave irradiation with near-ablation-threshold fluences. This field enhancement of polarization sensitiveness in deep-subwavelength apertures acts as an important feedback mechanism for the growth and polarization dependence of the deep-subwavelength gratings. In addition, we suggest that surface plasmons are responsible for the formation of seed deep-subwavelength apertures with a particular periodicity and the initial polarization dependence. Finally, we propose that the nanoscale Coulomb explosion occurring in the groove is responsible for the ultrafast nonthermal ablation mechanism.

Orientation-free and differentially pumped addition of a low-flux reactive gas beam to a surface analysis system.

PubMed

Harthcock, Colin; Jahanbekam, Abdolreza; Eskelsen, Jeremy R; Lee, David Y

2016-11-01

We describe an example of a piecewise gas chamber that can be customized to incorporate a low flux of gas-phase radicals with an existing surface analysis chamber for in situ and stepwise gas-surface interaction experiments without any constraint in orientation. The piecewise nature of this gas chamber provides complete angular freedom and easy alignment and does not require any modification of the existing surface analysis chamber. In addition, the entire gas-surface system is readily differentially pumped with the surface chamber kept under ultra-high-vacuum during the gas-surface measurements. This new design also allows not only straightforward reconstruction to accommodate the orientation of different surface chambers but also for the addition of other desired features, such as an additional pump to the current configuration. Stepwise interaction between atomic oxygen and a highly ordered pyrolytic graphite surface was chosen to test the effectiveness of this design, and the site-dependent O-atom chemisorption and clustering on the graphite surface were resolved by a scanning tunneling microscope in the nm-scale. X-ray photoelectron spectroscopy was used to further confirm the identity of the chemisorbed species on the graphite surface as oxygen.

Effective regeneration of anode material recycled from scrapped Li-ion batteries

NASA Astrophysics Data System (ADS)

Zhang, Jin; Li, Xuelei; Song, Dawei; Miao, Yanli; Song, Jishun; Zhang, Lianqi

2018-06-01

Recycling high-valuable metal elements (such as Li, Ni, Co, Al and Cu elements) from scrapped lithium ion batteries can bring significant economic benefits. However, recycling and reusing anode material has not yet attracted wide attention up to now, due to the lower added-value than the above valuable metal materials and the difficulties in regenerating process. In this paper, a novel regeneration process with significant green advance is proposed to regenerate anode material recycled from scrapped Li-ion batteries for the first time. After regenerated, most acetylene black (AB) and all the styrene butadiene rubber (SBR), carboxymethylcellulose sodium (CMC) in recycled anode material are removed, and the surface of anode material is coated with pyrolytic carbon from phenolic resin again. Finally, the regenerated anode material (graphite with coating layer, residual AB and a little CMC pyrolysis product) is obtained. As expected, all the technical indexs of regenerated anode material exceed that of a midrange graphite with the same type, and partial technical indexs are even closed to that of the unused graphite. The results indicate the effective regeneration of anode material recycled from scrapped Li-ion batteries is really achieved.

Atomic intercalation to measure adhesion of graphene on graphite

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

Wang, Jun; Sorescu, Dan C.; Jeon, Seokmin

The interest in mechanical properties of layered and 2D materials has reemerged in light of device concepts that take advantage of flexing, adhesion and friction in such systems. Here we provide an effective measurement of the nanoscale elastic adhesion of a graphene sheet atop highly ordered pyrolytic graphite (HOPG) based on the analysis of atomic intercalates in graphite. Atomic intercalation is carried out using conventional ion sputtering, creating blisters in the top-most layer of the HOPG surface. Scanning tunneling microscopy coupled with image analysis and density functional theory are used to reconstruct the atomic positions and the strain map withinmore » the deformed graphene sheet, as well as to demonstrate subsurface diffusion of the ions creating such blisters. To estimate the adhesion energy we invoke an analytical model originally devised for macroscopic deformations of graphene. This model yields a value of 0.221 ± 0.011 J/m -2 for the adhesion energy of graphite, which is in surprisingly good agreement with reported experimental and theoretical values. This implies that macroscopic mechanical properties of graphene scale down to at least a few nanometers length. The simplicity of our method, compared to the macroscale characterization, enables analysis of elastic mechanical properties in two-dimensional layered materials and provides a unique opportunity to investigate the local variability of mechanical properties on the nanoscale.« less

Atomic intercalation to measure adhesion of graphene on graphite

DOE PAGES

Wang, Jun; Sorescu, Dan C.; Jeon, Seokmin; ...

2016-10-31

The interest in mechanical properties of layered and 2D materials has reemerged in light of device concepts that take advantage of flexing, adhesion and friction in such systems. Here we provide an effective measurement of the nanoscale elastic adhesion of a graphene sheet atop highly ordered pyrolytic graphite (HOPG) based on the analysis of atomic intercalates in graphite. Atomic intercalation is carried out using conventional ion sputtering, creating blisters in the top-most layer of the HOPG surface. Scanning tunneling microscopy coupled with image analysis and density functional theory are used to reconstruct the atomic positions and the strain map withinmore » the deformed graphene sheet, as well as to demonstrate subsurface diffusion of the ions creating such blisters. To estimate the adhesion energy we invoke an analytical model originally devised for macroscopic deformations of graphene. This model yields a value of 0.221 ± 0.011 J/m -2 for the adhesion energy of graphite, which is in surprisingly good agreement with reported experimental and theoretical values. This implies that macroscopic mechanical properties of graphene scale down to at least a few nanometers length. The simplicity of our method, compared to the macroscale characterization, enables analysis of elastic mechanical properties in two-dimensional layered materials and provides a unique opportunity to investigate the local variability of mechanical properties on the nanoscale.« less

Photodeposition of Gold, Platinum, or Silver onto Titanium Dioxide Nanoparticles at Steps of Highly Oriented Pyrolytic Graphite

NASA Astrophysics Data System (ADS)

Taing, James

The photodeposition of gold, platinum, or silver nanoparticles selectively onto isolated titanium dioxide (TiO2) nanoparticles created metal/TiO2 photocatalysts and heterogeneous catalysts, and validated the photocatalytic property of the semiconductor. The isolated and ordered TiO2 nanoparticles permitted clear observations of the stability, and changes in morphology, of the particles in various experimental conditions. The fabrication of TiO2 nanoparticles at the steps of highly oriented pyrolytic graphite (HOPG), utilizing physical vapor deposition, required heating the graphite substrate to a minimum of 800 °C. The production of a photocurrent, and plating of gold nanoparticles, confirmed the photocatalytic property of the TiO2 nanoparticles on HOPG when utilized as a photoelectrode in a two half-cell setup. Employing sodium chloride (1.0 M) as an electrolyte resulted in an increase/decrease of the photocurrent with the addition of gold cations to the half-cell without/with the TiO2 nanoparticles. A poor distribution of gold nanoparticles, roughly 40-45 nm wide, deposited around few of the TiO2 nanoparticles. A lower concentration of sodium chloride (0.1 M) resulted in a coalescence of Au nanoparticles, roughly 10 nm, around many TiO2 nanoparticles. Using sodium nitrate as an electrolyte resulted in a rapid decay in the photocurrent and a growth of an unidentified material on the TiO2 nanoparticles. The unidentified material hindered the reduction of gold cations introduced midway through the experiment. With gold cations present at the onset of the experiment, disperse gold nanoparticles (˜5-10 nm) deposited around the TiO2 nanoparticles. In the absence of additional electrolyte, many disperse gold nanoparticles less than 5 nm deposited onto the TiO2 nanoparticles. More platinum than gold selectively deposited onto the TiO2 nanoparticles. On the contrary, less silver selectively deposited onto the TiO2 nanoparticles. Scanning electron microscopy and atomic force microscopy determined the morphology and distribution of the TiO2 nanoparticles and metal/TiO 2 nanocomposites. Energy dispersive X-ray spectroscopy, transmission electron microscopy, and X-ray photoelectron spectroscopy identified the composition of the materials.

Quantized edge modes in atomic-scale point contacts in graphene

NASA Astrophysics Data System (ADS)

Kinikar, Amogh; Phanindra Sai, T.; Bhattacharyya, Semonti; Agarwala, Adhip; Biswas, Tathagata; Sarker, Sanjoy K.; Krishnamurthy, H. R.; Jain, Manish; Shenoy, Vijay B.; Ghosh, Arindam

2017-07-01

The zigzag edges of single- or few-layer graphene are perfect one-dimensional conductors owing to a set of gapless states that are topologically protected against backscattering. Direct experimental evidence of these states has been limited so far to their local thermodynamic and magnetic properties, determined by the competing effects of edge topology and electron-electron interaction. However, experimental signatures of edge-bound electrical conduction have remained elusive, primarily due to the lack of graphitic nanostructures with low structural and/or chemical edge disorder. Here, we report the experimental detection of edge-mode electrical transport in suspended atomic-scale constrictions of single and multilayer graphene created during nanomechanical exfoliation of highly oriented pyrolytic graphite. The edge-mode transport leads to the observed quantization of conductance close to multiples of G0 = 2e2/h. At the same time, conductance plateaux at G0/2 and a split zero-bias anomaly in non-equilibrium transport suggest conduction via spin-polarized states in the presence of an electron-electron interaction.

Scanning tunneling microscopy investigation of copper phthalocyanine and truxenone derivative binary superstructures on graphite.

PubMed

Liu, Jia; Wang, Dong; Wang, Jie-Yu; Pei, Jian; Wan, Li-Jun

2011-02-01

The binary self-assembly of copper phthalocyanine (CuPc) and 2,3,7,8,12,13-hexahexyloxy-truxenone (TrO23) at the solid/liquid interface of highly oriented pyrolytic graphite (HOPG) was investigated by using scanning tunneling microscopy (STM) and scanning tunneling spectroscopy (STS). Pseduohexagonal and linear patterned superstructures of CuPc are obtained by co-adsorbing with TrO23. High-resolution STM images reveal the structural details of the arrangement of TrO23 and CuPc in the binary assembly structures. The molecular ratio between CuPc and TrO23 in the adlayer can be modulated by the CuPc concentration in liquid phase. The electronic properties of CuPc and TrO23 in the co-adsorbed self-assembly are investigated by STS. The results presented here are helpful to the design and fabrication of multi-component functional molecular nanostructures. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Imaging surface nanobubbles at graphite-water interfaces with different atomic force microscopy modes.

PubMed

Yang, Chih-Wen; Lu, Yi-Hsien; Hwang, Ing-Shouh

2013-05-08

We have imaged nanobubbles on highly ordered pyrolytic graphite (HOPG) surfaces in pure water with different atomic force microscopy (AFM) modes, including the frequency-modulation, the tapping, and the PeakForce techniques. We have compared the performance of these modes in obtaining the surface profiles of nanobubbles. The frequency-modulation mode yields a larger height value than the other two modes and can provide more accurate measurement of the surface profiles of nanobubbles. Imaging with PeakForce mode shows that a nanobubble appears smaller and shorter with increasing peak force and disappears above a certain peak force, but the size returns to the original value when the peak force is reduced. This indicates that imaging with high peak forces does not cause gas removal from the nanobubbles. Based on the presented findings and previous AFM observations, the existing models for nanobubbles are reviewed and discussed. The model of gas aggregate inside nanobubbles provides a better explanation for the puzzles of the high stability and the contact angle of surface nanobubbles.

An equipment for Rayleigh scattering of Mössbauer radiation

NASA Astrophysics Data System (ADS)

Enescu, S. E.; Bibicu, I.; Zoran, V.; Kluger, A.; Stoica, A. D.; Tripadus, V.

1998-07-01

A personal computer driven equipment designed for Rayleigh scattering of Mössbauer radiation experiments at room temperature is described. The performances of the system were tested using like scatterers crystals with different mosaic divergences: lithium fluoride (LiF) and pyrolytic graphite (C). The equipment, suitable for any kind of Mössbauer scattering experiments, permits low and adjustable horizontal divergences of the incident beam. On décrit un équipement dédié aux mesures de diffusion Rayleigh de la radiation Mössbauer controlée par ordinateur. Les performances du système ont été testées sur des cristaux ayant des divergences de mosaïque différentes: le fluorure de lithium (LiF) et le graphite pyrolytique (C). L'équipement, qui peut être utilisé dans des différents types d'expérimentations basées sur la diffusion de la radiation Mössbauer, admet des divergences horizontales du faisceau incident faibles et réglables.

Quantized edge modes in atomic-scale point contacts in graphene.

PubMed

Kinikar, Amogh; Phanindra Sai, T; Bhattacharyya, Semonti; Agarwala, Adhip; Biswas, Tathagata; Sarker, Sanjoy K; Krishnamurthy, H R; Jain, Manish; Shenoy, Vijay B; Ghosh, Arindam

2017-07-01

The zigzag edges of single- or few-layer graphene are perfect one-dimensional conductors owing to a set of gapless states that are topologically protected against backscattering. Direct experimental evidence of these states has been limited so far to their local thermodynamic and magnetic properties, determined by the competing effects of edge topology and electron-electron interaction. However, experimental signatures of edge-bound electrical conduction have remained elusive, primarily due to the lack of graphitic nanostructures with low structural and/or chemical edge disorder. Here, we report the experimental detection of edge-mode electrical transport in suspended atomic-scale constrictions of single and multilayer graphene created during nanomechanical exfoliation of highly oriented pyrolytic graphite. The edge-mode transport leads to the observed quantization of conductance close to multiples of G 0  = 2e 2 /h. At the same time, conductance plateaux at G 0 /2 and a split zero-bias anomaly in non-equilibrium transport suggest conduction via spin-polarized states in the presence of an electron-electron interaction.

A Novel Method for Fabricating Wearable, Piezoresistive, and Pressure Sensors Based on Modified-Graphite/Polyurethane Composite Films

PubMed Central

He, Yin; Li, Wei; Yang, Guilin; Liu, Hao; Lu, Junyu; Zheng, Tongtong; Li, Xiaojiu

2017-01-01

A wearable, low-cost, highly repeatable piezoresistive sensor was fabricated by the synthesis of modified-graphite and polyurethane (PU) composites and polydimethylsiloxane (PDMS). Graphite sheets functionalized by using a silane coupling agent (KH550) were distributed in PU/N,N-dimethylformamide (DMF) solution, which were then molded to modified-graphite/PU (MG/PU) composite films. Experimental results show that with increasing modified-graphite content, the tensile strength of the MG/PU films first increased and then decreased, and the elongation at break of the composite films showed a decreasing trend. The electrical conductivity of the composite films can be influenced by filler modification and concentration, and the percolation threshold of MG/PU was 28.03 wt %. Under liner uniaxial compression, the 30 wt % MG/PU composite films exhibited 0.274 kPa−1 piezoresistive sensitivity within the range of low pressure, and possessed better stability and hysteresis. The flexible MG/PU composite piezoresistive sensors have great potential for body motion, wearable devices for human healthcare, and garment pressure testing. PMID:28773047

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

Fedrigo, Anna, E-mail: anna.fedrigo@nbi.ku.dk; Istituto dei Sistemi Complessi, Consiglio Nazionale delle Ricerche, 50019 Sesto Fiorentino; European Spallation Source ESS AB, SE-221 00 Lund

VESPA, Vibrational Excitation Spectrometer with Pyrolytic-graphite Analysers, aims to probe molecular excitations via inelastic neutron scattering. It is a thermal high resolution inverted geometry time-of-flight instrument designed to maximise the use of the long pulse of the European Spallation Source. The wavelength frame multiplication technique was applied to provide simultaneously a broad dynamic range (about 0-500 meV) while a system of optical blind choppers allows to trade flux for energy resolution. Thanks to its high flux, VESPA will allow the investigation of dynamical and in situ experiments in physical chemistry. Here we describe the design parameters and the corresponding McStasmore » simulations.« less

Pulsed Laser Ablation Synthesis of Diamond Molecules in Supercritical Fluids

NASA Astrophysics Data System (ADS)

Nakahara, Sho; Stauss, Sven; Miyazoe, Hiroyuki; Shizuno, Tomoki; Suzuki, Minoru; Kataoka, Hiroshi; Sasaki, Takehiko; Terashima, Kazuo

2010-09-01

Nanocarbon materials have been synthesized by pulsed laser ablation (532 nm; 52 J/cm2; 7 ns; 10 Hz) of highly oriented pyrolytic graphite in adamantane-dissolved supercritical xenon at a temperature T = 290.2 K and pressure p = 5.86 MPa. Micro-Raman spectroscopy of the products revealed the presence of hydrocarbons possessing sp3 hybridized bonds also found in diamond structures. The synthesis of diamantane was confirmed by gas chromatography-mass spectrometry. The same measurements also indicate the possible synthesis of other diamondoids up to octamantane. Thus, laser ablation in supercritical fluids is proposed as one practical method of synthesizing diamondoids.

Bias-induced conformational switching of supramolecular networks of trimesic acid at the solid-liquid interface

NASA Astrophysics Data System (ADS)

Ubink, J.; Enache, M.; Stöhr, M.

2018-05-01

Using the tip of a scanning tunneling microscope, an electric field-induced reversible phase transition between two planar porous structures ("chickenwire" and "flower") of trimesic acid was accomplished at the nonanoic acid/highly oriented pyrolytic graphite interface. The chickenwire structure was exclusively observed for negative sample bias, while for positive sample bias only the more densely packed flower structure was found. We suggest that the slightly negatively charged carboxyl groups of the trimesic acid molecule are the determining factor for this observation: their adsorption behavior varies with the sample bias and is thus responsible for the switching behavior.

Microcontact Printing Patterning of an HOPG Surface by an Inverse Electron Demand Diels-Alder Reaction.

PubMed

Zhu, Jun; Hiltz, Jonathan; Tefashe, Ushula M; Mauzeroll, Janine; Lennox, R Bruce

2018-06-21

The chemical modification of an sp 2 hybridized carbon surface in a controllable manner is very challenging but also crucial for many applications. An inverse electron demand Diels-Alder (IEDDA) reaction using microcontact printing technique is introduced to spatially control the modification of a highly ordered pyrolytic graphite (HOPG) surface under ambient conditions. The covalent modification was characterized by Raman spectroscopy, XPS, and SECM. Tetrazine derivatives can effectively react with an HOPG surface and with microcontact printing methods resulting in spatially patterned surfaces being produced with micrometer-scale resolution. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Sulfur redox reactions on nanostructured highly oriented pyrolytic graphite (HOPG) electrodes: Direct evidence for superior electrocatalytic performance on defect sites

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

Wang, Gongwei; Zheng, Dong; Liu, Dan

Fundamental research of sulfur redox reactions on well-defined controlled model electrode surfaces can provide new information to design high-performance lithium-sulfur batteries. In this paper, we study the electrochemical reduction and oxidation of sulfur on the nanostructured HOPG electrodes with pure basal planes, step plans, and pure edge planes. Finally, our results directly indicate that electrochemical reduction and oxidation of sulfur is significantly affected by the carbon surface structure, namely, the electrochemical reversibility of sulfur redox reaction is much better on edge plane, compared with basal plane and step plane.

Sulfur redox reactions on nanostructured highly oriented pyrolytic graphite (HOPG) electrodes: Direct evidence for superior electrocatalytic performance on defect sites

DOE PAGES

Wang, Gongwei; Zheng, Dong; Liu, Dan; ...

2017-04-28

Fundamental research of sulfur redox reactions on well-defined controlled model electrode surfaces can provide new information to design high-performance lithium-sulfur batteries. In this paper, we study the electrochemical reduction and oxidation of sulfur on the nanostructured HOPG electrodes with pure basal planes, step plans, and pure edge planes. Finally, our results directly indicate that electrochemical reduction and oxidation of sulfur is significantly affected by the carbon surface structure, namely, the electrochemical reversibility of sulfur redox reaction is much better on edge plane, compared with basal plane and step plane.

Towards vaporized molecular discrimination: a quartz crystal microbalance (QCM) sensor system using cobalt-containing mesoporous graphitic carbon.

PubMed

Tang, Jing; Torad, Nagy L; Salunkhe, Rahul R; Yoon, Jang-Hee; Al Hossain, Md Shahriar; Dou, Shi Xue; Kim, Jung Ho; Kimura, Tatsuo; Yamauchi, Yusuke

2014-11-01

A recent study on nanoporous carbon based materials (J. Am. Chem. Soc. 2012, 134, 2864) showed that the presence of abundant graphitized sp(2) carbon species in the frameworks led to higher affinity for aromatic hydrocarbons than their aliphatic analogues. Herein, improved understanding of the sensitive and selective detection of aromatic substances by using mesoporous carbon (MPC)-based materials, combined with a quartz crystal microbalance (QCM) sensor system, was obtained. MPCs were synthesized by direct carbonization of mesoporous polymers prepared from resol through a soft templating approach with Pluronic F127. The carbon-based frameworks can be graphitized through the addition of a cobalt source to the precursor solution, according to the catalytic activity of the cobalt nanoparticles formed during the carbonization process. From the Raman data, the degree of the graphitization was clearly increased by increasing the cobalt content and elevating the carbonization temperature. From a QCM study, it was proved that the highly graphitized MPCs exhibited a higher affinity for aromatic hydrocarbons than their aliphatic analogues. By increasing the degree of graphitization in the carbon-based pore walls, the MPCs showed both larger adsorption uptake and faster sensor response towards toxic benzene and toluene vapors. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Pencil graphite leads as simple amperometric sensors for microchip electrophoresis.

PubMed

Natiele Tiago da Silva, Eiva; Marques Petroni, Jacqueline; Gabriel Lucca, Bruno; Souza Ferreira, Valdir

2017-11-01

In this work we demonstrate, for the first time, the use of inexpensive commercial pencil graphite leads as simple amperometric sensors for microchip electrophoresis. A PDMS support containing one channel was fabricated through soft lithography and sanded pencil graphite leads were inserted into this channel to be used as working electrodes. The electrochemical and morphological characterization of the sensor was carried out. The graphite electrode was coupled to PDMS microchips in end-channel configuration and electrophoretic experiments were performed using nitrite and ascorbate as probe analytes. The analytes were successfully separated and detected in well-defined peaks with satisfactory resolution using the microfluidic platform proposed. The repeatability of the pencil graphite electrode was satisfactory (RSD values of 1.6% for nitrite and 12.3% for ascorbate, regarding the peak currents) and its lifetime was estimated to be ca. 700 electrophoretic runs over a cost of ca. $ 0.05 per electrode. The limits of detection achieved with this system were 2.8 μM for nitrite and 5.7 μM for ascorbate. For proof of principle, the pencil graphite electrode was employed for the real analysis of well water samples and nitrite was successfully quantified at levels below its maximum contaminant level established in Brazil and US. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Tellurium speciation analysis using hydride generation in situ trapping electrothermal atomic absorption spectrometry and ruthenium or palladium modified graphite tubes.

PubMed

Yildirim, Emrah; Akay, Pınar; Arslan, Yasin; Bakirdere, Sezgin; Ataman, O Yavuz

2012-12-15

Speciation of tellurium can be achieved by making use of different kinetic behaviors of Te(IV) and Te(VI) upon their reaction with sodium borohydride using hydride generation. While Te(IV) can form H(2)Te, Te(VI) will not form any volatile species during the course of hydride formation and measurement by atomic absorption spectrometry. Quantitative reduction of Te(VI) was achieved through application of a microwave assisted prereduction of Te(VI) in 6.0 mol/L HCl solution. Enhanced sensitivity was achieved by in situ trapping of the generated H(2)Te species in a previously heated graphite furnace whose surface was modified using Pd or Ru. Overall efficiency for in situ trapping in pyrolytically coated graphite tube surface was found to be 15% when volatile analyte species are trapped for 60s at 300°C. LOD and LOQ values were calculated as 0.086 ng/mL and 0.29 ng/mL, respectively. Efficiency was increased to 46% and 36% when Pd and Ru surface modifiers were used, respectively. With Ru modified graphite tube 173-fold enhancement was obtained over 180 s trapping period with respect to ETAAS; the tubes could be used for 250 cycles. LOD values were 0.0064 and 0.0022 ng/mL for Pd and Ru treated ETAAS systems, respectively, for 180 s collection of 9.6 mL sample solution. Copyright © 2012 Elsevier B.V. All rights reserved.

High heat flux Langmuir probe array for the DIII-D divertor platesa)

NASA Astrophysics Data System (ADS)

Watkins, J. G.; Taussig, D.; Boivin, R. L.; Mahdavi, M. A.; Nygren, R. E.

2008-10-01

Two modular arrays of Langmuir probes designed to handle a heat flux of up to 25 MW/m2 for 10 s exposures have been installed in the lower divertor target plates of the DIII-D tokamak. The 20 pyrolytic graphite probe tips have more than three times higher thermal conductivity and 16 times larger mass than the original DIII-D isotropic graphite probes. The probe tips have a fixed 12.5° surface angle to distribute the heat flux more uniformly than the previous 6 mm diameter domed collectors and a symmetric "rooftop" design to allow operation with reversed toroidal magnetic field. A large spring-loaded contact area improves heat conduction from each probe tip through a ceramic insulator into a cooled graphite divertor floor tile. The probe tips, brazed to molybdenum foil to ensure good electrical contact, are mounted in a ceramic tray for electrical isolation and reliable cable connections. The new probes are located 1.5 cm radially apart in a staggered arrangement near the entrance to the lower divertor pumping baffle and are linearly spaced 3 cm apart on the shelf above the in-vessel cryopump. Typical target plate profiles of Jsat, Te, and Vf with 4 mm spatial resolution are shown.

Epitaxial Growth of Aligned and Continuous Carbon Nanofibers from Carbon Nanotubes.

PubMed

Lin, Xiaoyang; Zhao, Wei; Zhou, Wenbin; Liu, Peng; Luo, Shu; Wei, Haoming; Yang, Guangzhi; Yang, Junhe; Cui, Jie; Yu, Richeng; Zhang, Lina; Wang, Jiaping; Li, Qunqing; Zhou, Weiya; Zhao, Weisheng; Fan, Shoushan; Jiang, Kaili

2017-02-28

Exploiting the superior properties of nanomaterials at macroscopic scale is a key issue of nanoscience. Different from the integration strategy, "additive synthesis" of macroscopic structures from nanomaterial templates may be a promising choice. In this paper, we report the epitaxial growth of aligned, continuous, and catalyst-free carbon nanofiber thin films from carbon nanotube films. The fabrication process includes thickening of continuous carbon nanotube films by gas-phase pyrolytic carbon deposition and further graphitization of the carbon layer by high-temperature treatment. As-fabricated nanofibers in the film have an "annual ring" cross-section, with a carbon nanotube core and a graphitic periphery, indicating the templated growth mechanism. The absence of a distinct interface between the carbon nanotube template and the graphitic periphery further implies the epitaxial growth mechanism of the fiber. The mechanically robust thin film with tunable fiber diameters from tens of nanometers to several micrometers possesses low density, high electrical conductivity, and high thermal conductivity. Further extension of this fabrication method to enhance carbon nanotube yarns is also demonstrated, resulting in yarns with ∼4-fold increased tensile strength and ∼10-fold increased Young's modulus. The aligned and continuous features of the films together with their outstanding physical and chemical properties would certainly promote the large-scale applications of carbon nanofibers.

Electroanalytical applications of screen-printable surfactant-induced sol-gel graphite composites

DOEpatents

Guadalupe, Ana R.; Guo, Yizhu

2001-05-15

A process for preparing sol-gel graphite composite electrodes is presented. This process preferably uses the surfactant bis(2-ethylhexyl) sulfosuccinate (AOT) and eliminates the need for a cosolvent, an acidic catalyst, a cellulose binder and a thermal curing step from prior art processes. Fabrication of screen-printed electrodes by this process provides a simple approach for electroanalytical applications in aqueous and nonaqueous solvents. Examples of applications for such composite electrodes produced from this process include biochemical sensors such as disposable, single-use glucose sensors and ligand modified composite sensors for metal ion sensitive sensors.

Redox-dependent spatially resolved electrochemistry at graphene and graphite step edges.

PubMed

Güell, Aleix G; Cuharuc, Anatolii S; Kim, Yang-Rae; Zhang, Guohui; Tan, Sze-yin; Ebejer, Neil; Unwin, Patrick R

2015-04-28

The electrochemical (EC) behavior of mechanically exfoliated graphene and highly oriented pyrolytic graphite (HOPG) is studied at high spatial resolution in aqueous solutions using Ru(NH3)6(3+/2+) as a redox probe whose standard potential sits close to the intrinsic Fermi level of graphene and graphite. When scanning electrochemical cell microscopy (SECCM) data are coupled with that from complementary techniques (AFM, micro-Raman) applied to the same sample area, different time-dependent EC activity between the basal planes and step edges is revealed. In contrast, other redox couples (ferrocene derivatives) whose potential is further removed from the intrinsic Fermi level of graphene and graphite show uniform and high activity (close to diffusion-control). Macroscopic voltammetric measurements in different environments reveal that the time-dependent behavior after HOPG cleavage, peculiar to Ru(NH3)6(3+/2+), is not associated particularly with any surface contaminants but is reasonably attributed to the spontaneous delamination of the HOPG with time to create partially coupled graphene layers, further supported by conductive AFM measurements. This process has a major impact on the density of states of graphene and graphite edges, particularly at the intrinsic Fermi level to which Ru(NH3)6(3+/2+) is most sensitive. Through the use of an improved voltammetric mode of SECCM, we produce movies of potential-resolved and spatially resolved HOPG activity, revealing how enhanced activity at step edges is a subtle effect for Ru(NH3)6(3+/2+). These latter studies allow us to propose a microscopic model to interpret the EC response of graphene (basal plane and edges) and aged HOPG considering the nontrivial electronic band structure.

Ultralight anisotropic foams from layered aligned carbon nanotube sheets.

PubMed

Faraji, Shaghayegh; Stano, Kelly L; Yildiz, Ozkan; Li, Ang; Zhu, Yuntian; Bradford, Philip D

2015-10-28

In this work, we present large scale, ultralight aligned carbon nanotube (CNT) structures which have densities an order of magnitude lower than CNT arrays, have tunable properties and exhibit resiliency after compression. By stacking aligned sheets of carbon nanotubes and then infiltrating with a pyrolytic carbon (PyC), resilient foam-like materials were produced that exhibited complete recovery from 90% compressive strain. With density as low as 3.8 mg cm(-3), the foam structure is over 500 times less dense than bulk graphite. Microscopy revealed that PyC coated the junctions among CNTs, and also increased CNT surface roughness. These changes in the morphology explain the transition from inelastic behavior to foam-like recovery of the layered CNT sheet structure. Mechanical and thermal properties of the foams were tuned for different applications through variation of PyC deposition duration while dynamic mechanical analysis showed no change in mechanical properties over a large temperature range. Observation of a large and linear electrical resistance change during compression of the aligned CNT/carbon (ACNT/C) foams makes strain/pressure sensors a relevant application. The foams have high oil absorption capacities, up to 275 times their own weight, which suggests they may be useful in water treatment and oil spill cleanup. Finally, the ACNT/C foam's high porosity, surface area and stability allow for demonstration of the foams as catalyst support structures.

Interfacial nanobubbles on atomically flat substrates with different hydrophobicities.

PubMed

Wang, Xingya; Zhao, Binyu; Ma, Wangguo; Wang, Ying; Gao, Xingyu; Tai, Renzhong; Zhou, Xingfei; Zhang, Lijuan

2015-04-07

The dependence of the morphology of interfacial nanobubbles on atomically flat substrates with different wettability ranges was investigated by using PeakForce quantitative nanomechanics. Interfacial nanobubbles were formed and imaged on silicon nitride (Si3N4), mica, and highly ordered pyrolytic graphite (HOPG) substrates that were partly covered by reduced graphene oxide (rGO). The contact angles and sizes of those nanobubbles were measured under the same conditions. Nanobubbles with the same lateral width exhibited different heights on the different substrates, with the order Si3N4≈mica>rGO>HOPG, which is consistent with the trend of the hydrophobicity of the substrates. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Marcus-Hush-Chidsey theory of electron transfer to and from species bound at a non-uniform electrode surface: Theory and experiment

NASA Astrophysics Data System (ADS)

Henstridge, Martin C.; Batchelor-McAuley, Christopher; Gusmão, Rui; Compton, Richard G.

2011-11-01

Two simple models of electrode surface inhomogeneity based on Marcus-Hush theory are considered; a distribution in formal potentials and a distribution in electron tunnelling distances. Cyclic voltammetry simulated using these models is compared with that simulated using Marcus-Hush theory for a flat, uniform and homogeneous electrode surface, with the two models of surface inhomogeneity yielding broadened peaks with decreased peak-currents. An edge-plane pyrolytic graphite electrode is covalently modified with ferrocene via 'click' chemistry and the resulting voltammetry compared with each of the three previously considered models. The distribution of formal potentials is seen to fit the experimental data most closely.

Atomic Oxygen Energy in Low Frequency Hyperthermal Plasma Ashers

NASA Technical Reports Server (NTRS)

Banks, Bruce A.; Miller, Sharon K R.; Kneubel, Christian A.

2014-01-01

Experimental and analytical analysis of the atomic oxygen erosion of pyrolytic graphite as well as Monte Carlo computational modeling of the erosion of Kapton H (DuPont, Wilmington, DE) polyimide was performed to determine the hyperthermal energy of low frequency (30 to 35 kHz) plasma ashers operating on air. It was concluded that hyperthermal energies in the range of 0.3 to 0.9 eV are produced in the low frequency air plasmas which results in texturing similar to that in low Earth orbit (LEO). Monte Carlo computational modeling also indicated that such low energy directed ions are fully capable of producing the experimentally observed textured surfaces in low frequency plasmas.

Effect of mechanical and electrical stimuli in conductive atomic force microscopy with noble metal-coated tips

NASA Astrophysics Data System (ADS)

Zade, Vishal; Kang, Hung-Sen; Lee, Min Hwan

2018-01-01

Conductive atomic force microscopy has been widely employed to study the localized electrical properties of a wide range of substrates in non-vacuum conditions by the use of noble metal-coated tips. However, quantitative characterization of the electrical properties was often precluded by unpredictable changes in the tip apex morphology, and/or electronic transport characteristics of undesired oxide overcoats on the tip. In this paper, the impact of mechanical and electrical stimuli on the apex geometry of gold coated tips and electrical conduction properties at the tip-substrate contact is discussed by choosing gold and highly ordered pyrolytic graphite as the representative tip and substrate materials, respectively.

Measuring Ultrasonic Acoustic Velocity in a Thin Sheet of Graphite Epoxy Composite

NASA Technical Reports Server (NTRS)

2008-01-01

A method for measuring the acoustic velocity in a thin sheet of a graphite epoxy composite (GEC) material was investigated. This method uses two identical acoustic-emission (AE) sensors, one to transmit and one to receive. The delay time as a function of distance between sensors determines a bulk velocity. A lightweight fixture (balsa wood in the current implementation) provides a consistent method of positioning the sensors, thus providing multiple measurements of the time delay between sensors at different known distances. A linear fit to separation, x, versus delay time, t, will yield an estimate of the velocity from the slope of the line.

Skin inspired fractal strain sensors using a copper nanowire and graphite microflake hybrid conductive network.

PubMed

Jason, Naveen N; Wang, Stephen J; Bhanushali, Sushrut; Cheng, Wenlong

2016-09-22

This work demonstrates a facile "paint-on" approach to fabricate highly stretchable and highly sensitive strain sensors by combining one-dimensional copper nanowire networks with two-dimensional graphite microflakes. This paint-on approach allows for the fabrication of electronic skin (e-skin) patches which can directly replicate with high fidelity the human skin surface they are on, regardless of the topological complexity. This leads to high accuracy for detecting biometric signals for applications in personalised wearable sensors. The copper nanowires contribute to high stretchability and the graphite flakes offer high sensitivity, and their hybrid coating offers the advantages of both. To understand the topological effects on the sensing performance, we utilized fractal shaped elastomeric substrates and systematically compared their stretchability and sensitivity. We could achieve a high stretchability of up to 600% and a maximum gauge factor of 3000. Our simple yet efficient paint-on approach enabled facile fine-tuning of sensitivity/stretchability simply by adjusting ratios of 1D vs. 2D materials in the hybrid coating, and the topological structural designs. This capability leads to a wide range of biomedical sensors demonstrated here, including pulse sensors, prosthetic hands, and a wireless ankle motion sensor.

Eddy-Current Inspection Of Graphite-Fiber Composites

NASA Technical Reports Server (NTRS)

Workman, G. L.; Bryson, C. C.

1993-01-01

NASA technical memorandum describes initial research on, and proposed development of, automated system for nondestructive eddy-current inspection of parts made of graphite-fiber/epoxy-matrix composite materials. Sensors in system E-shaped or U-shaped eddy-current probes like those described in "Eddy-Current Probes For Inspecting Graphite-Fiber Composites" (MFS-26129).

Atomic Oxygen Fluence Monitor

NASA Technical Reports Server (NTRS)

Banks, Bruce A.

2011-01-01

This innovation enables a means for actively measuring atomic oxygen fluence (accumulated atoms of atomic oxygen per area) that has impinged upon spacecraft surfaces. Telemetered data from the device provides spacecraft designers, researchers, and mission managers with real-time measurement of atomic oxygen fluence, which is useful for prediction of the durability of spacecraft materials and components. The innovation is a compact fluence measuring device that allows in-space measurement and transmittance of measured atomic oxygen fluence as a function of time based on atomic oxygen erosion yields (the erosion yield of a material is the volume of material that is oxidized per incident oxygen atom) of materials that have been measured in low Earth orbit. It has a linear electrical response to atomic oxygen fluence, and is capable of measuring high atomic oxygen fluences (up to >10(exp 22) atoms/sq cm), which are representative of multi-year low-Earth orbital missions (such as the International Space Station). The durability or remaining structural lifetime of solar arrays that consist of polymer blankets on which the solar cells are attached can be predicted if one knows the atomic oxygen fluence that the solar array blanket has been exposed to. In addition, numerous organizations that launch space experiments into low-Earth orbit want to know the accumulated atomic oxygen fluence that their materials or components have been exposed to. The device is based on the erosion yield of pyrolytic graphite. It uses two 12deg inclined wedges of graphite that are over a grit-blasted fused silica window covering a photodiode. As the wedges erode, a greater area of solar illumination reaches the photodiode. A reference photodiode is also used that receives unobstructed solar illumination and is oriented in the same direction as the pyrolytic graphite covered photodiode. The short-circuit current from the photodiodes is measured and either sent to an onboard data logger, or transmitted to a receiving station on Earth. By comparison of the short-circuit currents from the fluence-measuring photodiode and the reference photodiode, one can compute the accumulated atomic oxygen fluence arriving in the direction that the fluence monitor is pointing. The device produces a signal that is linear with atomic oxygen fluence using a material whose atomic oxygen erosion yield has been measured over a period of several years in low-Earth orbit.

Graphite nanoplatelet enabled embeddable fiber sensor for in situ curing monitoring and structural health monitoring of polymeric composites.

PubMed

Luo, Sida; Liu, Tao

2014-06-25

A graphite nanoplatelet (GNP) thin film enabled 1D fiber sensor (GNP-FibSen) was fabricated by a continuous roll-to-roll spray coating process, characterized by scanning electron microscopy and Raman spectroscopy and evaluated by coupled electrical-mechanical tensile testing. The neat GNP-FibSen sensor shows very high gauge sensitivity with a gauge factor of ∼17. By embedding the sensor in fiberglass prepreg laminate parts, the dual functionalities of the GNP-FibSen sensor were demonstrated. In the manufacturing process, the resistance change of the embedded sensor provides valuable local resin curing information. After the manufacturing process, the same sensor is able to map the strain/stress states and detect the failure of the host composite. The superior durability of the embedded GNP-FibSen sensor has been demonstrated through 10,000 cycles of coupled electromechanical tests.

One-Step Pyrolytic Synthesis of Multiwalled Carbon Nanotubes: The Role of Resupply of Carbon Species on the Quality Control.

PubMed

Rajavel, Krishnamoorthy; Saravanan, Padmanapan; Kumar, Ramasamy Thangavelu Rajendra

2018-05-01

An investigation on varying experimental parameters such as solution quantity (2.5, 5 and 7.5 mL) and reaction time (15, 30, 45 and 60 min) was carried out for the production of high-quality multiwalled carbon nanotubes (MWCNTs) in one step pyrolysis. Structural analysis revealed the uniform diameter distribution and the length of nanotubes in the range of 60-80 nm and 0.4-2 μm, respectively. Raman and X-ray diffraction analysis showed a remarkable reduction in defect density with increase in graphitization degree, upon increasing the solution volume and reaction time. MWCNTs prepared at higher solution quantity (7.5 mL) with higher reaction time (60 min) showed higher crystallinity (70% graphitization) and lower defect density (ID/IG: 0.56). The attainment in equilibrium of evaporation cum precipitation in formation of high quality nanotubes structure is evaluated. An effective resupplying of condensed precursors by re-evaporation leads for the achievement of low defect density nanotubes with higher product yield is achieved.

Metal dependent motif transition in a self-assembled monolayer of bipyridine derivatives via coordination: An STM study.

PubMed

Wang, Yi; Yuan, Qunhui; Xu, Hongbo; Zhu, Xuefeng; Gan, Wei

2016-07-21

Low-dimensional molecular motifs with diversity developed via the on-surface chemistry are attracting growing interest for their potential in advanced nanofabrication. In this work, scanning tunneling microscopy was employed to investigate the in situ and ex situ metal coordinations between 4,4'-ditetradecyl-2,2'-bipyridine (bpy) and Zn(ii) or Cu(ii) ions at a highly oriented pyrolytic graphite (HOPG)/1-phenyloctane interface under ambient conditions. The results demonstrate that the bpy adopts a flat-lying orientation with its substituted alkyl chains in a tail-to-tail arrangement in a bpy monolayer. For the in situ coordination, the bpy/Zn(ii) and bpy/Cu(ii) complexes are aligned in edge-on fashions, wherein the bpy stands vertically on the HOPG surface and interdigitates at the alkyl chains. In the two-dimensional arrays of ex situ coordinated complexes, metal dependent motifs have been observed with Zn(ii) and Cu(ii), wherein the bipyridine moieties are parallel to the graphite surface. These results suggest that the desired on-surface coordination architectures may be achieved by the intentional selection of the metal centers.

Sb-Te alloy nanostructures produced on a graphite surface by a simple annealing process

NASA Astrophysics Data System (ADS)

Kuwahara, Masashi; Uratsuji, Hideaki; Abe, Maho; Sone, Hayato; Hosaka, Sumio; Sakai, Joe; Uehara, Yoichi; Endo, Rie; Tsuruoka, Tohru

2015-08-01

We have produced Sb-Te alloy nanostructures from a thin Sb2Te3 layer deposited on a highly oriented pyrolytic graphite substrate using a simple rf-magnetron sputtering and annealing technique. The size, shape, and chemical composition of the structures were investigated by scanning electron microscopy (SEM), atomic force microscopy (AFM), and energy dispersive X-ray spectrometry (EDX), respectively. The shape of the nanostructures was found to depend on the annealing temperature; nanoparticles appear on the substrate by annealing at 200 °C, while nanoneedles are formed at higher temperatures. Chemical composition analysis has revealed that all the structures were in the composition of Sb:Te = 1:3, Te rich compared to the target composition Sb2Te3, probably due to the higher movability of Te atoms on the substrate compared with Sb. We also tried to observe the production process of nanostructures in situ using SEM. Unfortunately, this was not possible because of evaporation in vacuum, suggesting that the formation of nanostructures is highly sensitive to the ambient pressure.

Macrosegregation of GeSi Alloys Grown in a Static Magnetic Field

NASA Technical Reports Server (NTRS)

Ritter, T. M.; Volz, M. P.; Cobb, S. D.; Szofran, F. R.

1999-01-01

Axial and radial macrosegregation profiles have been determined for GeSi alloy crystals grown by the vertical Bridgman technique. An axial 5 Tesla magnetic field was applied to several samples during growth to decrease the melt velocities by means of the Lorentz force. Compositions were measured with either energy dispersive X-ray spectroscopy (EDS) on a scanning electron microscope (SEM) or by wavelength dispersive X-ray spectroscopy (WDS) on a microprobe. The crystals were processed in graphite, hot-pressed boron nitride (BN), and pyrolytic boron nitride (PBN) ampoules, which produced various solid-liquid interface shapes during solidification. Those samples grown in a graphite ampoule exhibited radial profiles consistent with a highly concave interface and axial profiles indicative of complete mixing in the melt. The samples grown in BN and PBN ampoules had less radial variation. Axial macrosegregation profiles of these samples fell between the predictions for a completely mixed melt and one where solute transport is dominated by diffusion. Possible explanations for the apparent insufficiency of the magnetic field to achieve diffusion controlled growth conditions are discussed.

Electrochemical Functionalization of Graphene at the Nanoscale with Self-Assembling Diazonium Salts.

PubMed

Xia, Zhenyuan; Leonardi, Francesca; Gobbi, Marco; Liu, Yi; Bellani, Vittorio; Liscio, Andrea; Kovtun, Alessandro; Li, Rongjin; Feng, Xinliang; Orgiu, Emanuele; Samorì, Paolo; Treossi, Emanuele; Palermo, Vincenzo

2016-07-26

We describe a fast and versatile method to functionalize high-quality graphene with organic molecules by exploiting the synergistic effect of supramolecular and covalent chemistry. With this goal, we designed and synthesized molecules comprising a long aliphatic chain and an aryl diazonium salt. Thanks to the long chain, these molecules physisorb from solution onto CVD graphene or bulk graphite, self-assembling in an ordered monolayer. The sample is successively transferred into an aqueous electrolyte, to block any reorganization or desorption of the monolayer. An electrochemical impulse is used to transform the diazonium group into a radical capable of grafting covalently to the substrate and transforming the physisorption into a covalent chemisorption. During covalent grafting in water, the molecules retain the ordered packing formed upon self-assembly. Our two-step approach is characterized by the independent control over the processes of immobilization of molecules on the substrate and their covalent tethering, enabling fast (t < 10 s) covalent functionalization of graphene. This strategy is highly versatile and works with many carbon-based materials including graphene deposited on silicon, plastic, and quartz as well as highly oriented pyrolytic graphite.

The electrochemical performance of graphene modified electrodes: an analytical perspective.

PubMed

Brownson, Dale A C; Foster, Christopher W; Banks, Craig E

2012-04-21

We explore the use of graphene modified electrodes towards the electroanalytical sensing of various analytes, namely dopamine hydrochloride, uric acid, acetaminophen and p-benzoquinone via cyclic voltammetry. In line with literature methodologies and to investigate the full-implications of employing graphene in this electrochemical context, we modify electrode substrates that exhibit either fast or slow electron transfer kinetics (edge- or basal- plane pyrolytic graphite electrodes respectively) with well characterised commercially available graphene that has not been chemically treated, is free from surfactants and as a result of its fabrication has an extremely low oxygen content, allowing the true electroanalytical applicability of graphene to be properly de-convoluted and determined. In comparison to the unmodified underlying electrode substrates (constructed from graphite), we find that graphene exhibits a reduced analytical performance in terms of sensitivity, linearity and observed detection limits towards each of the various analytes studied within. Owing to graphene's structural composition, low proportion of edge plane sites and consequent slow heterogeneous electron transfer rates, there appears to be no advantages, for the analytes studied here, of employing graphene in this electroanalytical context.

Electrochemical Control of Peptide Self-Organization on Atomically Flat Solid Surfaces: A Case Study with Graphite.

PubMed

Seki, Takakazu; So, Christopher R; Page, Tamon R; Starkebaum, David; Hayamizu, Yuhei; Sarikaya, Mehmet

2018-02-06

The nanoscale self-organization of biomolecules, such as proteins and peptides, on solid surfaces under controlled conditions is an important issue in establishing functional bio/solid soft interfaces for bioassays, biosensors, and biofuel cells. Electrostatic interaction between proteins and surfaces is one of the most essential parameters in the adsorption and self-assembly of proteins on solid surfaces. Although the adsorption of proteins has been studied with respect to the electrochemical surface potential, the self-assembly of proteins or peptides forming well-organized nanostructures templated by lattice structure of the solid surfaces has not been studied in the relation to the surface potential. In this work, we utilize graphite-binding peptides (GrBPs) selected by the phage display method to investigate the relationship between the electrochemical potential of the highly ordered pyrolytic graphite (HOPG) and peptide self-organization forming long-range-ordered structures. Under modulated electrical bias, graphite-binding peptides form various ordered structures, such as well-ordered nanowires, dendritic structures, wavy wires, amorphous (disordered) structures, and islands. A systematic investigation of the correlation between peptide sequence and self-organizational characteristics reveals that the presence of the bias-sensitive amino acid modules in the peptide sequence has a significant effect on not only surface coverage but also on the morphological features of self-assembled structures. Our results show a new method to control peptide self-assembly by means of applied electrochemical bias as well as peptide design-rules for the construction of functional soft bio/solid interfaces that could be integrated in a wide range of practical implementations.

Spectroscopic investigation of the wettability of multilayer graphene using highly ordered pyrolytic graphite as a model material.

PubMed

Ashraf, Ali; Wu, Yanbin; Wang, Michael C; Aluru, Narayana R; Dastgheib, Seyed A; Nam, SungWoo

2014-11-04

We report the intrinsic water contact angle (WCA) of multilayer graphene, explore different methods of cleaning multilayer graphene, and evaluate the efficiency of those methods on the basis of spectroscopic analysis. Highly ordered pyrolytic graphite (HOPG) was used as a model material system to study the wettability of the multilayer graphene surface by WCA measurements. A WCA value of 45° ± 3° was measured for a clean HOPG surface, which can serve as the intrinsic WCA for multilayer graphene. A 1 min plasma treatment (100 W) decreased the WCA to 6°, owing to the creation of surface defects and functionalization by oxygen-containing groups. Molecular dynamics simulations of water droplets on the HOPG surface with or without the oxygen-containing defect sites confirmed the experimental results. Heat treatment at near atmospheric pressure and wet chemical cleaning methods using hydrofluoric acid and chloroform did not change the WCA significantly. Low-pressure, high-temperature annealing under argon and hydrogen reduced the WCA to 54°, close to the intrinsic WCA of HOPG. Raman spectroscopy and atomic force microscopy did not show any significant change for the HOPG surface after this treatment, confirming low-pressure, high-temperature annealing as an effective technique to clean multilayer graphene without damaging the surface. Time-of-flight secondary ion mass spectrometry indicated the existence of hydrocarbon species on the surface of the HOPG sample that was exposed to air for <5 min and the absence of these impurities in the bulk. X-ray photoelectron spectroscopy analyses of the sample surfaces after the different cleaning techniques were performed to correlate the WCA to the surface chemistry. X-ray photoelectron spectroscopy results revealed that the WCA value changed drastically, depending on the amounts of oxygen-containing and hydrocarbon-containing groups on the surface.

Sound velocities in highly oriented pyrolytic graphite shocked to 18 GPa: Orientational order dependence and elastic instability

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

Lucas, Marcel; Winey, J. M.; Gupta, Y. M.

Previous reports of rapid phase transformation above 18 GPa [Erskine and Nellis, Nature 349, 317 (1991)] and large elastic waves below 18 GPa [Lucas et al., J. Appl. Phys. 114, 093515 (2013)] for shock-compressed ZYB-grade highly-oriented pyrolytic graphite (HOPG), but not for less oriented ZYH-grade HOPG, indicated a link between the orientational order dependence of the HOPG response above and below the phase transformation stress. To gain insight into this link and into the mechanical response of HOPG shocked to peak stresses approaching the phase transformation onset, the compressibility of ZYB- and ZYH-grade HOPG in the shocked state was examinedmore » using front surface impact experiments. Particle velocity histories and sound velocities were measured for peak stresses reaching 18 GPa. Although the locus of the measured peak stress-particle velocity states is indistinguishable for the two grades of HOPG, the measured sound velocities in the peak state reveal significant differences between the two grades. Specifically, 1) The measured sound velocities are somewhat higher for ZYH-grade HOPG, compared to ZYB-grade HOPG. 2) The measured sound velocities for ZYH-grade HOPG increase smoothly with compression, whereas those for ZYB-2 grade HOPG exhibit a significant reduction in the compression dependence from 12 GPa to 17 GPa and an abrupt increase from 17 GPa to 18 GPa. 3) The longitudinal moduli, determined from the measured sound velocities, are smaller than the calculated bulk moduli for ZYB-grade HOPG shocked to peak stresses above 15 GPa, indicating the onset of an elastic instability. The present findings demonstrate that the softening of the longitudinal modulus (or elastic instability) presented here is linked to the large elastic waves and the rapid phase transformation reported previously – all observed only for shocked ZYB-grade HOPG. The elastic instability in shocked ZYB-grade HOPG is likely a precursor to the rapid phase transformation observed above 18 GPa for this HOPG grade.« less

Sound velocities in highly oriented pyrolytic graphite shocked to 18 GPa: Orientational order dependence and elastic instability

DOE PAGES

Lucas, Marcel; Winey, J. M.; Gupta, Y. M.

2015-12-28

Previous reports of rapid phase transformation above 18 GPa [Erskine and Nellis, Nature 349, 317 (1991)] and large elastic waves below 18 GPa [Lucas et al., J. Appl. Phys. 114, 093515 (2013)] for shock-compressed ZYB-grade highly-oriented pyrolytic graphite (HOPG), but not for less oriented ZYH-grade HOPG, indicated a link between the orientational order dependence of the HOPG response above and below the phase transformation stress. To gain insight into this link and into the mechanical response of HOPG shocked to peak stresses approaching the phase transformation onset, the compressibility of ZYB- and ZYH-grade HOPG in the shocked state was examinedmore » using front surface impact experiments. Particle velocity histories and sound velocities were measured for peak stresses reaching 18 GPa. Although the locus of the measured peak stress-particle velocity states is indistinguishable for the two grades of HOPG, the measured sound velocities in the peak state reveal significant differences between the two grades. Specifically, 1) The measured sound velocities are somewhat higher for ZYH-grade HOPG, compared to ZYB-grade HOPG. 2) The measured sound velocities for ZYH-grade HOPG increase smoothly with compression, whereas those for ZYB-2 grade HOPG exhibit a significant reduction in the compression dependence from 12 GPa to 17 GPa and an abrupt increase from 17 GPa to 18 GPa. 3) The longitudinal moduli, determined from the measured sound velocities, are smaller than the calculated bulk moduli for ZYB-grade HOPG shocked to peak stresses above 15 GPa, indicating the onset of an elastic instability. The present findings demonstrate that the softening of the longitudinal modulus (or elastic instability) presented here is linked to the large elastic waves and the rapid phase transformation reported previously – all observed only for shocked ZYB-grade HOPG. The elastic instability in shocked ZYB-grade HOPG is likely a precursor to the rapid phase transformation observed above 18 GPa for this HOPG grade.« less

Ultra-facile fabrication of phosphorus doped egg-like hierarchic porous carbon with superior supercapacitance performance by microwave irradiation combining with self-activation strategy

NASA Astrophysics Data System (ADS)

Zhang, Deyi; Han, Mei; Li, Yubing; He, Jingjing; Wang, Bing; Wang, Kunjie; Feng, Huixia

2017-12-01

Herein, we report an ultra-facile fabrication method for a phosphorus doped egg-like hierarchic porous carbon by microwave irradiation combining with self-activation strategy under air atmosphere. Comparing with the traditional pyrolytic carbonization method, the reported method exhibits incomparable merits, such as high energy efficiency, ultra-fast and inert atmosphere protection absent fabrication process. Similar morphology and graphitization degree with the sample fabricated by the traditional pyrolytic carbonization method under inert atmosphere protection for 2 h can be easily achieved by the reported microwave irradiation method just for 3 min under ambient atmosphere. The samples fabricated by the reported method display a unique phosphorus doped egg-like hierarchic porous structure, high specific surface area (1642 m2 g-1) and large pore volume (2.04 cm3 g-1). Specific capacitance of the samples fabricated by the reported method reaches up to 209 F g-1, and over 96.2% of initial capacitance remains as current density increasing from 0.5 to 20 A g-1, indicating the superior capacitance performance of the fabricated samples. The hierarchic porous structure, opened microporosity, additional pseudocapacitance, high electrolyte-accessible surface area and good conductivity make essential contribution to its superior capacitance performance.

Nucleation, aggregative growth and detachment of metal nanoparticles during electrodeposition at electrode surfaces.

PubMed

Lai, Stanley C S; Lazenby, Robert A; Kirkman, Paul M; Unwin, Patrick R

2015-02-01

The nucleation and growth of metal nanoparticles (NPs) on surfaces is of considerable interest with regard to creating functional interfaces with myriad applications. Yet, key features of these processes remain elusive and are undergoing revision. Here, the mechanism of the electrodeposition of silver on basal plane highly oriented pyrolytic graphite (HOPG) is investigated as a model system at a wide range of length scales, spanning electrochemical measurements from the macroscale to the nanoscale using scanning electrochemical cell microscopy (SECCM), a pipette-based approach. The macroscale measurements show that the nucleation process cannot be modelled as either truly instantaneous or progressive, and that step edge sites of HOPG do not play a dominant role in nucleation events compared to the HOPG basal plane, as has been widely proposed. Moreover, nucleation numbers extracted from electrochemical analysis do not match those determined by atomic force microscopy (AFM). The high time and spatial resolution of the nanoscale pipette set-up reveals individual nucleation and growth events at the graphite basal surface that are resolved and analysed in detail. Based on these results, corroborated with complementary microscopy measurements, we propose that a nucleation-aggregative growth-detachment mechanism is an important feature of the electrodeposition of silver NPs on HOPG. These findings have major implications for NP electrodeposition and for understanding electrochemical processes at graphitic materials generally.

Parallel Microcracks-based Ultrasensitive and Highly Stretchable Strain Sensors.

PubMed

Amjadi, Morteza; Turan, Mehmet; Clementson, Cameron P; Sitti, Metin

2016-03-02

There is an increasing demand for flexible, skin-attachable, and wearable strain sensors due to their various potential applications. However, achieving strain sensors with both high sensitivity and high stretchability is still a grand challenge. Here, we propose highly sensitive and stretchable strain sensors based on the reversible microcrack formation in composite thin films. Controllable parallel microcracks are generated in graphite thin films coated on elastomer films. Sensors made of graphite thin films with short microcracks possess high gauge factors (maximum value of 522.6) and stretchability (ε ≥ 50%), whereas sensors with long microcracks show ultrahigh sensitivity (maximum value of 11,344) with limited stretchability (ε ≤ 50%). We demonstrate the high performance strain sensing of our sensors in both small and large strain sensing applications such as human physiological activity recognition, human body large motion capturing, vibration detection, pressure sensing, and soft robotics.

Sheath-Core Graphite/Silk Fiber Made by Dry-Meyer-Rod-Coating for Wearable Strain Sensors.

PubMed

Zhang, Mingchao; Wang, Chunya; Wang, Qi; Jian, Muqiang; Zhang, Yingying

2016-08-17

Recent years have witnessed the explosive development of flexible strain sensors. Nanomaterials have been widely utilized to fabricate flexible strain sensors, because of their high flexibility and electrical conductivity. However, the fabrication processes for nanomaterials and the subsequent strain sensors are generally complicated and are manufactured at high cost. In this work, we developed a facile dry-Meyer-rod-coating process to fabricate sheath-core-structured single-fiber strain sensors using ultrafine graphite flakes as the sheath and silk fibers as the core by virtue of their flexibility, high production, and low cost. The fabricated strain sensor exhibits a high sensitivity with a gauge factor of 14.5 within wide workable strain range up to 15%, and outstanding stability (up to 3000 cycles). The single-fiber-based strain sensors could be attached to a human body to detect joint motions or easily integrated into the multidirectional strain sensor for monitoring multiaxial strain, showing great potential applications as wearable strain sensors.

Electrochemical exfoliation of graphite to stage-III graphite bisulfate flakes in low concentration sulfuric acid solution: A novel synthesis route to completely trilayer graphene suspension

NASA Astrophysics Data System (ADS)

Mir, Afkham; Shukla, Anupam

2018-06-01

Graphene produced from electrochemical exfoliation of graphite show a scatter in the number of layers. This scatter is a serious drawback for sensor and opto-electronic applications since the electronic properties of graphene change with number of layers. The scatter in the layer number of graphene is caused by formation of the intermediate graphite intercalation compounds (GIC) of different stage numbers as well as simultaneous cleaving of the GICs in the dispersion-unsuitable aqueous environment. In this work, we show the synthesis of stage-III graphite bisulfate (GB) enriched flakes by electrochemical exfoliation of graphite in low concentration (0.1 M) sulfuric acid from two different routes. We further show that the intercalated bisulfate planes provide sites for selective cleaving of the GB particles to trilayer graphene in DMF, a solvent favorable for graphene dispersion. Morphological characterizations show that while GB particles from one of the routes give graphene with a small scatter in the layer numbers, the other route provides a completely trilayer graphene dispersion. TEM and optical micrographs show graphene flakes have linear dimensions of several micrometers and a low aspect ratio suitable for use in sensor applications.

Deducing 2D crystal structure at the liquid/solid interface with atomic resolution: a combined STM and SFG study.

PubMed

McClelland, Arthur A; Ahn, Seokhoon; Matzger, Adam J; Chen, Zhan

2009-11-17

Sum frequency generation vibrational spectroscopy (SFG) has been applied to study two-dimensional (2D) crystals formed by an isophthalic acid diester on the surface of highly oriented pyrolytic graphite, providing complementary measurements to scanning tunneling microscopy (STM) and computational modeling. SFG results indicate that both aromatic and C=O groups in the 2D crystal tilt from the surface. This study demonstrates that a combination of SFG and STM techniques can be used to gain a more complete picture of 2D crystal structure, and it is necessary to consider solvent-2D crystal interactions and dynamics in the computer models to achieve an accurate representation of interfacial structure.

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

Hoenig, M.; Elsen, Y.V.; Cauter, R.V.

The progressive degradation of the pyrolytic graphite surface of atomizers provides variable and misleading results of molybdenum peak-height measurements. The changes in the peak shapes produce no analytical problems during the lifetime of the atomizer (approx.300 firings) when integrated absorbance (A.s signals) is considered and the possible base-line drifts are controlled. This was demonstrated on plant samples mineralized by simple digestion with a mixture of HNO/sub 3/ and H/sub 2/O/sub 2/. The value of this method was assessed by comparison with a standard dry oxidation method and by molybdenum determination in National Bureau of Standards reference plant samples. The relativemore » standard deviations (n = 5) of the full analytical procedure do not exceed 7%. 13 references, 3 figures, 3 tables.« less

Supercooling of Hydrogen on Template Materials to Deterministically Seed Ignition-Quality Solid Fuel Layers

DOE PAGES

Shin, S. J.; Zepeda-Ruiz, L. A.; Lee, J. R. I.; ...

2016-09-01

In this study, we explored templating effects of various materials for hydrogen (H 2 and D 2) solidification by measuring the degree of supercooling required for liquid hydrogen to solidify below each triple point. The results show high supercooling (>100 mK) for most metallic, covalent, and ionic solids, and low supercooling (<100 mK) for van der Waals (vdW) solids. We attribute the low supercooling of vdW solids to the weak interaction of the substrate and hydrogen. Highly ordered pyrolytic graphite showed the lowest supercooling among materials that are solid at room temperature, but did not exhibit a templating effect withinmore » a fill-tube and capsule assembly.« less

Chiral symmetry breaking during the self-assembly of monolayers from achiral purine molecules.

PubMed

Sowerby, S J; Heckl, W M; Petersen, G B

1996-11-01

Scanning tunneling microscopy was used to investigate the structure of the two-dimensional adsorbate formed by molecular self-assembly of the purine base, adenine, on the surfaces of the naturally occurring mineral molybdenite and the synthetic crystal highly oriented pyrolytic graphite. Although formed from adenine, which is achiral, the observed adsorbate surface structures were enantiomorphic on molybdenite. This phenomenon suggests a mechanism for the introduction of a localized chiral symmetry break by the spontaneous crystallization of these prebiotically available molecules on inorganic surfaces and may have some role in the origin of biomolecular optical asymmetry. The possibility that purine-pyrimidine arrays assembled on naturally occurring mineral surfaces might act as possible templates for biomolecular assembly is discussed.

Bandgap engineering through nanocrystalline magnetic alloy grafting on reduced graphene oxide.

PubMed

De, D; Chakraborty, M; Majumdar, S; Giri, S

2014-09-28

High conductivity and the absence of ferromagnetism in pristine graphene fail to satisfy primary criteria for possible technological application in spintronics. Opening of the bandgap in graphene is primarily desirable for such applications. We report a simplified and novel approach of controlled grafting of a magnetic alloy on reduced graphene oxide. This eventually leads to ferromagnetism of the stable hybrid material at room temperature, with a large moment (∼1.2 μB) and a remarkable decrease in conductivity (∼10 times) compared to highly ordered pyrolytic graphite. Our model band-structure calculation indicates that the combined effect of controlled vacancies and impurities attributed to the nanocrystalline alloy grafting leads to a promising step toward band gap engineering.

Structural Transformation of Guanine Coordination Motifs in Water Induced by Metal ions and Temperature.

PubMed

Li, Wei; Jin, Jing; Liu, Xiaoqing; Wang, Li

2018-06-15

The transformation effects of metal ions and temperature on the DNA bases guanine (G) metal-organic coordination motifs in water have been investigated by scanning tunneling microcopy (STM). The G molecules form an ordered hydrogen-bonded structure at the water- highly oriented pyrolytic graphite (HOPG) interface. The STM observations reveal that the canonical G/9H form can be transformed into the G/(3H, 7H) tautomer by increasing the temperature of the G solution to 38.6oC. Moreover, metal ions bind with G molecules to form G4Fe13+, G3Fe32+ and the heterochiral intermixed G4Na1+ metal-organic networks after the introduction of the alkali-metal ions in cellular environment.

Nanoscale multiple gaseous layers on a hydrophobic surface.

PubMed

Zhang, Lijuan; Zhang, Xuehua; Fan, Chunhai; Zhang, Yi; Hu, Jun

2009-08-18

The nanoscale gas state at the interfaces of liquids (water, acid, and salt solutions) and highly oriented pyrolytic graphite (HOPG) was investigated via tapping-mode atomic force microscopy (AFM). For the first time, we report that the interfacial gases could form bilayers and trilayers, i.e., on the top of a flat gas layer, there are one or two more gas layers. The formation of these gas layers could be induced by a local supersaturation of gases, which can be achieved by (1) temperature difference between the liquids and the HOPG substrates or (2) exchange ethanol with water. Furthermore, we found that the gas layers were less stable than spherical bubbles. They could transform to bubbles with time or under the perturbation of the AFM tip.

A fluorescent sensor for selective detection of cyanide using mesoporous graphitic carbon(IV) nitride.

PubMed

Lee, Eun Zoo; Lee, Sun Uk; Heo, Nam-Su; Stucky, Galen D; Jun, Young-Si; Hong, Won Hi

2012-04-25

A turn-on fluorescence sensor, Cu(2+)-c-mpg-C(3)N(4), was developed for detection of CN(-) in aqueous solution by simply mixing cubic mesoporous graphitic carbon nitride (c-mpg-C(3)N(4)) and aqueous solution of Cu(NO(3))(2). The highly sensitive detection of CN(-) with a detection limit of 80 nM is not only possible in aqueous solution but also in human blood serum.

Recent Advances in Preparation, Structure, Properties and Applications of Graphite Oxide.

PubMed

Srivastava, Suneel Kumar; Pionteck, Jürgen

2015-03-01

Graphite oxide, also referred as graphitic oxide or graphitic acid, is an oxidized bulk product of graphite with a variable composition. However, it did not receive immense attention until it was identified as an important and easily obtainable precursor for the preparation of graphene. This inspired many researchers to explore facts related to graphite oxide in exploiting its fascinating features. The present article culminates up-dated review on different preparative methods, morphology and characterization of physical/chemical properties of graphite oxide by XRD, XPS, FTIR, Raman, NMR, UV-visible, and DRIFT analyses. Finally, recent developments on intercalation and applications of GO in multifaceted areas of catalysis, sensor, supercapacitors, water purification, hydrogen storage and magnetic shielding etc. has also been reviewed.

Strain and dynamic measurements using fiber optic sensors embedded into graphite/epoxy tubes

NASA Technical Reports Server (NTRS)

Dehart, D. W.; Doederlein, T.; Koury, J.; Rogowski, R. S.; Heyman, J. S.; Holben, M. S., Jr.

1989-01-01

Graphite/epoxy tubes were fabricated with embedded optical fibers to evaluate the feasibility of monitoring strains with a fiber optic technique. Resistance strain gauges were attached to the tubes to measure strain at four locations along the tube for comparison with the fiber optic sensors. Both static and dynamic strain measurements were made with excellent agreement between the embedded fiber optic strain sensor and the strain gauges. Strain measurements of 10(exp -7) can be detected with the optical phase locked loop (OPLL) system using optical fiber. Because of their light weight, compatibility with composites, immunity to electromagnetic interference, and based on the static and dynamic results obtained, fiber optic sensors embedded in composites may be useful as the sensing component of smart structures.

Vaporization thermodynamics of K2S and K2SO3

NASA Technical Reports Server (NTRS)

Bennet, J. E.

1982-01-01

The vaporization reactions, vapor pressures, and thermodynamics of potassium sulfide and potassium sulfite were studied for purposes of providing fundamental data for the seed cycle in magnetohydrodynamic electric power generation. Rate of effusion studies, supported by tube furnace experiments, X-ray powder diffraction, mass spectrometry and appropriate chemical analyses and tests, revealed that potassium sulfite disproportionates at high temperatures to form potassium sulfide and potassium sulfate. Potassium sulfide was observed to vaporize incongruently, the initial vapors beng predominantly potassium atoms, with minor species being S2 and various K-S molecules. The ratio of K/S2 in the vapor is very large initially and decreases steadily with prolonged heating. Several materials were evaluated for purposes of containing K2S/K2SO3 at temperatures or = 800 C: Pt, Mo, W, quartz, machinable glass, BN, high density graphite, pyrolytic coated graphite, and alumina. Of these, only alumina was observed to be chemically inert to both K2S but reacted with K2SO3. The other materials were not suitable for either substance. Thermodynamic calculations based on measured vapor pressures and approximate free energy functions are described. Results from isothermal total mass loss experiments and from thermogravimetric experiments are also included.

Comparison of VVV Auger electron spectra from single and multilayer graphene and graphite.

NASA Astrophysics Data System (ADS)

Chirayath, V. A.; Callewaert, V.; Fairchild, A. J.; Chrysler, M. D.; Gladen, R. W.; Imam, S. K.; Koymen, A. R.; Saniz, R.; Barbiellini, B.; Rajeshwar, K.; Partoens, B.; Weiss, A. H.

A direct observation of a low energy electron peak in the positron annihilation induced Auger electron spectra (PAES) from a single layer of graphene was made recently. A low energy positron beam (<1.25 eV) was used to deposit the positron on single layer graphene on a Cu substrate and the low energy peak was designated as VVV following the X-ray notation. The PAES signal is almost entirely from the top graphene layer due to the trapping of positrons in the image potential well on the surface of graphene. We utilize this monolayer sensitivity of PAES to compare the shape of the VVV Auger peak from the single layer graphene to the shapes of the VVV Auger peak obtained from multilayer graphene on Cu and from highly oriented pyrolytic graphite (HOPG). The VVV Auger peak from multilayer graphene on Cu and HOPG shows a systematic shift towards lower energies relative to the VVV Auger peak from the single layer graphene. The influence of the hole-hole interaction in distorting and shifting the VVV Auger spectra are discussed in relation to this observed shift. NSF Grant No. DMR 1508719 and DMR 1338130.

Facilitation of NADH Electrooxidation at Treated Carbon Nanotubes

PubMed Central

Wooten, Marilyn; Gorski, Waldemar

2010-01-01

The relationship between the state of the surface of carbon nanotubes (CNT) and their electrochemical activity was investigated using the enzyme cofactor dihydronicotinamide adenine dinucleotide (NADH) as a redox probe. The boiling of CNT in water, while nondestructive, activated them toward the oxidation of NADH as indicated by a shift in the anodic peak potential of NADH (ENADH) from 0.4 to 0.0 V. The shift in ENADH was due to the redox mediation of NADH oxidation by traces of quinone species that were formed on the surface of treated CNT. The harsher treatment that comprised of microwaving of CNT in concentrated nitric acid had a similar effect on the ENADH and, additionally, it increased the anodic peak current of NADH. The latter correlated with the formation of defects on the surface of acid-microwaved CNT as indicated by their Raman spectra. The increase in current was discussed considering a role of surface mediators on the buckled graphene sheets of acid-microwaved CNT. The other carbon allotropes including the edge plane pyrolytic graphite, graphite powder, and glassy carbon did not display a comparable activation toward the oxidation of NADH. PMID:20088562

Development of a Scanning Microscale Fast Neutron Irradiation Platform for Examining the Correlation Between Local Neutron Damage and Graphite Microstructure

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

Pinhero, Patrick; Windes, William

2015-03-10

The fast particle radiation damage effect of graphite, a main material in current and future nuclear reactors, has significant influence on the utilization of this material in fission and fusion plants. Atoms on graphite crystals can be easily replaced or dislocated by fast protons and result in interstitials and vacancies. The currently accepted model indicates that after most of the interstitials recombine with vacancies, surviving interstitials form clusters and furthermore gather to create loops with each other between layers. Meanwhile, surviving vacancies and interstitials form dislocation loops on the layers. The growth of these inserted layers cause the dimensional increase,more » i.e. swelling, of graphite. Interstitial and vacancy dislocation loops have been reported and they can easily been observed by electron microscope. However, observation of the intermediate atom clusters becomes is paramount in helping prove this model. We utilize fast protons generated from the University of Missouri Research Reactor (MURR) cyclotron to irradiate highly- oriented pyrolytic graphite (HOPG) as target for this research. Post-irradiation examination (PIE) of dosed targets with high-resolution transmission electron microscopy (HRTEM) has permit observation and analysis of clusters and dislocation loops to support the proposed theory. Another part of the research is to validate M.I. Heggie’s Ruck and Tuck model, which introduced graphite layers may fold under fast particle irradiation. Again, we employed microscopy to image irradiated specimens to determine how the extent of Ruck and Tuck by calculating the number of folds as a function of dose. Our most significant accomplishment is the invention of a novel class of high-intensity pure beta-emitters for long-term lightweight batteries. We have filed four invention disclosure records based on the research conducted in this project. These batteries are lightweight because they consist of carbon and tritium and can be fabricated to conform to many geometric shapes. In addition, we have published eight peer-reviewed American Nuclear Society (ANS) transactions, and presented our findings at ANS National Meetings, and several universities.« less

NANOWIRE CATHODE MATERIAL FOR LITHIUM-ION BATTERIES

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

John Olson, PhD

2004-07-21

This project involved the synthesis of nanowire ã-MnO2 and characterization as cathode material for high-power lithium-ion batteries for EV and HEV applications. The nanowire synthesis involved the edge site decoration nanowire synthesis developed by Dr. Reginald Penner at UC Irvine (a key collaborator in this project). Figure 1 is an SEM image showing ã-MnO2 nanowires electrodeposited on highly oriented pyrolytic graphite (HOPG) electrodes. This technique is unique to other nanowire template synthesis techniques in that it produces long (>500 um) nanowires which could reduce or eliminate the need for conductive additives due to intertwining of fibers. Nanowire cathode for lithium-ionmore » batteries with surface areas 100 times greater than conventional materials can enable higher power batteries for electric vehicles (EVs) and hybrid electric vehicles (HEVs). The synthesis of the ã-MnO2 nanowires was successfully achieved. However, it was not found possible to co-intercalate lithium directly in the nanowire synthesis. Based on input from proposal reviewers, the scope of the project was altered to attempt the conversion into spinel LiMn2O4 nanowire cathode material by solid state reaction of the ã-MnO2 nanowires with LiNO3 at elevated temperatures. Attempts to perform the conversion on the graphite template were unsuccessful due to degradation of the graphite apparently caused by oxidative attack by LiNO3. Emphasis then shifted to quantitative removal of the nanowires from the graphite, followed by the solid state reaction. Attempts to quantitatively remove the nanowires by several techniques were unsatisfactory due to co-removal of excess graphite or poor harvesting of nanowires. Intercalation of lithium into ã-MnO2 electrodeposited onto graphite was demonstrated, showing a partial demonstration of the ã-MnO2 material as a lithium-ion battery cathode material. Assuming the issues of nanowires removal can be solved, the technique does offer potential for creating high-power lithium-ion battery cathode needed for advanced EV and HEVs. Several technical advancements will still be required to meet this goal, and are likely topics for future SBIR feasibility studies.« less

Fullerenes, nanotubes, and graphite as matrices for collision mechanism in secondary ion mass spectrometry: determination of cyclodextrin.

PubMed

Stupavska, Monika; Jerigova, Monika; Michalka, Miroslav; Hasko, Daniel; Szoecs, Vojtech; Velic, Dusan

2011-12-01

A technique for improving the sensitivity of high mass molecular analysis is described. Three carbon species, fullerenes, single walled carbon nanotubes, and highly ordered pyrolytic graphite are introduced as matrices for the secondary ion mass spectrometry analysis of cyclodextrin (C(42)H(70)O(35), 1134 u). The fullerene and nanotubes are deposited as single deposition, and 10, 20, or 30 deposition films and cyclodextrin is deposited on top. The cyclodextrin parent-like ions and two fragments were analyzed. A 30 deposition fullerene film enhanced the intensity of cationized cyclodextrin with Na by a factor of 37. While the C(6)H(11)O(5) fragment, corresponding to one glucopyranose unit, increased by a factor of 16. Although fragmentation on fullerene is not suppressed, the intensity is twice as low as the parent-like ion. Deprotonated cyclodextrin increases by 100× and its C(8)H(7)O fragment by 10×. While the fullerene matrix enhances secondary ion emission, the nanotubes matrix film generates a basically constant yield. Graphite gives rise to lower intensity peaks than either fullerene or nanotubes. Scanning electron microscopy and atomic force microscopy provide images of the fullerene and nanotubes deposition films revealing flat and web structured surfaces, respectively. A "colliding ball" model is presented to provide a plausible physical mechanism of parent-like ion enhancement using the fullerene matrix. © American Society for Mass Spectrometry, 2011

Reexamination of Basal Plane Thermal Conductivity of Suspended Graphene Samples Measured by Electro-Thermal Micro-Bridge Methods

DOE PAGES

Jo, Insun; Pettes, Michael; Lindsay, Lucas R.; ...

2015-05-18

Thermal transport in suspended graphene samples has been measured in prior works and this work with the use of a suspended electro-thermal micro-bridge method. These measurement results are analyzed here to evaluate and eliminate the errors caused by the extrinsic thermal contact resistance. It is noted that the thermal resistance measured in a recent work increases linearly with the suspended length of the single-layer graphene samples synthesized by chemical vapor deposition (CVD), and that such a feature does not reveal the failure of Fourier s law despite the increase in the apparent thermal conductivity with length. The re-analyzed thermal conductivitymore » of a single-layer CVD graphene sample reaches about ( 1680 180 )Wm-1K-1 at room temperature, which is close to the highest value reported for highly oriented pyrolytic graphite. In comparison, the thermal conductivity values measured for two suspended exfoliated bi-layer graphene samples are about ( 880 60 ) and ( 730 60 ) Wm-1K-1 at room temperature, and approach that of the natural graphite source above room temperature. However, the low-temperature thermal conductivities of these suspended graphene samples are still considerably lower than the graphite values, with the peak thermal conductivities shifted to much higher temperatures. Analysis of the thermal conductivity data reveals that the low temperature behavior is dominated by phonon scattering by polymer residue instead of by the lateral boundary.« less

The low temperature oxidation of lithium thin films on HOPG by O 2 and H 2O

DOE PAGES

Wulfsberg, Steven M.; Koel, Bruce E.; Bernasek, Steven L.

2016-04-16

Lithiated graphite and lithium thin films have been used in fusion devices. In this environment, lithiated graphite will undergo oxidation by background gases. In order to gain insight into this oxidation process, thin (< 15 monolayer (ML)) lithium films on highly ordered pyrolytic graphite (HOPG) were exposed in this paper to O 2(g) and H 2O (g) in an ultra-high vacuum chamber. High resolution electron energy loss spectroscopy (HREELS) was used to identify the surface species formed during O 2(g) and H 2O (g) exposure. Auger electron spectroscopy (AES) was used to obtain the relative oxidation rates during O 2(g)more » and H 2O (g) exposure. AES showed that as the lithium film thickness decreased from 15 to 5 to 1 ML, the oxidation rate decreased for both O 2(g) and H 2O (g). HREELS showed that a 15 ML lithium film was fully oxidized after 9.7 L (L) of O 2(g) exposure and Li 2O was formed. HREELS also showed that during initial exposure (< 0.5 L) H 2O (g), lithium hydride and lithium hydroxide were formed on the surface of a 15 ML lithium film. Finally, after 0.5 L of H 2O (g) exposure, the H 2O (g) began to physisorb, and after 15 L of H 2O (g) exposure, the 15 ML lithium film was not fully oxidized.« less

The low temperature oxidation of lithium thin films on HOPG by O 2 and H 2O

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

Wulfsberg, Steven M.; Koel, Bruce E.; Bernasek, Steven L.

Lithiated graphite and lithium thin films have been used in fusion devices. In this environment, lithiated graphite will undergo oxidation by background gases. In order to gain insight into this oxidation process, thin (< 15 monolayer (ML)) lithium films on highly ordered pyrolytic graphite (HOPG) were exposed in this paper to O 2(g) and H 2O (g) in an ultra-high vacuum chamber. High resolution electron energy loss spectroscopy (HREELS) was used to identify the surface species formed during O 2(g) and H 2O (g) exposure. Auger electron spectroscopy (AES) was used to obtain the relative oxidation rates during O 2(g)more » and H 2O (g) exposure. AES showed that as the lithium film thickness decreased from 15 to 5 to 1 ML, the oxidation rate decreased for both O 2(g) and H 2O (g). HREELS showed that a 15 ML lithium film was fully oxidized after 9.7 L (L) of O 2(g) exposure and Li 2O was formed. HREELS also showed that during initial exposure (< 0.5 L) H 2O (g), lithium hydride and lithium hydroxide were formed on the surface of a 15 ML lithium film. Finally, after 0.5 L of H 2O (g) exposure, the H 2O (g) began to physisorb, and after 15 L of H 2O (g) exposure, the 15 ML lithium film was not fully oxidized.« less

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

Atomic force microscope characterization of self-assembly behaviors of cyclo[8] pyrrole on solid substrates

NASA Astrophysics Data System (ADS)

Xu, Hai; Zhao, Siqi; Xiong, Xiang; Jiang, Jinzhi; Xu, Wei; Zhu, Daoben; Zhang, Yi; Liang, Wenjie; Cai, Jianfeng

2017-04-01

Cyclo [8] pyrrole (CP) is a porphyrin analogue containing eight α-conjugated pyrrole units which are arranged in a nearly coplanar conformation. The π-π interactions between CP molecules lead to regular aggregations through a solution casting process. Using tapping mode atomic force microscope (AFM), we investigated the morphology of self-assembled aggregates formed by deposition of different CP solutions on different substrates. We found that in the n-butanol solution, nanofibrous structures could be formed on the silicon or mica surface. Interestingly, on the highly oriented pyrolytic graphite (HOPG) surface, or silicon and mica surface with a toluene solution, only irregular spherical structures were identified. The difference in the nanomorphology may be attributed to distinct interactions between molecule-molecule, molecule-solvent and molecule-substrate.

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

Wertsching, Alan Kevin; Trantor, Troy Joseph; Ebner, Matthias Anthony

A method and device for producing secure, high-density tritium bonded with carbon. A substrate comprising carbon is provided. A precursor is intercalated between carbon in the substrate. The precursor intercalated in the substrate is irradiated until at least a portion of the precursor, preferably a majority of the precursor, is transmutated into tritium and bonds with carbon of the substrate forming bonded tritium. The resulting bonded tritium, tritium bonded with carbon, produces electrons via beta decay. The substrate is preferably a substrate from the list of substrates consisting of highly-ordered pyrolytic graphite, carbon fibers, carbon nanotunes, buckministerfullerenes, and combinations thereof.more » The precursor is preferably boron-10, more preferably lithium-6. Preferably, thermal neutrons are used to irradiate the precursor. The resulting bonded tritium is preferably used to generate electricity either directly or indirectly.« less

Highly sensitive protein detection by biospecific AFM-based fishing with pulsed electrical stimulation.

PubMed

Pleshakova, Tatyana O; Malsagova, Kristina A; Kaysheva, Anna L; Kopylov, Arthur T; Tatur, Vadim Yu; Ziborov, Vadim S; Kanashenko, Sergey L; Galiullin, Rafael A; Ivanov, Yuri D

2017-08-01

We report here the highly sensitive detection of protein in solution at concentrations from 10 -15 to 10 -18 m using the combination of atomic force microscopy (AFM) and mass spectrometry. Biospecific detection of biotinylated bovine serum albumin was carried out by fishing out the protein onto the surface of AFM chips with immobilized avidin, which determined the specificity of the analysis. Electrical stimulation was applied to enhance the fishing efficiency. A high sensitivity of detection was achieved by application of nanosecond electric pulses to highly oriented pyrolytic graphite placed under the AFM chip. A peristaltic pump-based flow system, which is widely used in routine bioanalytical assays, was employed throughout the analysis. These results hold promise for the development of highly sensitive protein detection methods using nanosensor devices.

[AFM fishing of proteins under impulse electric field].

PubMed

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

2016-05-01

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

Femtosecond laser ablation of highly oriented pyrolytic graphite: a green route for large-scale production of porous graphene and graphene quantum dots

NASA Astrophysics Data System (ADS)

Russo, Paola; Hu, Anming; Compagnini, Giuseppe; Duley, Walter W.; Zhou, Norman Y.

2014-01-01

Porous graphene (PG) and graphene quantum dots (GQDs) are attracting attention due to their potential applications in photovoltaics, catalysis, and bio-related fields. We present a novel way for mass production of these promising materials. The femtosecond laser ablation of highly oriented pyrolytic graphite (HOPG) is employed for their synthesis. Porous graphene (PG) layers were found to float at the water-air interface, while graphene quantum dots (GQDs) were dispersed in the solution. The sheets consist of one to six stacked layers of spongy graphene, which form an irregular 3D porous structure that displays pores with an average size of 15-20 nm. Several characterization techniques have confirmed the porous nature of the collected layers. The analyses of the aqueous solution confirmed the presence of GQDs with dimensions of about 2-5 nm. It is found that the formation of both PG and GQDs depends on the fs-laser ablation energy. At laser fluences less than 12 J cm-2, no evidence of either PG or GQDs is detected. However, polyynes with six and eight carbon atoms per chain are found in the solution. For laser energies in the 20-30 J cm-2 range, these polyynes disappeared, while PG and GQDs were found at the water-air interface and in the solution, respectively. The origin of these materials can be explained based on the mechanisms for water breakdown and coal gasification. The absence of PG and GQDs, after the laser ablation of HOPG in liquid nitrogen, confirms the proposed mechanisms.Porous graphene (PG) and graphene quantum dots (GQDs) are attracting attention due to their potential applications in photovoltaics, catalysis, and bio-related fields. We present a novel way for mass production of these promising materials. The femtosecond laser ablation of highly oriented pyrolytic graphite (HOPG) is employed for their synthesis. Porous graphene (PG) layers were found to float at the water-air interface, while graphene quantum dots (GQDs) were dispersed in the solution. The sheets consist of one to six stacked layers of spongy graphene, which form an irregular 3D porous structure that displays pores with an average size of 15-20 nm. Several characterization techniques have confirmed the porous nature of the collected layers. The analyses of the aqueous solution confirmed the presence of GQDs with dimensions of about 2-5 nm. It is found that the formation of both PG and GQDs depends on the fs-laser ablation energy. At laser fluences less than 12 J cm-2, no evidence of either PG or GQDs is detected. However, polyynes with six and eight carbon atoms per chain are found in the solution. For laser energies in the 20-30 J cm-2 range, these polyynes disappeared, while PG and GQDs were found at the water-air interface and in the solution, respectively. The origin of these materials can be explained based on the mechanisms for water breakdown and coal gasification. The absence of PG and GQDs, after the laser ablation of HOPG in liquid nitrogen, confirms the proposed mechanisms. Electronic supplementary information (ESI) available. See DOI: 10.1039/c3nr05572h

Passive-quadrature demodulated localized-Michelson fiber-optic strain sensor embedded in composite materials

NASA Astrophysics Data System (ADS)

Valis, Tomas; Tapanes, Edward; Liu, Kexing; Measures, Raymond M.

1991-04-01

A strain sensor embedded in composite materials that is intrinsic, all fiber, local, and phase demodulated is described. It is the combination of these necessary elements that represents an advance in the state of the art. Sensor localization is achieved by using a pair of mirror-ended optical fibers of different lengths that are mechanically coupled up until the desired gauge length for common-mode suppression has been reached. This fiber-optic sensor has been embedded in both thermoset (Kevlar/epoxy and graphite/epoxy) and thermoplastic (graphite/PEEK) composite materials in order to make local strain measurements at the lamina level. The all-fiber system uses a 3 x 3 coupler for phase demodulation. Parameters such as strain sensitivity, transverse strain sensitivity, failure strain, and frequency response are discussed, along with applications.

Pseudo-Hall Effect in Graphite on Paper Based Four Terminal Devices for Stress Sensing Applications

NASA Astrophysics Data System (ADS)

Qamar, Afzaal; Sarwar, Tuba; Dinh, Toan; Foisal, A. R. M.; Phan, Hoang-Phuong; Viet Dao, Dzung

2017-04-01

A cost effective and easy to fabricate stress sensor based on pseudo-Hall effect in Graphite on Paper (GOP) has been presented in this article. The four terminal devices were developed by pencil drawing with hand on to the paper substrate. The stress was applied to the paper containing four terminal devices with the input current applied at two terminals and the offset voltage observed at other two terminals called pseudo-Hall effect. The GOP stress sensor showed significant response to the applied stress which was smooth and linear. These results showed that the pseudo-Hall effect in GOP based four terminal devices can be used for cost effective, flexible and easy to make stress, strain or force sensors.

X-ray photoelectron spectroscopic and morphologic studies of Ru nanoparticles deposited onto highly oriented pyrolytic graphite

NASA Astrophysics Data System (ADS)

Bavand, R.; Yelon, A.; Sacher, E.

2015-11-01

Ruthenium nanoparticles (Ru NPs) function as effective catalysts in specific reactions, such as methanation and Fischer-Tropsch syntheses. It is our purpose to physicochemically characterize their surfaces, at which catalysis occurs, by surface-sensitive X-ray photoelectron spectroscopy (XPS), using the symmetric peak component anaylsis technique developed in our laboratory to reveal previously hidden components. Ru NPs were deposited by evaporation (0.25-1.5 nm nominal deposition range) onto highly oriented pyrolytic graphite (HOPG). In addition to their surfaces being characterized by XPS, an indication of morphology was obtained from transmission electron microscopy (TEM). Our use of symmetric peak component XPS analysis has revealed detailed information on a previously unidentified surface oxide initially formed, as well as on the valence electronic structure and its variation with NP size, information that is of potential importance in the use of these NPs in catalysis. Each of the several Ru core XPS spectra characterized (3d, 3p and 3s) was found to be composed of three symmetric components. Together with two metal oxide O1s components, these give evidence of a rather complex, previously unidentified oxide that is initially formed. The Ru valence band (4d and 5s) spectra clearly demonstrate a loss of metallicity, a simultaneous increase of the Kubo gap, and an abrupt transfer in valence electron density from the 4d to the 5s orbitals (known as electron spill-over), as the NP size decreases below 0.5 nm. TEM photomicrographs, as a function of deposition rate, show that, at a rate that gives insufficient time for the NP condensation energy to dissipate, the initially well-separated NPs are capable of diffusing laterally and aggregating. This indicates weak NP bonding to the HOPG substrate. Carbide is formed, at both high and low deposition rates, at Ru deposition thicknesses greater than 0.25 nm, its formation explained by Ru NPs reacting with residual hydrocarbon vapor, under the influence of the heat of condensation released on Ru deposition, and not by Ru reacting with the HOPG substrate.

Drawing Sensors with Ball-Milled Blends of Metal-Organic Frameworks and Graphite

PubMed Central

Ko, Michael; Aykanat, Aylin; Smith, Merry K.

2017-01-01

The synthetically tunable properties and intrinsic porosity of conductive metal-organic frameworks (MOFs) make them promising materials for transducing selective interactions with gaseous analytes in an electrically addressable platform. Consequently, conductive MOFs are valuable functional materials with high potential utility in chemical detection. The implementation of these materials, however, is limited by the available methods for device incorporation due to their poor solubility and moderate electrical conductivity. This manuscript describes a straightforward method for the integration of moderately conductive MOFs into chemiresistive sensors by mechanical abrasion. To improve electrical contacts, blends of MOFs with graphite were generated using a solvent-free ball-milling procedure. While most bulk powders of pure conductive MOFs were difficult to integrate into devices directly via mechanical abrasion, the compressed solid-state MOF/graphite blends were easily abraded onto the surface of paper substrates equipped with gold electrodes to generate functional sensors. This method was used to prepare an array of chemiresistors, from four conductive MOFs, capable of detecting and differentiating NH3, H2S and NO at parts-per-million concentrations. PMID:28946624

Pyrolytic product characteristics of biosludge from the wastewater treatment plant of a petrochemical industry.

PubMed

Lin, Kuo-Hsiung; Hsu, Hui-Tsung; Ko, Ya-Wen; Shieh, Zhu-Xin; Chiang, Hung-Lung

2009-11-15

Biosludge was produced from the wastewater treatment plant of a petrochemical industry. The element compositions of pyrolytic residues, CO, CO(2), NOx, SOx, total hydrocarbons and detailed volatile organic compounds of pyrolytic gas, and C, H, N, S content and compositions in biofuel were determined in this study. Generally, 75-80% water content in sludge cakes and about 65-70% weight of water vapor and volatile compounds were volatilized during the drying process. Propene, propane, 1-butene, n-butane, isobutene, toluene and benzene were the major volatile organic compounds (VOCs) of the pyrolytic gas, and the concentrations for most of the top 20 VOC species were greater than 5 ppm. C(5)-C(9) compounds contributed 60% by weight of biofuel; 4-hydroxy-4-methyl-2-pentanone was the highest species, accounting for 28-53% of biofuel at various pyrolytic temperatures. Based on the dried residues, there was 8.5-13% weight in pyrolytic residues, 62-82% weight in liquid products (water and crude oil) and 5.8-30% weight in the gas phase after pyrolytic processing at 500-800 degrees C. Finally, 1.5-2.5 wt% liquid fuel was produced after the distillation process. The pyrolytic residues could be reused, the pyrolytic liquid product could be used as a fuel after distillation, and the pyrolytic gas could be recycled in the pyrolytic process to achieve non-toxic discharge and reduce the cost of sludge disposal.

Graphitic and oxidised high pressure high temperature (HPHT) nanodiamonds induce differential biological responses in breast cancer cell lines.

PubMed

Woodhams, Benjamin; Ansel-Bollepalli, Laura; Surmacki, Jakub; Knowles, Helena; Maggini, Laura; de Volder, Michael; Atatüre, Mete; Bohndiek, Sarah

2018-06-19

Nanodiamonds have demonstrated potential as powerful sensors in biomedicine, however, their translation into routine use requires a comprehensive understanding of their effect on the biological system being interrogated. Under normal fabrication processes, nanodiamonds are produced with a graphitic carbon shell, but are often oxidized in order to modify their surface chemistry for targeting to specific cellular compartments. Here, we assessed the biological impact of this purification process, considering cellular proliferation, uptake, and oxidative stress for graphitic and oxidized nanodiamond surfaces. We show for the first time that oxidized nanodiamonds possess improved biocompatibility compared to graphitic nanodiamonds in breast cancer cell lines, with graphitic nanodiamonds inducing higher levels of oxidative stress despite lower uptake.

Large Scale Reduction of Graphite Oxide Project

NASA Technical Reports Server (NTRS)

Calle, Carlos; Mackey, Paul; Falker, John; Zeitlin, Nancy

2015-01-01

This project seeks to develop an optical method to reduce graphite oxide into graphene efficiently and in larger formats than currently available. Current reduction methods are expensive, time-consuming or restricted to small, limited formats. Graphene has potential uses in ultracapacitors, energy storage, solar cells, flexible and light-weight circuits, touch screens, and chemical sensors. In addition, graphite oxide is a sustainable material that can be produced from any form of carbon, making this method environmentally friendly and adaptable for in-situ reduction.

Biomimetic graphene sensors: functionalizing graphene with peptides

NASA Astrophysics Data System (ADS)

Ishigami, Masa; Nyon Kim, Sang; Naik, Rajesh; Tatulian, Suren A.; Katoch, Jyoti

2012-02-01

Non-covalent biomimetic functionalization of graphene using peptides is one of more promising methods for producing novel sensors with high sensitivity and selectivity. Here we combine atomic force microscopy, Raman spectroscopy, and attenuated total reflection Fourier transform infrared spectroscopy to investigate peptide binding to graphene and graphite. We choose to study a dodecamer peptide identified with phage display to possess affinities for graphite and we find that the peptide forms a complex mesh-like structure upon adsorption on graphene. Moreover, optical spectroscopy reveals that the peptide binds non-covalently to graphene and possesses an optical signature of an ?-helical conformation on graphene.

Stripping voltammetry in environmental and food analysis.

PubMed

Brainina, K Z; Malakhova, N A; Stojko, N Y

2000-10-01

The review covers over 230 papers published mostly in the last 5 years. The goal of the review is to attract the attention of researchers and users to stripping voltammetry in particular, its application in environmental monitoring and analysis of foodstuffs. The sensors employed are impregnated graphite, carbon paste, thick film carbon/graphite and thin film metallic electrodes modified in-situ or beforehand. Hanging mercury drop electrodes and mercury coated glassy carbon electrodes are also mentioned. Strip and long-lived sensors for portable instruments and flow through systems are discussed as devices for future development and application of stripping voltammetry.

Development of Nitrogen Sensor for Determination of PN(2) in Body Tissues.

DTIC Science & Technology

1982-07-01

3) The progress of the reduction reaction (1) was followed by voltammetry. A single anodic potential sweep , starting from the open circuit...Graphite Electrode The progressive attachment of [Ru(NH3 ) 5 H2 0] +2 to PVP-coated graphite electrodes was observed by cyclic voltametry as an

FennoFlakes: a project for identifying flake graphite ores in the Fennoscandian shield and utilizing graphite in different applications

NASA Astrophysics Data System (ADS)

Palosaari, Jenny; Eklund, O.; Raunio, S.; Lindfors, T.; Latonen, R.-M.; Peltonen, J.; Smått, J.-H.; Kauppila, J.; Lund, S.; Sjöberg-Eerola, P.; Blomqvist, R.; Marmo, J.

2016-04-01

Natural graphite is a strategic mineral, since the European Commission stated (Report on critical raw materials for the EU (2014)) that graphite is one of the 20 most critical materials for the European Union. The EU consumed 13% of all flake graphite in the world but produced only 3%, which stresses the demand of the material. Flake graphite, which is a flaky version of graphite, forms under high metamorphic conditions. Flake graphite is important in different applications like batteries, carbon brushes, heat sinks etc. Graphene (a single layer of graphite) can be produced from graphite and is commonly used in many nanotechnological applications, e.g. in electronics and sensors. The steps to obtain pure graphene from graphite ore include fragmentation, flotation and exfoliation, which can be cumbersome and resulting in damaging the graphene layers. We have started a project named FennoFlakes, which is a co-operation between geologists and chemists to fill the whole value chain from graphite to graphene: 1. Exploration of graphite ores (geological and geophysical methods). 2. Petrological and geochemical analyses on the ores. 3. Development of fragmentation methods for graphite ores. 4. Chemical exfoliation of the enriched flake graphite to separate flake graphite into single and multilayer graphene. 5. Test the quality of the produced material in several high-end applications with totally environmental friendly and disposable material combinations. Preliminary results show that flake graphite in high metamorphic areas has better qualities compared to synthetic graphite produced in laboratories.

Role of iron modifier on boron atomization process using graphite furnace-atomic absorption spectrometry based on speciation of iron using X-ray absorption fine structure

NASA Astrophysics Data System (ADS)

Yamamoto, Yuhei; Tagami, Azusa; Shiarasaki, Toshihiro; Yonetani, Akira; Yamamoto, Takashi; Imai, Shoji

2018-04-01

The role of an Fe modifier on boron atomization process using graphite furnace-atomic absorbance spectrometry was investigated using a spectroscopic approach. The initial state of the Fe modifier in a pyrolytic graphite (PG) furnace was trivalent. With an increase in pyrolysis temperature, the Fe modifier was reduced in a stepwise manner. Fe2O3 and Fe3O4 were dominant at pyrolysis temperatures below 1300 K. From 1300 to 1500 K, FeO was dominant. At temperatures higher than 1700 K, Fe metal was dominant. After a drying step, 17.7% of the initial B remained in the PG furnace. After the pyrolysis step at 773 K, the residual fraction of B was similar to that after the drying step. After the pyrolysis step at a temperature of 1073 K, the residual fraction was 11.7%. At pyrolysis temperatures > 1738 K, the residual fraction was <3.3% (

Electrothermal atomic absorption spectrometric determination of arsenic in essential lavender and rose oils.

PubMed

Karadjova, Irina B; Lampugnani, Leonardo; Tsalev, Dimiter L

2005-02-28

Analytical procedures for electrothermal atomic absorption spectrometric (ETAAS) determination of arsenic in essential oils from lavender (Lavendula angustifolia) and rose (Rosa damascena) are described. For direct ETAAS analysis, oil samples are diluted with ethanol or i-propanol for lavender and rose oil, respectively. Leveling off responses of four different arsenic species (arsenite, arsenate, monomethylarsonate and dimethylarsinate) is achieved by using a composite chemical modifier: l-cysteine (0.05gl(-1)) in combination with palladium (2.5mug) and citric acid (100mug). Transverse-heated graphite atomizer (THGA) with longitudinal Zeeman-effect background correction and 'end-capped' graphite tubes with integrated pyrolytic graphite platforms, pre-treated with Zr-Ir for permanent modification are employed as most appropriate atomizer. Calibration with solvent-matched standard solutions of As(III) is used for four- and five-fold diluted samples of lavender and rose oil, respectively. Lower dilution factors required standard addition calibration by using aqueous (for lavender oil) or i-propanol (for rose oil) solutions of As(III). The limits of detection (LOD) for the whole analytical procedure are 4.4 and 4.7ngg(-1) As in levender and rose oil, respectively. The relative standard deviation (R.S.D.) for As at 6-30ngg(-1) levels is between 8 and 17% for both oils. As an alternative, procedure based on low temperature plasma ashing in oxygen with ETAAS, providing LODs of 2.5 and 2.7ngg(-1) As in levender and rose oil, respectively, and R.S.D. within 8-12% for both oils has been elaborated. Results obtained by both procedures are in good agreement.

The nucleation and growth of uranium on the basal plane of graphite studied by scanning tunneling microscopy

NASA Astrophysics Data System (ADS)

Tench, R. J.

1992-11-01

For the first time, nanometer scale uranium clusters were created on the basal plane of highly oriented pyrolytic graphite by laser ablation under ultra-high vacuum conditions. The physical and chemical properties of these clusters were investigated by scanning tunneling microscopy (STM) as well as standard surface science techniques. Auger electron and X-ray photoelectron spectroscopies found the uranium deposit to be free of contamination and showed that no carbide had formed with the underlying graphite. Clusters with sizes ranging from 42 to 630 sq A were observed upon initial room temperature deposition. Surface diffusion of uranium was observed after annealing the substrate above 800 K, as evidenced by the decreased number density and the increased size of the clusters. Preferential depletion of clusters on terraces near step edges as a result of annealing was observed. The activation energy for diffusion deduced from these measurements was found to be 15 Kcal/mole. Novel formation of ordered uranium thin films was observed for coverages greater than two monolayers after annealing above 900 K. These ordered films displayed islands with hexagonally faceted edges rising in uniform step heights characteristic of the unit cell of the P-phase of uranium. In addition, atomic resolution STM images of these ordered films indicated the formation of the (beta)-phase of uranium. The chemical properties of these surfaces were investigated and it was shown that these uranium films had a reduced oxidation rate in air as compared to bulk metal and that STM imaging in air induced a polarity-dependent enhancement of the oxidation rate.

Formation and composition of adsorbates on hydrophobic carbon surfaces from aqueous laccase-maltodextrin mixture suspension

NASA Astrophysics Data System (ADS)

Corrales Ureña, Yendry Regina; Lisboa-Filho, Paulo Noronha; Szardenings, Michael; Gätjen, Linda; Noeske, Paul-Ludwig Michael; Rischka, Klaus

2016-11-01

A robust procedure for the surface bio-functionalization of carbon surfaces was developed. It consists on the modification of carbon materials in contact with an aqueous suspension of the enzyme laccase from Trametes versicolor and the lyophilization agent maltodextrin, with the pH value adjusted close to the isoelectric point of the enzyme. We report in-situ investigations applying Quartz Crystal Microbalance with Dissipation (QCM-D) for carbon-coated sensor surfaces and, moreover, ex-situ measurements with static contact angle measurements, X-ray Photoelectron Spectroscopy (XPS) and Scanning Force Microscopy (SFM) for smooth Highly Oriented Pyrolytic Graphite (HOPG) substrates, for contact times between the enzyme formulation and the carbon material surface ranging from 20 s to 24 h. QCM-D studies reveals the formation of rigid layer of biomaterial, a few nanometers thin, which shows a strongly improved wettability of the substrate surface upon contact angle measurements. Following spectroscopic characterization, these layers are composed of mixtures of laccase and maltodextrin. The formation of these adsorbates is attributed to attractive interactions between laccase, the maltodextrin-based lyophilization agent and the hydrophobic carbon surfaces; a short-term contact between the aqueous laccase mixture suspension and HOPG surfaces is shown to merely result in de-wetting patterns influencing the results of contact angle measurements. The new enzyme-based surface modification of carbon-based materials is suggested to be applicable for the improvement of not only the wettability of low energy substrate surfaces with fluid formulations like coatings or adhesives, but also their adhesion in contact with hardened polymers.

Deposition of an Ultraflat Graphene Oxide Nanosheet on Atomically Flat Substrates

NASA Astrophysics Data System (ADS)

Khan, M. Z. H.; Shahed, S. M. F.; Yuta, N.; Komeda, T.

2017-07-01

In this study, graphene oxide (GO) sheets produced in the form of stable aqueous dispersions were deposited on Au (111), freshly cleaved mica, and highly oriented pyrolytic graphite (HOPG) substrates. Atomic force microscopy (AFM) and scanning electron microscopy (SEM) were used to study the presence and distinct contact of GO sheets on the substrates. It was revealed from the topography images that high-quality ultraflat GO monolayer sheets formed on the substrates without distinct cracking/wrinkling or folding. GO sheets with apparent height variation observed by microscopy also indicate ultraflat deposition with clear underlying steps. It was observed that ultrasonication and centrifuge steps prior to deposition were very effective for getting oxidation debris (OD)-free ultraflat single monolayer GO nanosheets onto substrates and that the process depends on the concentration of supplied GO solutions.

Investigations by Protein Film Electrochemistry of Alternative Reactions of Nickel-Containing Carbon Monoxide Dehydrogenase.

PubMed

Wang, Vincent C-C; Islam, Shams T A; Can, Mehmet; Ragsdale, Stephen W; Armstrong, Fraser A

2015-10-29

Protein film electrochemistry has been used to investigate reactions of highly active nickel-containing carbon monoxide dehydrogenases (CODHs). When attached to a pyrolytic graphite electrode, these enzymes behave as reversible electrocatalysts, displaying CO2 reduction or CO oxidation at minimal overpotential. The O2 sensitivity of CODH is suppressed by adding cyanide, a reversible inhibitor of CO oxidation, or by raising the electrode potential. Reduction of N2O, isoelectronic with CO2, is catalyzed by CODH, but the reaction is sluggish, despite a large overpotential, and results in inactivation. Production of H2 and formate under highly reducing conditions is consistent with calculations predicting that a nickel-hydrido species might be formed, but the very low rates suggest that such a species is not on the main catalytic pathway.

Calibration and characterization of a highly efficient spectrometer in von Hamos geometry for 7-10 keV x-rays

DOE PAGES

Jarrott, L. C.; Wei, M. S.; McGuffey, C.; ...

2017-04-27

Here, we have built an absolutely calibrated, highly efficient, Bragg crystal spectrometer in von Hamos geometry. This zinc von Hamos spectrometer uses a crystal made from highly oriented pyrolytic graphite that is cylindrically bent along the non-dispersive axis. It is tuned to measure x-ray spectra in the 7–10 keV range and has been designed to be used on a Ten Inch Manipulator for the Omega and OmegaEP target chambers at the Laboratory for Laser Energetics in Rochester, USA. Significant shielding strategies and fluorescence mitigation have been implemented in addition to an imaging plate detector making it well suited for experimentsmore » in high-intensity environments. Here we present the design and absolute calibration as well as mosaicity and integrated reflectivity measurements.« less

Imaging of subunit complexes of thermophilic bacterium H(+)-ATPase with scanning tunneling microscopy.

PubMed

Masai, J; Shibata, T; Kagawa, Y; Kondo, S

1992-07-01

Using a scanning tunneling microscope (STM), we observed reconstructed subunit complexes of H(+)-ATPase of a thermophilic bacterium. The measurement was carried out in air without conductive coating on the samples deposited on a highly oriented pyrolytic graphite (HOPG). The F1 subunit complex of the H(+)-ATPase, and an H(+)-ATPase whose F0 portion was embedded into liposomes prepared from soybean lecithin were imaged. Overall structural images of the subunit complex F1 were obtained: the structural dimensions of the STM images are in agreement with those deduced from conventional methods such as an transmission electron microscopy (TEM) and small-angle X-ray scattering (SAX) experimentation. Regarding the STM imaging of these samples, we discuss the advantages and disadvantages of the STM over those of conventional methods such as a TEM and SAX.

Characterization of submonolayer film composed of soft-landed copper nanoclusters on HOPG

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

Mondal, Shyamal, E-mail: shyamal.mondal@saha.ac.in; Das, Pabitra; Chowdhury, Debasree

Preformed Copper nanoclusters are deposited on highly oriented pyrolytic graphite (HOPG) at very low energy. For the study of chemical composition X-ray Photoelectron Spectroscopy (XPS) is performed for a wide range of binding energy without exposing the sample in the ambient. Morphological aspects of the supported clusters are characterized employing high resolution scanning electron microscope (SEM). Different types of morphology are observed depending on the nature of the substrate surface. Big fractal islands are formed on terraces while at the step edges small islands are found to form. Ex-situ cathodoluminescence (CL) measurement shows peak at 558 nm wavelength which corresponds tomore » the band gap of 2.22 eV which is due to Cu{sub 2}O nanocrystals formed due to oxidation of the deposited film in ambient.« less

High resolution x-ray Thomson scattering measurements from cryogenic hydrogen jets using the linac coherent light source

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

Fletcher, L. B., E-mail: lbfletch@slac.stanford.edu; Galtier, E.; Gamboa, E. J.

2016-11-15

We present the first spectrally resolved measurements of x-rays scattered from cryogenic hydrogen jets in the single photon counting limit. The 120 Hz capabilities of the LCLS, together with a novel hydrogen jet design [J. B. Kim et al., Rev. Sci. Instrum. (these proceedings)], allow for the ability to record a near background free spectrum. Such high-dynamic-range x-ray scattering measurements enable a platform to study ultra-fast, laser-driven, heating dynamics of hydrogen plasmas. This measurement has been achieved using two highly annealed pyrolytic graphite crystal spectrometers to spectrally resolve 5.5 keV x-rays elastically and inelastically scattered from cryogenic hydrogen and focusedmore » on Cornell-SLAC pixel array detectors [S. Herrmann et al., Nucl. Instrum. Methods Phys. Res., Sect. A 718, 550 (2013)].« less

Molecular and electronic structure of thin films of protoporphyrin(IX)Fe(III)Cl

NASA Astrophysics Data System (ADS)

Snyder, Shelly R.; White, Henry S.

1991-11-01

Electrochemical, scanning tunneling microscopy (STM), and tunneling spectroscopy studies of the molecular and electronic properties of thin films of protoporphyrin(IX)Fe(III)Cl (abbreviated as PP(IX)Fe(III)Cl) on highly oriented pyrolytic graphite (HOPG) electrodes are reported. PP(IX)Fe(III)Cl films are prepared by two different methods: (1) adsorption, yielding an electrochemically-active film, and (2) irreversible electrooxidative polymerization, yielding an electrochemically-inactive film. STM images, in conjunction with electro-chemical results, indicate that adsorption of PP(IX)Fe(III)Cl from aqueous solutions onto freshly cleaved HOPG results in a film comprised of molecular aggregates. In contrast, films prepared by irreversible electrooxidative polymerization of PP(IX)Fe(III)Cl have a denser, highly structured morphology, including what appear to be small pinholes (approx. 50A diameter) in an otherwise continuous film.

Self-assembled PCBM bilayers on graphene and HOPG examined by AFM and STM

NASA Astrophysics Data System (ADS)

Li, Yanlong; Chen, Chuanhui; Burton, John; Park, Kyungwha; Heflin, James R.; Tao, Chenggang

2018-05-01

In this work we report fabrication and characterization of phenyl-C61-butyric acid methyl ester (PCBM) bilayer structures on graphene and highly oriented pyrolytic graphite (HOPG). Through careful control of the PCBM solution concentration (from 0.1 to 2 mg ml-1) and the deposition conditions, we demonstrate that PCBM molecules self-assemble into bilayer structures on graphene and HOPG substrates. Interestingly, the PCBM bilayers are formed with two distinct heights on HOPG, but only one unique representative height on graphene. At elevated annealing temperatures, edge diffusion allows neighboring vacancies to merge into a more ordered structure. This is, to the best of our knowledge, the first experimental realization of PCBM bilayer structures on graphene. This work could provide valuable insight into fabrication of new hybrid, ordered structures for applications to organic solar cells.

A study to improve the mechanical properties of silicon carbide ribbon fibers

NASA Technical Reports Server (NTRS)

Debolt, H. E.; Robey, R. J.

1976-01-01

Preliminary deposition studies of SiC ribbon on a carbon ribbon substrate showed that the dominant strength limiting flaws were at the substrate surface. Procedures for making the carbon ribbon substrate from polyimide film were improved, providing lengths up to 450 meters (1,500 ft.) of flat carbon ribbon substrate 1,900 microns (75 mils) wide by 25 microns (1 mil) thick. The flaws on the carbon ribbon were smaller and less frequent than on carbon ribbon used earlier. SiC ribbon made using the improved substrate, including a layer of pyrolytic graphite to reduce further the severity of substrate surface flaws, showed strength levels up to the 2,068 MPa (300 Ksi) target of the program, with average strength levels over 1,700 MPa (250 Ksi) with coefficient of variation as low as 10% for some runs.

Formation of Amorphous Carbon Nanoparticles by the Laser Electrodispersion Method

NASA Astrophysics Data System (ADS)

Gurevich, S. A.; Gorokhov, M. V.; Kozhevin, V. M.; Kukushkin, M. V.; Levitskii, V. S.; Markov, L. K.; Yavsin, D. A.

2018-03-01

Experimental results on the laser ablation of the highly oriented pyrolytic graphite by using light pulses of an Nd:YAG laser (pulse width 25 ns, pulse energy 220 mJ) are presented. Analysis of the surface profile of the carbon target shows that the target material melts in the course of the laser ablation. As a result of ablation, a coating consisting of carbon nanoparticles about 10 nm in size is formed on the substrate placed at a distance of 4 cm from the target. It is assumed that such particles are formed as a result of the electrodispersion of carbon droplets detached from the target surface and charged to an unstable state in the laser plasma plume. Raman spectra of the coatings indicate that the carbon nanoparticles being formed have an amorphous structure.

Orientation-dependent energy level alignment and film growth of 2,7-diocty[1]benzothieno[3,2-b]benzothiophene (C8-BTBT) on HOPG

NASA Astrophysics Data System (ADS)

Lyu, Lu; Niu, Dongmei; Xie, Haipeng; Cao, Ningtong; Zhang, Hong; Zhang, Yuhe; Liu, Peng; Gao, Yongli

2016-01-01

Combining ultraviolet photoemission spectroscopy, X-ray photoemission spectroscopy, atomic force microscopy, and X-ray diffraction measurements, we performed a systematic investigation on the correlation of energy level alignment, film growth, and molecular orientation of 2,7-diocty[1]benzothieno[3,2-b]benzothiophene (C8-BTBT) on highly oriented pyrolytic graphite. The molecules lie down in the first layer and then stand up from the second layer. The ionization potential shows a sharp decrease from the lying down region to the standing up region. When C8-BTBT molecules start standing up, unconventional energy level band-bending-like shifts are observed as the film thickness increases. These shifts are ascribed to gradual decreasing of the molecular tilt angle about the substrate normal with the increasing film thickness.

Orientation-dependent energy level alignment and film growth of 2,7-diocty[1]benzothieno[3,2-b]benzothiophene (C8-BTBT) on HOPG.

PubMed

Lyu, Lu; Niu, Dongmei; Xie, Haipeng; Cao, Ningtong; Zhang, Hong; Zhang, Yuhe; Liu, Peng; Gao, Yongli

2016-01-21

Combining ultraviolet photoemission spectroscopy, X-ray photoemission spectroscopy, atomic force microscopy, and X-ray diffraction measurements, we performed a systematic investigation on the correlation of energy level alignment, film growth, and molecular orientation of 2,7-diocty[1]benzothieno[3,2-b]benzothiophene (C8-BTBT) on highly oriented pyrolytic graphite. The molecules lie down in the first layer and then stand up from the second layer. The ionization potential shows a sharp decrease from the lying down region to the standing up region. When C8-BTBT molecules start standing up, unconventional energy level band-bending-like shifts are observed as the film thickness increases. These shifts are ascribed to gradual decreasing of the molecular tilt angle about the substrate normal with the increasing film thickness.

Self-assembled PCBM bilayers on graphene and HOPG examined by AFM and STM.

PubMed

Li, Yanlong; Chen, Chuanhui; Burton, John; Park, Kyungwha; Heflin, James R; Tao, Chenggang

2018-05-04

In this work we report fabrication and characterization of phenyl-C61-butyric acid methyl ester (PCBM) bilayer structures on graphene and highly oriented pyrolytic graphite (HOPG). Through careful control of the PCBM solution concentration (from 0.1 to 2 mg ml -1 ) and the deposition conditions, we demonstrate that PCBM molecules self-assemble into bilayer structures on graphene and HOPG substrates. Interestingly, the PCBM bilayers are formed with two distinct heights on HOPG, but only one unique representative height on graphene. At elevated annealing temperatures, edge diffusion allows neighboring vacancies to merge into a more ordered structure. This is, to the best of our knowledge, the first experimental realization of PCBM bilayer structures on graphene. This work could provide valuable insight into fabrication of new hybrid, ordered structures for applications to organic solar cells.

Improving a high-efficiency, gated spectrometer for x-ray Thomson scattering experiments at the National Ignition Facility.

PubMed

Döppner, T; Kraus, D; Neumayer, P; Bachmann, B; Emig, J; Falcone, R W; Fletcher, L B; Hardy, M; Kalantar, D H; Kritcher, A L; Landen, O L; Ma, T; Saunders, A M; Wood, R D

2016-11-01

We are developing x-ray Thomson scattering for applications in implosion experiments at the National Ignition Facility. In particular we have designed and fielded MACS, a high-efficiency, gated x-ray spectrometer at 7.5-10 keV [T. Döppner et al., Rev. Sci. Instrum. 85, 11D617 (2014)]. Here we report on two new Bragg crystals based on Highly Oriented Pyrolytic Graphite (HOPG), a flat crystal and a dual-section cylindrically curved crystal. We have performed in situ calibration measurements using a brass foil target, and we used the flat HOPG crystal to measure Mo K-shell emission at 18 keV in 2nd order diffraction. Such high photon energy line emission will be required to penetrate and probe ultra-high-density plasmas or plasmas of mid-Z elements.

Nanospectroscopy of thiacyanine dye molecules adsorbed on silver nanoparticle clusters

NASA Astrophysics Data System (ADS)

Ralević, Uroš; Isić, Goran; Anicijević, Dragana Vasić; Laban, Bojana; Bogdanović, Una; Lazović, Vladimir M.; Vodnik, Vesna; Gajić, Radoš

2018-03-01

The adsorption of thiacyanine dye molecules on citrate-stabilized silver nanoparticle clusters drop-cast onto freshly cleaved mica or highly oriented pyrolytic graphite surfaces is examined using colocalized surface-enhanced Raman spectroscopy and atomic force microscopy. The incidence of dye Raman signatures in photoluminescence hotspots identified around nanoparticle clusters is considered for both citrate- and borate-capped silver nanoparticles and found to be substantially lower in the former case, suggesting that the citrate anions impede the efficient dye adsorption. Rigorous numerical simulations of light scattering on random nanoparticle clusters are used for estimating the electromagnetic enhancement and elucidating the hotspot formation mechanism. The majority of the enhanced Raman signal, estimated to be more than 90%, is found to originate from the nanogaps between adjacent nanoparticles in the cluster, regardless of the cluster size and geometry.

Main principles of passive devices based on graphene and carbon films in microwave-THz frequency range

NASA Astrophysics Data System (ADS)

Kuzhir, Polina P.; Paddubskaya, Alesia G.; Volynets, Nadezhda I.; Batrakov, Konstantin G.; Kaplas, Tommi; Lamberti, Patrizia; Kotsilkova, Rumiana; Lambin, Philippe

2017-07-01

The ability of thin conductive films, including graphene, pyrolytic carbon (PyC), graphitic PyC (GrPyC), graphene with graphitic islands (GrI), glassy carbon (GC), and sandwich structures made of all these materials separated by polymer slabs to absorb electromagnetic radiation in microwave-THz frequency range, is discussed. The main physical principles making a basis for high absorption ability of these heterostructures are explained both in the language of electromagnetic theory and using representation of equivalent electrical circuits. The idea of using carbonaceous thin films as the main working elements of passive radiofrequency (RF) devices, such as shields, filters, polarizers, collimators, is proposed theoretically and proved experimentally. The important advantage of PyC, GrI, GrPyC, and GC is that, in contrast to graphene, they either can be easily deposited onto a dielectric substrate or are strong enough to allow their transfer from the catalytic substrate without a shuttle polymer layer. This opens a new avenue toward the development of a scalable protocol for cost-efficient production of ultralight electromagnetic shields that can be transferred to commercial applications. A robust design via finite-element method and design of experiment for RF devices based on carbon/graphene films and sandwiches is also discussed in the context of virtual prototyping.

Suspended-Bed Reactor preliminary design, /sup 233/U--/sup 232/Th cycle. Final report (revised)

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

Karam, R.A.; Alapour, A.; Lee, C.C.

1977-11-01

The preliminary design Suspended-Bed Reactor is described. Coated particles about 2 mm in diameter are used as the fuel. The coatings consist of three layers: (1) low density pyrolytic graphite, 70 ..mu.. thick, (2) silicon carbide pressure vessel, 30 ..mu.. thick, and (3) ZrC layer, 50 ..mu.. thick, to protect the pressure vessel from moisture and oxygen. The fuel kernel can be either uranium-thorium dicarbide or metal. The coated particles are suspended by helium gas (coolant) in a cluster of pressurized tubes. The upward flow of helium fluidizes the coated particles. As the flow rate increases, the bed of particlesmore » is lifted upward to the core section. The particles are restrained at the upper end of the core by a suitable screen. The overall particle density in the core is just enough for criticality condition. Should the helium flow cease, the bed in the core section will collapse, and the particles will flow downward into the section where the increased physical spacings among the tubes brings about a safe shutdown. By immersing this section of the tubes in a large graphite block to serve as a heat sink, dissipation of decay heat becomes manageable. This eliminates the need for emergency core cooling systems.« less

Trace element content and magnetic properties of commercial HOPG samples studied by ion beam microscopy and SQUID magnetometry

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

Spemann, D., E-mail: spemann@uni-leipzig.de; Esquinazi, P., E-mail: esquin@physik.uni-leipzig.de; Setzer, A.

In this study, the impurity concentration and magnetic response of nine highly oriented pyrolytic graphite (HOPG) samples with different grades and from different providers were determined using ion beam microscopy and SQUID magnetometry. Apart from sideface contaminations in the as-received state, bulk contamination of the samples in most cases consists of disk-shaped micron-sized particles made of Ti and V with an additional Fe contamination around the grain perimeter. The saturation magnetization typically increases with Fe concentration, however, there is no simple correlation between Fe content and magnetic moment. The saturation magnetization of one, respectively six, out of nine samples clearlymore » exceeds the maximum contribution from pure Fe or Fe{sub 3}C. For most samples the temperature dependence of the remanence decreases linearly with T – a dependence found previously for defect-induced magnetism (DIM) in HOPG. We conclude that apart from magnetic impurities, additional contribution to the ferromagnetic magnetization exists in pristine HOPG in agreement with previous studies. A comparative study between the results of ion beam microscopy and the commonly used EDX analysis shows clearly that EDX is not a reliable method for quantitative trace elemental analysis in graphite, clarifying weaknesses and discrepancies in the element concentrations given in the recent literature.« less

Reactive Capture of Gold Nanoparticles by Strongly Physisorbed Monolayers on Graphite

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

Wei, Xiaoliang; Tong, Wenjun; Fidler, Vlastimil

2012-12-01

Anthracene Diels Alder adducts (DAa) bearing two long side chains (H-(CH2)22O(CH2)6OCH2-) at the 1- and 5-positions form self-assembled monolayers (SAMs) at the phenyloctane - highly oriented pyrolytic graphite (HOPG) interface. The long DAa side chains promote strong physisorption of the monolayer to HOPG and maintain the monolayer morphology upon rinsing or incubation in ethanol and air-drying of the substrate. Incorporating a carboxylic acid group on the DAa core enables capture of 1 - 4 nm diameter gold nanoparticles (AuNP) provided (i) the monolayer containing DAa-carboxylic acids is treated with Cu2+ ions and (ii) the organic coating on the AuNP containsmore » carboxylic acids (11-mercaptoundecanoic acid, MUA-AuNP). AuNP capture by the monolayer proceeds with formation of Cu2+ - carboxylate coordination complexes. The captured AuNP appear as mono- and multi-layered clusters at high coverage on HOPG. The surface density of the captured AuNPs can be adjusted from AuNP multi-layers to isolated AuNPs by varying incubation times, MUA-AuNP concentration, the number density of carboxylic acids in the monolayer, the number of MUA per AuNP, and the post-incubation treatments.« less

Magnetically Orchestrated Formation of Diamond at Lower Temperatures and Pressures

NASA Astrophysics Data System (ADS)

Little, Reginald B.; Lochner, Eric; Goddard, Robert

2005-01-01

Man's curiosity and fascination with diamonds date back to ancient times. The knowledge of the many properties of diamond is recorded during Biblical times. Antoine Lavoisier determined the composition of diamond by burning in O2 to form CO2. With the then existing awareness of graphite as carbon, the race began to convert graphite to diamond. The selective chemical synthesis of diamond has been pursued by Cagniard, Hannay, Moisson and Parson. On the basis of the thermodynamically predicted equilibrium line of diamond and graphite, P W Bridgman attempted extraordinary conditions of high temperature (>2200°C) and pressure (>100,000 atm) for the allotropic conversion of graphite to diamond. H T Hall was the first to successfully form bulk diamond by realizing the kinetic restrictions to Bridgman's (thermodynamic) high pressure high temperature direct allotropic conversion. Moreover, Hall identified catalysts for the faster kinetics of diamond formation. H M Strong determined the import of the liquid catalyst during Hall's catalytic synthesis. W G Eversole discovered the slow metastable low pressure diamond formation by pyrolytic chemical vapor deposition with the molecular hydrogen etching of the rapidly forming stable graphitic carbon. J C Angus determined the import of atomic hydrogen for faster etching for faster diamond growth at low pressure. S Matsumoto has developed plasma and hot filament technology for faster hydrogen and carbon radical generations at low pressure for faster diamond formation. However the metastable low pressure chemical vapor depositions by plasma and hot filament are prone to polycrystalline films. From Bridgman to Hall to Eversole, Angus and Matsumoto, much knowledge has developed of the importance of pressure, temperature, transition metal catalyst, liquid state of metal (metal radicals atoms) and the carbon radical intermediates for diamond synthesis. Here we advance this understanding of diamond formation by demonstrating the external magnetic organization of carbon, metal and hydrogen radicals for lower temperature and pressure synthesis. Here we show that strong static external magnetic field (>15 T) enhances the formation of single crystal diamond at lower pressure and even atmospheric pressure with implications for much better, faster high quality diamond formation by magnetization of current high pressure and temperature technology.

Analyzing the impact of reactive transport on the repository performance of TRISO fuel

NASA Astrophysics Data System (ADS)

Schmidt, Gregory

One of the largest determiners of the amount of electricity generated by current nuclear reactors is the efficiency of the thermodynamic cycle used for power generation. Current light water reactors (LWR) have an efficiency of 35% or less for the conversion of heat energy generated by the reactor to electrical energy. If this efficiency could be improved, more power could be generated from equivalent volumes of nuclear fuel. One method of improving this efficiency is to use a coolant flow that operates at a much higher temperature for electricity production. A reactor design that is currently proposed to take advantage of this efficiency is a graphite-moderated, helium-cooled reactor known as a High Temperature Gas Reactor (HTGR). There are significant differences between current LWR's and the proposed HTGR's but most especially in the composition of the nuclear fuel. For LWR's, the fuel elements consist of pellets of uranium dioxide or plutonium dioxide that are placed in long tubes made of zirconium metal alloys. For HTGR's, the fuel, known as TRISO (TRIstructural-ISOtropic) fuel, consists of an inner sphere of fissile material, a layer of dense pyrolytic carbon (PyC), a ceramic layer of silicon carbide (SiC) and a final dense outer layer of PyC. These TRISO particles are then compacted with graphite into fuel rods that are then placed in channels in graphite blocks. The blocks are then arranged in an annular fashion to form a reactor core. However, this new fuel form has unanswered questions on the environmental post-burn-up behavior. The key question for current once-through fuel operations is how these large irradiated graphite blocks with spent fuel inside will behave in a repository environment. Data in the literature to answer this question is lacking, but nevertheless this is an important question that must be answered before wide-spread adoption of HTGR's could be considered. This research has focused on answering the question of how the large quantity of graphite surrounding the spent HTGR fuel will impact the release of aqueous uranium from the TRISO fuel. In order to answer this question, the sorption and partitioning behavior of uranium to graphite under a variety of conditions was investigated. Key systematic variables that were analyzed include solution pH, dissolved carbonate concentration, uranium metal concentration and ionic strength. The kinetics and desorption characteristics of uranium/graphite partitioning were studied as well. The graphite used in these experiments was also characterized by a variety of techniques and conclusions are drawn about the relevant surface chemistry of graphite. This data was then used to generate a model for the reactive transport of uranium in a graphite matrix. This model was implemented with the software code CXTFIT and validated through the use of column studies mirroring the predicted system.

Friction and transfer behavior of pyrolytic boron nitride in contact with various metals

NASA Technical Reports Server (NTRS)

Buckley, D. H.

1976-01-01

Sliding friction experiments were conducted with pyrolytic boron nitride in sliding contact with itself and various metals. Auger emission spectroscopy was used to monitor transfer of pyrolytic boron nitride to metals and metals to pyrolytic boron nitride. Results indicate that the friction coefficient for pyrolytic boron nitride in contact with metals can be related to the chemical activity of the metals and more particularly to the d valence bond character of the metal. Transfer was found to occur to all metals except silver and gold and the amount of transfer was less in the presence than in the absence of metal oxide. Friction was less for pyrolytic boron nitride in contact with a metal in air than in vacuum.

Influence of carbonization conditions on the pyrolytic carbon deposition in acacia and eucalyptus wood chars

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

Kumar, M.; Gupta, R.C.

1997-04-01

The amount of deposited pyrolytic carbon (resulting from the cracking of volatile matter) was found to depend on wood species and carbonization conditions, such as temperature and heating rate. Maximum pyrolytic carbon deposition in both the acacia and eucalyptus wood chars has been observed at a carbonization temperature of 800 C. Rapid carbonization (higher heating rate) of wood significantly reduces the amount of deposited pyrolytic carbon in resulting chars. Results also indicate that the amount of deposited pyrolytic carbon in acacia wood char is less than that in eucalyptus wood char.

Sensitive Adsorptive Voltammetric Method for Determination of Bisphenol A by Gold Nanoparticle/Polyvinylpyrrolidone-Modified Pencil Graphite Electrode

PubMed Central

Yaman, Yesim Tugce; Abaci, Serdar

2016-01-01

A novel electrochemical sensor gold nanoparticle (AuNP)/polyvinylpyrrolidone (PVP) modified pencil graphite electrode (PGE) was developed for the ultrasensitive determination of Bisphenol A (BPA). The gold nanoparticles were electrodeposited by constant potential electrolysis and PVP was attached by passive adsorption onto the electrode surface. The electrode surfaces were characterized by electrochemical impedance spectroscopy (EIS) and scanning electron microscopy (SEM). The parameters that affected the experimental conditions were researched and optimized. The AuNP/PVP/PGE sensor provided high sensitivity and selectivity for BPA recognition by using square wave adsorptive stripping voltammetry (SWAdSV). Under optimized conditions, the detection limit was found to be 1.0 nM. This new sensor system offered the advantages of simple fabrication which aided the expeditious replication, low cost, fast response, high sensitivity and low background current for BPA. This new sensor system was successfully tested for the detection of the amount of BPA in bottled drinking water with high reliability. PMID:27231912

Carbon treated commercial aluminium alloys as anodes for aluminium-air batteries in sodium chloride electrolyte

NASA Astrophysics Data System (ADS)

Pino, M.; Herranz, D.; Chacón, J.; Fatás, E.; Ocón, P.

2016-09-01

An easy treatment based in carbon layer deposition into aluminium alloys is presented to enhance the performance of Al-air primary batteries with neutral pH electrolyte. The jellification of aluminate in the anode surface is described and avoided by the carbon covering. Treated commercial Al alloys namely Al1085 and Al7475 are tested as anodes achieving specific capacities above 1.2 Ah g-1vs 0.5 Ah g-1 without carbon covering. The influence of the binder proportion in the treatment as well as different carbonaceous materials, Carbon Black, Graphene and Pyrolytic Graphite are evaluated as candidates for the covering. Current densities of 1-10 mA cm-2 are measured and the influence of the alloy explored. A final battery design of 4 cells in series is presented for discharges with a voltage plateau of 2 V and 1 Wh g-1 energy density.

Low-noise humidity controller for imaging water mediated processes in atomic force microscopy

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

Gaponenko, I., E-mail: iaroslav.gaponenko@unige.ch; Gamperle, L.; Herberg, K.

2016-06-15

We demonstrate the construction of a novel low-noise continuous flow humidity controller and its integration with a commercial variable-temperature atomic force microscope fluid cell, allowing precise control of humidity and temperature at the sample during nanoscale measurements. Based on wet and dry gas mixing, the design allows a high mechanical stability to be achieved by means of an ultrasonic atomiser for the generation of water-saturated gas, improving upon previous bubbler-based architectures. Water content in the flow is measured both at the inflow and outflow of the fluid cell, enabling the monitoring of water condensation and icing, and allowing controlled variationmore » of the sample temperature independently of the humidity. To benchmark the performance of the controller, the results of detailed noise studies and time-based imaging of the formation of ice layers on highly oriented pyrolytic graphite are shown.« less

High resolution x-ray Thomson scattering measurements from cryogenic hydrogen jets using the linac coherent light source

DOE PAGES

Fletcher, L. B.; Zastrau, U.; Galtier, E.; ...

2016-08-15

Here, we present the first spectrally resolved measurements of x-rays scattered from cryogenic hydrogen jets in the single photon counting limit. The 120 Hz capabilities of the LCLS, together with a novel hydrogen jet design [J. B. Kim et al., Rev. Sci. Instrum. (these proceedings)], allow for the ability to record a near background free spectrum. Such high-dynamic-range x-ray scattering measurements enable a platform to study ultra-fast, laser-driven, heating dynamics of hydrogen plasmas. This measurement has been achieved using two highly annealed pyrolytic graphite crystal spectrometers to spectrally resolve 5.5 keV x-rays elastically and inelastically scattered from cryogenic hydrogen andmore » focused on Cornell-SLAC pixel array detectors [S. Herrmann et al., Nucl. Instrum. Methods Phys. Res., Sect. A 718, 550 (2013)].« less

Comparison of Hyperthermal Ground Laboratory Atomic Oxygen Erosion Yields With Those in Low Earth Orbit

NASA Technical Reports Server (NTRS)

Banks, Bruce A.; Dill, Grace C.; Loftus, Ryan J.; deGroh, Kim K.; Miller, Sharon K.

2013-01-01

The atomic oxygen erosion yields of 26 materials (all polymers except for pyrolytic graphite) were measured in two directed hyperthermal radio frequency (RF) plasma ashers operating at 30 or 35 kHz with air. The hyperthermal asher results were compared with thermal energy asher results and low Earth orbital (LEO) results from the Materials International Space Station Experiment 2 and 7 (MISSE 2 and 7) flight experiments. The hyperthermal testing was conducted to a significant portion of the atomic oxygen fluence similar polymers were exposed to during the MISSE 2 and 7 missions. Comparison of the hyperthermal asher prediction of LEO erosion yields with thermal energy asher erosion yields indicates that except for the fluorocarbon polymers of PTFE and FEP, the hyperthermal energy ashers are a much more reliable predictor of LEO erosion yield than thermal energy asher testing, by a factor of four.

Improving a high-efficiency, gated spectrometer for x-ray Thomson scattering experiments at the National Ignition Facility

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

Döppner, T., E-mail: doeppner1@llnl.gov; Bachmann, B.; Emig, J.

We are developing x-ray Thomson scattering for applications in implosion experiments at the National Ignition Facility. In particular we have designed and fielded MACS, a high-efficiency, gated x-ray spectrometer at 7.5–10 keV [T. Döppner et al., Rev. Sci. Instrum. 85, 11D617 (2014)]. Here we report on two new Bragg crystals based on Highly Oriented Pyrolytic Graphite (HOPG), a flat crystal and a dual-section cylindrically curved crystal. We have performed in situ calibration measurements using a brass foil target, and we used the flat HOPG crystal to measure Mo K-shell emission at 18 keV in 2nd order diffraction. Such high photonmore » energy line emission will be required to penetrate and probe ultra-high-density plasmas or plasmas of mid-Z elements.« less

Orientation-dependent energy level alignment and film growth of 2,7-diocty[1]benzothieno[3,2-b]benzothiophene (C8-BTBT) on HOPG

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

Lyu, Lu; Niu, Dongmei, E-mail: mayee@csu.edu.cnmailto; Xie, Haipeng

Combining ultraviolet photoemission spectroscopy, X-ray photoemission spectroscopy, atomic force microscopy, and X-ray diffraction measurements, we performed a systematic investigation on the correlation of energy level alignment, film growth, and molecular orientation of 2,7-diocty[1]benzothieno[3,2-b]benzothiophene (C8-BTBT) on highly oriented pyrolytic graphite. The molecules lie down in the first layer and then stand up from the second layer. The ionization potential shows a sharp decrease from the lying down region to the standing up region. When C8-BTBT molecules start standing up, unconventional energy level band-bending-like shifts are observed as the film thickness increases. These shifts are ascribed to gradual decreasing of the molecularmore » tilt angle about the substrate normal with the increasing film thickness.« less

Moiré-Modulated Conductance of Hexagonal Boron Nitride Tunnel Barriers.

PubMed

Summerfield, Alex; Kozikov, Aleksey; Cheng, Tin S; Davies, Andrew; Cho, Yong-Jin; Khlobystov, Andrei N; Mellor, Christopher J; Foxon, C Thomas; Watanabe, Kenji; Taniguchi, Takashi; Eaves, Laurence; Novoselov, Kostya S; Novikov, Sergei V; Beton, Peter H

2018-06-27

Monolayer hexagonal boron nitride (hBN) tunnel barriers investigated using conductive atomic force microscopy reveal moiré patterns in the spatial maps of their tunnel conductance consistent with the formation of a moiré superlattice between the hBN and an underlying highly ordered pyrolytic graphite (HOPG) substrate. This variation is attributed to a periodc modulation of the local density of states and occurs for both exfoliated hBN barriers and epitaxially grown layers. The epitaxial barriers also exhibit enhanced conductance at localized subnanometer regions which are attributed to exposure of the substrate to a nitrogen plasma source during the high temperature growth process. Our results show clearly a spatial periodicity of tunnel current due to the formation of a moiré superlattice and we argue that this can provide a mechanism for elastic scattering of charge carriers for similar interfaces embedded in graphene/hBN resonant tunnel diodes.

Intrinsic stress modulation in diamond like carbon films with incorporation of gold nanoparticles by PLA

NASA Astrophysics Data System (ADS)

Panda, Madhusmita; Krishnan, R.; Krishna, Nanda Gopala; Madapu, Kishore K.; Kamruddin, M.

2018-04-01

Intrinsic stress modulation in the diamond-like carbon (DLC) coatings with incorporation of gold nanoparticles was studied qualitatively from Raman shift. The films were deposited on Si (1 0 0) substrates by using Pulsed laser ablation (PLA) of pure pyrolytic graphite target and with a gold foil on it. Films compositional and chemical behavior was studied by X-ray photoelectron spectroscopy (XPS) and Visible Raman spectroscopy, respectively. The sp3 content obtained from XPS shows dramatic variation in DLC, DLC-Au(100), DLC-Au(200) and DLC-Au(300) as 39%, 41%, 47% and 66% with various gold contentsas 0%, 12%, 7.3% and 4.7%, respectively. The Raman spectra of DLC/Au films showed G-peak shift towards lower wavenumber indicating the reduction of intrinsic stress (internal compressive stress). The sp2, sp3 fraction in the films are also determined from FWHM (G-Peak).

Method of making carbon-carbon composites

DOEpatents

Engle, Glen B.

1993-01-01

A process for making 2D and 3D carbon-carbon composites having a combined high crystallinity, high strength, high modulus and high thermal and electrical conductivity. High-modulus/high-strength mesophase derived carbon fibers are woven into a suitable cloth. Layers of this easily graphitizible woven cloth are infiltrated with carbon material to form green composites. The carbonized composite is then impregnated several times with pitch by covering the composite with hot pitch under pressure. The composites are given a heat treatment between each impregnant step to crack up the infiltrated carbon and allow additional pitch to enter the microstructure during the next impregnation cycle. The impregnated composites are then given a final heat treatment in the range 2500.degree. to 3100.degree. C. to fully graphitize the fibers and the matrix carbon. The composites are then infiltrated with pyrolytic carbon by chemical vapor deposition in the range 1000.degree. C. to 1300.degree. C. at a reduced. pressure.

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

NASA Astrophysics Data System (ADS)

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

2014-02-01

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

Improving a high-efficiency, gated spectrometer for x-ray Thomson scattering experiments at the National Ignition Facility

DOE PAGES

Döppner, T.; Kraus, D.; Neumayer, P.; ...

2016-08-03

We are developing x-ray Thomson scattering for applications in implosion experiments at the National Ignition Facility. In particular we have designed and fielded MACS, a high-efficiency, gated x-ray spectrometer at 7.5-10 keV [T. Döppner et al., Rev. Sci. Instrum. 85, 11D617 (2014)]. Here in this paper we report on two new Bragg crystals based on Highly Oriented Pyrolytic Graphite (HOPG), a flat crystal and a dual-section cylindrically curved crystal. We have performed in situ calibration measurements using a brass foil target, and we used the flat HOPG crystal to measure Mo K-shell emission at 18 keV in 2nd order diffraction.more » Such high photon energy line emission will be required to penetrate and probe ultra-high-density plasmas or plasmas of mid-Z elements.« less

Optically transparent cathode for Co(III/II) mediated dye-sensitized solar cells based on graphene oxide.

PubMed

Kavan, Ladislav; Yum, Jun-Ho; Graetzel, Michael

2012-12-01

Thin semitransparent films were fabricated on F-doped SnO(2) (FTO) from single-layer graphene oxide (GO) either pure or in a composite with graphene nanoplatelets. Electrocatalytic activity of prepared films was tested for the Co(bpy)(3)(3+/2+) redox couple in acetonitrile electrolyte solution. Pristine GO showed almost no activity, resembling the properties of basal plane pyrolytic graphite. However, electrochemical performance of graphene oxide improved dramatically upon chemical reduction with hydrazine and/or heat treatment. All GO-containing films were firmly bonded to FTO, which contrasted with the poor adhesion of sole graphene nanoplatelets to this support. The activity loss during long-term aging was considerably improved, too. Enhanced stability of GO-containing films together with high electrocatalytic activity is beneficial for application in a new generation of dye-sensitized solar cells employing Co(bpy)(3)(3+/2+) as the redox shuttle.

Electrochemical studies on polysorbate-20 (Tween 20)-entrapped haemoglobin and its application in a hydrogen peroxide biosensor.

PubMed

Ma, Xiang; Chen, Ting; Liu, Lifang; Li, Genxi

2005-06-01

Haemoglobin (Hb) was entrapped in polysorbate 20 and then modified on a pyrolytic graphite electrode. Electrochemical studies revealed that a pair of stable and well-defined redox peaks attributed to the direct redox reaction of Hb could be observed in a phosphate buffer solution (pH 6.0). The anodic and cathodic peaks were located at -236 and -316 mV (versus a saturated calomel reference electrode) separately. The formal potential, E0', was linearly varied with pH in the range from 3.0 to 10.0 with a slope of -48.0 mV.pH-1. Moreover, the protein was capable of catalysing the reduction of H2O2. Accordingly, an unmediated biosensor for H2O2 was prepared with a linear range from 8.0x10(-7) to 1.0x10(-3) M. This biosensor exhibited good stability, sensitivity and reproducibility.

Preparation of iron oxide-impregnated spherical granular activated carbon-carbon composite and its photocatalytic removal of methylene blue in the presence of oxalic acid.

PubMed

Kadirova, Zukhra C; Hojamberdiev, Mirabbos; Katsumata, Ken-Ichi; Isobe, Toshihiro; Matsushita, Nobuhiro; Nakajima, Akira; Sharipov, Khasan; Okada, Kiyoshi

2014-01-01

The spherical granular activated carbon-carbon composites (GAC-Fe) with different iron oxide contents (Fe mass% = 0.6-10) were prepared by a pore volume impregnation method. The X-ray diffraction (XRD), scanning electron microscopy (SEM), and N2-adsorption results confirm the presence of amorphous iron oxide, pyrolytic carbon, and graphitized globular carbon nanoparticles covered with amorphous carbon in the CAG-Fe. The rate of photodegradation of methylene blue (MB) in aqueous solution under UV light in the presence of oxalic acid correlates with porosity of the prepared materials. The total MB removal includes the combination of adsorption and photodegradation without the addition of H2O2. The results of total organic carbon (TOC) analysis reveal that the decolorization of MB in aqueous solution containing oxalic acid corresponds to the decomposition of organic compounds to CO2 and H2O.

A low-temperature scanning tunneling microscope capable of microscopy and spectroscopy in a Bitter magnet at up to 34 T.

PubMed

Tao, W; Singh, S; Rossi, L; Gerritsen, J W; Hendriksen, B L M; Khajetoorians, A A; Christianen, P C M; Maan, J C; Zeitler, U; Bryant, B

2017-09-01

We present the design and performance of a cryogenic scanning tunneling microscope (STM) which operates inside a water-cooled Bitter magnet, which can attain a magnetic field of up to 38 T. Due to the high vibration environment generated by the magnet cooling water, a uniquely designed STM and a vibration damping system are required. The STM scan head is designed to be as compact and rigid as possible, to minimize the effect of vibrational noise as well as fit the size constraints of the Bitter magnet. The STM uses a differential screw mechanism for coarse tip-sample approach, and operates in helium exchange gas at cryogenic temperatures. The reliability and performance of the STM are demonstrated through topographic imaging and scanning tunneling spectroscopy on highly oriented pyrolytic graphite at T = 4.2 K and in magnetic fields up to 34 T.

Recent results concerning the stability of viscoelastic shear deformable plates under compressive edge loading

NASA Technical Reports Server (NTRS)

Librescu, L.; Chandiramani, N. K.

1989-01-01

Some recent results obtained by the authors are summarized concerning the stability of transversely isotropic flat panels whose materials exhibit a viscoelastic behavior and whose edges are subjected to in-plane biaxial compressive loads. Two transversely isotropic type materials, largely used in advanced technology, are considered: (1) the pyrolytic-graphite type, used in the thermal protection of aerospace vehicles, and (2) the type corresponding to unidirectional fiber-reinforced composites. In the former case, the planes of isotropy are parallel at each point to the midplane of the plate. In the latter case, they are normal to the fiber directions. The micromechanical relations developed by Aboudi (1984, 1986, 1987) are considered in conjunction with the correspondence principle of linear viscoelastic theory in order to predict the macroscopic viscoelastic properties of a material composed of uniaxial elastic fibers embedded in a linear viscoelastic matrix.

Production and characterization of pyrolytic oils by pyrolysis of waste machinery oil.

PubMed

Sinağ, Ali; Gülbay, Selen; Uskan, Burçin; Uçar, Suat; Ozgürler, Sara Bilge

2010-01-15

The main objective of this work is to propose an alternative method for evaluation of the waste machinery oil which is an environmental problem in Turkey. For this purpose, pyrolysis of waste machinery oil was conducted in a tubular reactor. Effect of the experimental conditions (various temperatures, catalyst type) on the formation of pyrolytic oil, gas, and char was investigated. Nickel supported on silica and zeolite (HZSM-5) were used as catalysts. Properties of the pyrolytic oils were characterized by gas chromatograph equipped with a mass selective detector (GC-MS), gas chromatography with flame ionization detector (GC-FID for boiling point range distribution), nuclear magnetic resonance ((1)H NMR) spectroscopy, higher heating value measurement, and elemental analysis. The behavior of the metals in the waste machinery oil and the pyrolytic oil samples was also quantitatively detected by inductively coupled plasma (ICP) analysis. As, Cd and Cr contents of the all pyrolytic oils were found as <0.05 ppm, while Cu content of the pyrolytic oils varied between 0.3 ppm and 0.61 ppm. Only Vanadium contents of the pyrolytic oils obtained at 800 degrees C (0.342 ppm) and in the presence of HZSM5 (0.57 ppm) increased compared to that obtained by waste machinery oil (0.1 ppm). Lower metal contents of the pyrolytic oils reveal that pyrolysis of the waste machinery oils leads to the formation of environmental friendly pyrolytic oils with higher heating values.

Self-sensing paper-based actuators employing ferromagnetic nanoparticles and graphite

NASA Astrophysics Data System (ADS)

Phan, Hoang-Phuong; Dinh, Toan; Nguyen, Tuan-Khoa; Vatani, Ashkan; Md Foisal, Abu Riduan; Qamar, Afzaal; Kermany, Atieh Ranjbar; Dao, Dzung Viet; Nguyen, Nam-Trung

2017-04-01

Paper-based microfluidics and sensors have attracted great attention. Although a large number of paper-based devices have been developed, surprisingly there are only a few studies investigating paper actuators. To fulfill the requirements for the integration of both sensors and actuators into paper, this work presents an unprecedented platform which utilizes ferromagnetic particles for actuation and graphite for motion monitoring. The use of the integrated mechanical sensing element eliminates the reliance on image processing for motion detection and also allows real-time measurements of the dynamic response in paper-based actuators. The proposed platform can also be quickly fabricated using a simple process, indicating its potential for controllable paper-based lab on chip.

Roll-to-Roll Laser-Printed Graphene-Graphitic Carbon Electrodes for High-Performance Supercapacitors.

PubMed

Kang, Sangmin; Lim, Kyungmi; Park, Hyeokjun; Park, Jong Bo; Park, Seong Chae; Cho, Sung-Pyo; Kang, Kisuk; Hong, Byung Hee

2018-01-10

Carbon electrodes including graphene and thin graphite films have been utilized for various energy and sensor applications, where the patterning of electrodes is essentially included. Laser scribing in a DVD writer and inkjet printing were used to pattern the graphene-like materials, but the size and speed of fabrication has been limited for practical applications. In this work, we devise a simple strategy to use conventional laser-printer toner materials as precursors for graphitic carbon electrodes. The toner was laser-printed on metal foils, followed by thermal annealing in hydrogen environment, finally resulting in the patterned thin graphitic carbon or graphene electrodes for supercapacitors. The electrochemical cells made of the graphene-graphitic carbon electrodes show remarkably higher energy and power performance compared to conventional supercapacitors. Furthermore, considering the simplicity and scalability of roll-to-roll (R2R) electrode patterning processes, the proposed method would enable cheaper and larger-scale synthesis and patterning of graphene-graphitic carbon electrodes for various energy applications in the future.

Analysis of vibrational response in graphite oxide nanoplatelets

NASA Astrophysics Data System (ADS)

Prias Barragan, Jhon Jairo; Gross, Katherine; Lajaunie, Luc; Arenal, Raul; Ariza Calderon, Hernando; Prieto, Pedro

In this work, we present a new low-cost fabrication process to obtain graphite oxide nanoplatelets from bamboo pyroligneous acid (GO-BPA) by thermal decomposition method using a pyrolysis system for different carbonization temperatures from 673 to 973 K. The GO-BPA samples were characterized by using Raman, FTIR, XRD, SEM and TEM techniques, whose results suggest that increased carbonization temperature increases graphite conversion, boundary defects, desorption of some organic compounds and phonon response, respectively. We discuss potential applications of the GO-BPA samples involving phonon response that would benefit from a fully scaled technology, advanced electronic sensors and devices.

Rhodium nanoparticle-modified screen-printed graphite electrodes for the determination of hydrogen peroxide in tea extracts in the presence of oxygen.

PubMed

Gatselou, Vasiliki A; Giokas, Dimothenis L; Vlessidis, Athanasios G; Prodromidis, Mamas I

2015-03-01

In this work we describe the fabrication of nanostructured electrocatalytic surfaces based on polyethyleneimine (PEI)-supported rhodium nanoparticles (Rh-NP) over graphite screen-printed electrodes (SPEs) for the determination of hydrogen peroxide in the presence of oxygen. Rh-NP, electrostatically stabilized by citrate anions, were immobilized over graphite SPEs, through coulombic attraction on a thin film of positively charged PEI. The functionalized sensors, polarized at 0.0 V vs. Ag/AgCl/3 M KCl, exhibited a linear response to H2O2 over the concentration range from 5 to 600 μmol L(-1) H2O2 in the presence of oxygen. The 3σ limit of detection was 2 μmol L(-1) H2O2, while the reproducibility of the method at the concentration level of 10 μmol L(-1) H2O2 (n=10) and between different sensors (n=4) was lower than 3 and 5%, respectively. Most importantly, the sensors showed an excellent working and storage stability at ambient conditions and they were successfully applied to the determination of H2O2 produced by autooxidation of polylphenols in tea extracts with ageing. Recovery rates ranged between 97 and 104% suggesting that the as-prepared electrodes can be used for the development of small-scale, low-cost chemical sensors for use in on-site applications. Copyright © 2014 Elsevier B.V. All rights reserved.

Metal-coated optical fiber damage sensors

NASA Astrophysics Data System (ADS)

Chang, Chia-Chen; Sirkis, James S.

1993-07-01

A process which uses electroplating methods has been developed to fabricate metal coated optical fiber sensors. The elastic-plastic characteristics of the metal coatings have been exploited to develop a sensor capable of `remembering' low velocity impact damage. These sensors have been investigated under uniaxial tension testing of unembedded sensors and under low velocity impact of graphite/epoxy specimens with embedded sensors using both Michelson and polarimetric optical arrangements. The tests show that coating properties alter the optical fiber sensor performance and that the permanent deformation in the coating can be used to monitor composite delamination/impact damage.

Toward tunable doping in graphene FETs by molecular self-assembled monolayers

NASA Astrophysics Data System (ADS)

Li, Bing; Klekachev, Alexander V.; Cantoro, Mirco; Huyghebaert, Cedric; Stesmans, André; Asselberghs, Inge; de Gendt, Stefan; de Feyter, Steven

2013-09-01

In this paper, we report the formation of self-assembled monolayers (SAMs) of oleylamine (OA) on highly oriented pyrolytic graphite (HOPG) and graphene surfaces and demonstrate the potential of using such organic SAMs to tailor the electronic properties of graphene. Molecular resolution Atomic Force Microscopy (AFM) and Scanning Tunneling Microscopy (STM) images reveal the detailed molecular ordering. The electrical measurements show that OA strongly interacts with graphene leading to n-doping effects in graphene devices. The doping levels are tunable by varying the OA deposition conditions. Importantly, neither hole nor electron mobilities are decreased by the OA modification. As a benefit from this noncovalent modification strategy, the pristine characteristics of the device are recoverable upon OA removal. From this study, one can envision the possibility to correlate the graphene-based device performance with the molecular structure and supramolecular ordering of the organic dopant.In this paper, we report the formation of self-assembled monolayers (SAMs) of oleylamine (OA) on highly oriented pyrolytic graphite (HOPG) and graphene surfaces and demonstrate the potential of using such organic SAMs to tailor the electronic properties of graphene. Molecular resolution Atomic Force Microscopy (AFM) and Scanning Tunneling Microscopy (STM) images reveal the detailed molecular ordering. The electrical measurements show that OA strongly interacts with graphene leading to n-doping effects in graphene devices. The doping levels are tunable by varying the OA deposition conditions. Importantly, neither hole nor electron mobilities are decreased by the OA modification. As a benefit from this noncovalent modification strategy, the pristine characteristics of the device are recoverable upon OA removal. From this study, one can envision the possibility to correlate the graphene-based device performance with the molecular structure and supramolecular ordering of the organic dopant. Electronic supplementary information (ESI) available: AFM images of self-assembled monolayers of OA on HOPG; AFM height image of the graphene surface on a SiC substrate; high resolution STM image of a self-assembled monolayer of OA on HOPG; transfer curves of a graphene FET with and without baking steps; transfer curves of a graphene FET under high vacuum conditions; transfer curves of a graphene FET and its Raman response before and after OA treatment; transfer curves of a graphene FET before and after rinsing with n-hexane. See DOI: 10.1039/c3nr01255g

Porous graphitic carbon nanosheets derived from cornstalk biomass for advanced supercapacitors.

PubMed

Wang, Lei; Mu, Guang; Tian, Chungui; Sun, Li; Zhou, Wei; Yu, Peng; Yin, Jie; Fu, Honggang

2013-05-01

Porous graphitic carbon nanosheets (PGCS) are synthesized by an in situ self-generating template strategy based on the carburized effect of iron with cornstalks. Cornstalks firstly coordinate with [Fe(CN)(6)](4-) ions to form the cornstalk-[Fe(CN)(6)](4-) precursor. After carbonization and removal of the catalyst, PGCS are obtained. Series experiments indicate that PGCS can only be formed when using an iron-based catalyst that can generate a carburized phase during the pyrolytic process. The unique structures of PGCS exhibit excellent capacitive performance. The PGCS-1-1100 sample (synthesized from 0.1 M [Fe(CN)(6)](4-) with a carbonization temperature of 1100 °C), which shows excellent electrochemical capacitance (up to 213 F g(-1) at 1 A g(-1)), cycling stability, and rate performance in 6 M KOH electrolyte. In the two-electrode symmetric supercapacitors, the maximum energy densities that can be achieved are as high as 9.4 and 61.3 Wh kg(-1) in aqueous and organic electrolytes, respectively. Moreover, high energy densities of 8.3 and 40.6 Wh kg(-1) are achieved at the high power density of 10.5 kW kg(-1) in aqueous and organic electrolytes, respectively. This strategy holds great promise for preparing PGCS from natural resources, including cornstalks, as advanced electrodes in supercapacitors. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Influence of Applied Thermal Gradients and a Static Magnetic Field on Bridgman-Grown GeSi Alloys

NASA Technical Reports Server (NTRS)

Volz, M. P.; Szofran, F. R.; Cobb, S. D.; Ritter, T. M.

1999-01-01

The effect of applied axial and radial thermal gradients and an axial static magnetic field on the macrosegregation profiles of Bridgman-grown GeSi alloy crystals has been assessed. The axial thermal gradients were adjusted by changing the control setpoints of a seven-zone vertical Bridgman furnace. The radial thermal gradients were affected by growing samples in ampoules with different thermal conductivities, namely graphite, hot-pressed boron nitride (BN), and pyrolytic boron nitride (PBN). Those samples grown in a graphite ampoule exhibited radial profiles consistent with a highly concave interface and axial profiles indicative of complete mixing in the melt. The samples grown in BN and PBN ampoules had less radial variation. Axial macrosegregation profiles of these samples fell between the predictions for a completely mixed melt and one where solute transport is dominated by diffusion. All of the samples were grown on Ge seeds. This resulted in a period of free growth until the Si concentration in the solid was in equilibrium with the Si concentration in the liquid. The length of crystal grown during this period was inversely proportional to the applied axial thermal gradient. Several samples were grown in an axial 5 Tesla magnetic field. Measured macroscopic segregation profiles on these samples indicate that the magnetic field did not, in general, reduce the melt flow velocities to below the growth velocities.

Physical vapor deposition of one-dimensional nanoparticle arrays on graphite: seeding the electrodeposition of gold nanowires.

PubMed

Cross, C E; Hemminger, J C; Penner, R M

2007-09-25

One-dimensional (1D) ensembles of 2-15 nm diameter gold nanoparticles were prepared using physical vapor deposition (PVD) on highly oriented pyrolytic graphite (HOPG) basal plane surfaces. These 1D Au nanoparticle ensembles (NPEs) were prepared by depositing gold (0.2-0.6 nm/s) at an equivalent thickness of 3-4 nm onto HOPG surfaces at 670-690 K. Under these conditions, vapor-deposited gold nucleated selectively at the linear step edge defects present on these HOPG surfaces with virtually no nucleation of gold particles on terraces. The number density of 2-15 nm diameter gold particles at step edges was 30-40 microm-1. These 1D NPEs were up to a millimeter in length and organized into parallel arrays on the HOPG surface, following the organization of step edges. Surprisingly, the deposition of more gold by PVD did not lead to the formation of continuous gold nanowires at step edges under the range of sample temperature or deposition flux we have investigated. Instead, these 1D Au NPEs were used as nucleation templates for the preparation by electrodeposition of gold nanowires. The electrodeposition of gold occurred selectively on PVD gold nanoparticles over the potential range from 700-640 mV vs SCE, and after optimization of the electrodeposition parameters continuous gold nanowires as small as 80-90 nm in diameter and several micrometers in length were obtained.

Ion irradiation induced surface modification studies of polymers using SPM

NASA Astrophysics Data System (ADS)

Tripathi, A.; Kumar, Amit; Singh, F.; Kabiraj, D.; Avasthi, D. K.; Pivin, J. C.

2005-07-01

Various types of scanning probe microscopy (SPM) techniques: atomic force microscopy (AFM) (contact and tapping in height and amplitude mode), scanning tunnelling microscopy (STM) and conducting atomic force microscopy (C-AFM) are used for studying ion beam induced surface modifications, nanostructure/cluster formation and disintegration in polymers and similar soft carbon based materials. In the present study, the results of studies on four materials, namely, (A) methyltriethoxysilane/phenyltriethoxysilane (MTES/PTES) based gel, (B) triethoxisilane (TH) based gel, (C) highly oriented pyrolytic graphite (HOPG) bulk and (D) fullerene (C60) thin films are discussed. In the case of Si based gels prepared from pre-cursors containing organic groups (MTES/PTES), hillocks are observed at the surface and their size decreases from 70 to 25 nm with increasing fluence, whereas, in the case of a gel with a stoichiometry SiO1.25H1, prepared from TH, an increases in the size of hillocks is observed. Hillocks are also formed at the surface of HOPG irradiated with 120 MeV Au beam at a low fluence, whereas, formation of craters and a re-organisation of surface features is observed at a higher fluence. In the case of C60 films, 120 MeV Au ion irradiation induces the formation of conducting ion tracks, which is attributed to the transformation from insulating C60 to conducting graphite like carbon.

Some Recent Sensor-Related Army Critical Technology Events

DTIC Science & Technology

2013-02-01

Excalibur (XM982), US Army 2010 Weapon Systems, prepared by OASA (ALT), 92. 15 HAudraH Colloway, “Picatinney’s GPS-guided Excalibur artillery round deemed...liquid phase epitaxy (LPE) and molecular-organo-chemical vapor deposition (MOCVD). There was also an effort in platinum silicide (PtSi) infrared...protective interphasial chemistry not only on transition metal oxide cathodes at high voltage, but also on graphitic graphite at low voltage making

Method for fabricating thin films of pyrolytic carbon

DOEpatents

Brassell, G.W.; Lewis, J. Jr.; Weber, G.W.

1980-03-13

The present invention relates to a method for fabricating ultrathin films of pyrolytic carbon. Pyrolytic carbon is vapor deposited onto a concave surface of a heated substrate to a total uniform thickness in the range of about 0.1 to 1.0 micrometer. The carbon film on the substrate is provided with a layer of adherent polymeric resin. The resulting composite film of pyrolytic carbon and polymeric resin is then easily separated from the substrate by shrinking the 10 polymeric resin coating with thermally induced forces.

Method for fabricating thin films of pyrolytic carbon

DOEpatents

Brassell, Gilbert W.; Lewis, Jr., John; Weber, Gary W.

1982-01-01

The present invention relates to a method for fabricating ultra-thin films of pyrolytic carbon. Pyrolytic carbon is vapor deposited onto a concave surface of a heated substrate to a total uniform thickness in the range of about 0.1 to 1.0 micrometer. The carbon film on the substrate is provided with a layer of adherent polymeric resin. The resulting composite film of pyrolytic carbon and polymeric resin is then easily separated from the substrate by shrinking the polymeric resin coating with thermally induced forces.

Graphene-based electrochemical sensor for detection of 2,4,6-trinitrotoluene (TNT) in seawater: the comparison of single-, few-, and multilayer graphene nanoribbons and graphite microparticles.

PubMed

Goh, Madeline Shuhua; Pumera, Martin

2011-01-01

The detection of explosives in seawater is of great interest. We compared response single-, few-, and multilayer graphene nanoribbons and graphite microparticle-based electrodes toward the electrochemical reduction of 2,4,6-trinitrotoluene (TNT). We optimized parameters such as accumulation time, accumulation potential, and pH. We found that few-layer graphene exhibits about 20% enhanced signal for TNT after accumulation when compared to multilayer graphene nanoribbons. However, graphite microparticle-modified electrode provides higher sensitivity, and there was no significant difference in the performance of single-, few-, and multilayer graphene nanoribbons and graphite microparticles for the electrochemical detection of TNT. We established the limit of detection of TNT in untreated seawater at 1 μg/mL.

Fundamental studies of graphene/graphite and graphene-based Schottky photovoltaic devices

NASA Astrophysics Data System (ADS)

Miao, Xiaochang

In the carbon allotropes family, graphene is one of the most versatile members and has been extensively studied since 2004. The goal of this dissertation is not only to investigate the novel fundamental science of graphene and its three-dimensional sibling, graphite, but also to explore graphene's promising potential in modern electronic and optoelectronic devices. The first two chapters provide a concise introduction to the fundamental solid state physics of graphene (as well as graphite) and the physics at the metal/semiconductor interfaces. In the third chapter, we demonstrate the formation of Schottky junctions at the interfaces of graphene (semimetal) and various inorganic semiconductors that play dominating roles in today's semiconductor technology, such as Si, SiC, GaAs and GaN. As shown from their current-voltage (I -V) and capacitance-voltage (C-V) characteristics, the interface physics can be well described within the framework of the Schottky-Mott model. The results are also well consist with that from our previous studies on graphite based Schottky diodes. In the fourth chapter, as an extension of graphene based Schottky work, we investigate the photovoltaic (PV) effect of graphene/Si junctions after chemically doped with an organic polymer (TFSA). The power conversion efficiency of the solar cell improves from 1.9% to 8.6% after TFSA doping, which is the record in all graphene based PVs. The I -V, C-V and external quantum efficiency measurements suggest 12 that such a significant enhancement in the device performance can be attributed to a doping-induced decrease in the series resistance and a simultaneous increase in the built-in potential. In the fifth chapter, we investigate for the first time the effect of uniaxial strains on magneto-transport properties of graphene. We find that low-temperature weak localization effect in monolayer graphene is gradually suppressed under increasing strains, which is due to a strain-induced decreased intervalley-scattering rate. In chapter 6, we study the high vacuum thermal annealing effect on an unconventional ferromagnetism (FM) in highly oriented pyrolytic graphite (HOPG). The FM diminishes and eventually disappears in annealed samples accompanied by improved electrical transport properties and crystallinity. Our results indicate that the FM is mainly coming from the lattice imperfections.

Graphene Oxide-Assisted Liquid Phase Exfoliation of Graphite into Graphene for Highly Conductive Film and Electromechanical Sensors.

PubMed

Tung, Tran Thanh; Yoo, Jeongha; Alotaibi, Faisal K; Nine, Md J; Karunagaran, Ramesh; Krebsz, Melinda; Nguyen, Giang T; Tran, Diana N H; Feller, Jean-Francois; Losic, Dusan

2016-06-29

Here, we report a new method to prepare graphene from graphite by the liquid phase exfoliation process with sonication using graphene oxide (GO) as a dispersant. It was found that GO nanosheets act a as surfactant to the mediated exfoliation of graphite into a GO-adsorbed graphene complex in the aqueous solution, from which graphene was separated by an additional process. The preparation of isolated graphene from a single to a few layers is routinely achieved with an exfoliation yield of up to higher than 40% from the initial graphite material. The prepared graphene sheets showed a high quality (C/O ∼ 21.5), low defect (ID/IG ∼ 0.12), and high conductivity (6.2 × 10(4) S/m). Moreover, the large lateral size ranging from 5 to 10 μm of graphene, which is believed to be due to the shielding effect of GO avoiding damage under ultrasonic jets and cavitation formed by the sonication process. The thin graphene film prepared by the spray-coating technique showed a sheet resistance of 668 Ω/sq with a transmittance of 80% at 550 nm after annealing at 350 °C for 3 h. The transparent electrode was even greater with the resistance only 66.02 Ω when graphene is deposited on an interdigitated electrode (1 mm gap). Finally, a flexible sensor based on a graphene spray-coating polydimethylsiloxane (PDMS) is demonstrated showing excellent performance working under human touch pressure (<10 kPa). The graphene prepared by this method has some distinct properties showing it as a promising material for applications in electronics including thin film coatings, transparent electrodes, wearable electronics, human monitoring sensors, and RFID tags.

Structure and radical scavenging activity relationships of pyrolytic lignins

USDA-ARS?s Scientific Manuscript database

This work deals with antioxidant properties of pyrolytic lignins against two free radicals, the 1,1-diphenyl-2-picrylhydrazyl and the 2,2'-Azino-bis(3-ethylbenzothiazoline-6-sulfonic acid). Pyrolytic lignins produced by the thermal pyrolysis of the Etek lignin were extracted from the liquid pyrolysi...

Glucose sensing on graphite screen-printed electrode modified by sparking of copper nickel alloys.

PubMed

Riman, Daniel; Spyrou, Konstantinos; Karantzalis, Alexandros E; Hrbac, Jan; Prodromidis, Mamas I

2017-04-01

Electric spark discharge was employed as a green, fast and extremely facile method to modify disposable graphite screen-printed electrodes (SPEs) with copper, nickel and mixed copper/nickel nanoparticles (NPs) in order to be used as nonenzymatic glucose sensors. Direct SPEs-to-metal (copper, nickel or copper/nickel alloys with 25/75, 50/50 and 75/25wt% compositions) sparking at 1.2kV was conducted in the absence of any solutions under ambient conditions. Morphological characterization of the sparked surfaces was performed by scanning electron microscopy, while the chemical composition of the sparked NPs was evaluated with energy dispersive X-ray spectroscopy and X-ray photoelectron spectroscopy. The performance of the various sparked SPEs towards the electro oxidation of glucose in alkaline media and the critical role of hydroxyl ions were evaluated with cyclic voltammetry and kinetic studies. Results indicated a mixed charge transfer- and hyroxyl ion transport-limited process. Best performing sensors fabricated by Cu/Ni 50/50wt% alloy showed linear response over the concentration range 2-400μM glucose and they were successfully applied to the amperometric determination of glucose in blood. The detection limit (S/N 3) and the relative standard deviation of the method were 0.6µM and <6% (n=5, 2µM glucose), respectively. Newly devised sparked Cu/Ni graphite SPEs enable glucose sensing with distinct advantages over existing glucose chemical sensors in terms of cost, fabrication simplicity, disposability, and adaptation of green methods in sensor's development. Copyright © 2017 Elsevier B.V. All rights reserved.

Carbon paste electrode with covalently immobilized thionine for electrochemical sensing of hydrogen peroxide

NASA Astrophysics Data System (ADS)

Thenmozhi, K.; Sriman Narayanan, S.

2017-11-01

A water-soluble redox mediator, thionin was covalently immobilized to the functionalized graphite powder and a carbon paste electrode was fabricated from this modified graphite powder. The immobilization procedure proved to be effective in anchoring the thionin mediator in the graphite electrode setup without any leakage problem during the electrochemical studies. The covalent immobilization of the thionin mediator was studied with FT-IR and the electrochemical response of the thionin carbon paste electrode was optimized on varying the supporting electrolyte, pH and scan rate. The modified electrode exhibited well-defined electrocatalytic activity towards the reduction of H2O2 at a lower potential of -0.266 V with good sensitivity. The developed amperometric sensor was efficient towards H2O2 in the linear range from 2.46 × 10-5 M to 4.76 × 10-3 M, with a detection limit of 1.47 × 10-5 M respectively. Important advantages of this sensor are its excellent electrochemical performance, simple fabrication, easy renewability, reproducible analytical results, acceptable accuracy and good operational and long-term stability.

Interfacial effects in ZnO nanotubes/needle-structured graphitic diamond nanohybrid for detecting dissolved acetone at room temperature

NASA Astrophysics Data System (ADS)

Kathiravan, Deepa; Huang, Bohr-Ran; Saravanan, Adhimoorthy; Yeh, Chien-Jui; Leou, Keh-Chyang; Lin, I.-Nan

2017-12-01

A high-performance ZnO nanotubes (ZNTs)/needle-structured graphitic diamond (NGD) nanohybrid material was prepared and observed the electrochemical sensing properties of liquid acetone in water. Initially, we synthesized NGD film using bias-enhanced growth (BEG) process. Afterwards, a well-etched ZNTs were spatially grown on the NGD film using simple hydrothermal method, and utilized as sensing material for assemble an electrochemical sensor (via EGFET configuration) operating at room temperature. The systematic investigations depict the ultra-high sensing properties attained from ZNTs grown on NGD film. The NGD film mostly have needle or wire shaped diamond grains, which contributes extremely high electrical conductivity. Furthermore, needle shaped diamond grains cover with multi-layer graphitic material generates conduction channels for ZNTs and leads to enhance the oxygen residuals and species. The material stability and conductivity of NGD as well the defects exist with oxygen vacancies in ZNTs offers superior sensing properties. Thus, the interesting combination of these wide band gap semiconductor materials exhibit high sensor response (89 mV/mL), high stability and long-term reliability (tested after 60 days).

Flower-like Copper Cobaltite Nanosheets on Graphite Paper as High-Performance Supercapacitor Electrodes and Enzymeless Glucose Sensors.

PubMed

Liu, Shude; Hui, K S; Hui, K N

2016-02-10

Flower-like copper cobaltite (CuCo2O4) nanosheets anchored on graphite paper have been synthesized using a facile hydrothermal method followed by a postannealing treatment. Supercapacitor electrodes employing CuCo2O4 nanosheets exhibit an enhanced capacitance of 1131 F g(-1) at a current density of 1 A g(-1) compared with previously reported supercapacitor electrodes. The CuCo2O4 electrode delivers a specific capacitance of up to 409 F g(-1) at a current density of as high as 50 A g(-1), and a good long-term cycling stability, with 79.7% of its specific capacitance retained after 5000 cycles at 10 A g(-1). Furthermore, the as-prepared CuCo2O4 nanosheets on graphite paper can be fabricated as electrodes and used as enzymeless glucose sensors, which exhibit good sensitivity (3.625 μA μM(-1) cm(-2)) and an extraordinary linear response ranging up to 320 μM with a low detection limit (5 μM).

Label-free voltammetric detection of MicroRNAs at multi-channel screen printed array of electrodes comparison to graphite sensors.

PubMed

Erdem, Arzum; Congur, Gulsah

2014-01-01

The multi-channel screen-printed array of electrodes (MUX-SPE16) was used in our study for the first time for electrochemical monitoring of nucleic acid hybridization related to different miRNA sequences (miRNA-16, miRNA-15a and miRNA-660, i.e, the biomarkers for Alzheimer disease). The MUX-SPE16 was also used for the first time herein for the label-free electrochemical detection of nucleic acid hybridization combined magnetic beads (MB) assay in comparison to the disposable pencil graphite electrode (PGE). Under the principle of the magnetic beads assay, the biotinylated inosine substituted DNA probe was firstly immobilized onto streptavidin coated MB, and then, the hybridization process between probe and its complementary miRNA sequence was performed at MB surface. The voltammetric transduction was performed using differential pulse voltammetry (DPV) technique in combination with the single-use graphite sensor technologies; PGE and MUX-SPE16 for miRNA detection by measuring the guanine oxidation signal without using any external indicator. The features of single-use sensor technologies, PGE and MUX-SPE16, were discussed concerning to their reproducibility, detection limit, and selectivity compared to the results in the earlier studies presenting the electrochemical miRNA detection related to different miRNA sequences. © 2013 Elsevier B.V. All rights reserved.

Linearization of calibration curves by aerosol carrier effect of CCl 4 vapor in electrothermal vaporization inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Kántor, Tibor; de Loos-Vollebregt, Margaretha T. C.

2005-03-01

Carbon tetrachloride vapor as gaseous phase modifier in a graphite furnace electrothermal vaporizer (GFETV) converts heavy volatile analyte forms to volatile and medium volatile chlorides and produces aerosol carrier effect, the latter being a less generally recognized benefit. However, the possible increase of polyatomic interferences in inductively coupled plasma mass spectrometry (GFETV-ICP-MS) by chlorine and carbon containing species due to CCl 4 vapor introduction has been discouraging with the use of low resolution, quadrupole type MS equipment. Being aware of this possible handicap, it was aimed at to investigate the feasibility of the use of this halogenating agent in ICP-MS with regard of possible hazards to the instrument, and also to explore the advantages under these specific conditions. With sample gas flow (inner gas flow) rate not higher than 900 ml min -1 Ar in the torch and 3 ml min -1 CCl 4 vapor flow rate in the furnace, the long-term stability of the instrument was ensured and the following benefits by the halocarbon were observed. The non-linearity error (defined in the text) of the calibration curves (signal versus mass functions) with matrix-free solution standards was 30-70% without, and 1-5% with CCl 4 vapor introduction, respectively, at 1 ng mass of Cu, Fe, Mn and Pb analytes. The sensitivity for these elements increased by 2-4-fold with chlorination, while the relative standard deviation (RSD) was essentially the same (2-5%) for the two cases in comparison. A vaporization temperature of 2650 °C was required for Cr in Ar atmosphere, while 2200 °C was sufficient in Ar + CCl 4 atmosphere to attain complete vaporization. Improvements in linear response and sensitivity were the highest for this least volatile element. The pyrolytic graphite layer inside the graphite tube was protected by the halocarbon, and tube life time was further increased by using traces of hydrocarbon vapor in the external sheath gas of the graphite furnace. Details of the modification of the gas supply for HGA-600MS furnace and the design of the volatilization device are described.

Rapid prototyping of carbon-based chemiresistive gas sensors on paper

PubMed Central

Mirica, Katherine A.; Azzarelli, Joseph M.; Weis, Jonathan G.; Schnorr, Jan M.; Swager, Timothy M.

2013-01-01

Chemically functionalized carbon nanotubes (CNTs) are promising materials for sensing of gases and volatile organic compounds. However, the poor solubility of carbon nanotubes hinders their chemical functionalization and the subsequent integration of these materials into devices. This manuscript describes a solvent-free procedure for rapid prototyping of selective chemiresistors from CNTs and graphite on the surface of paper. This procedure enables fabrication of functional gas sensors from commercially available starting materials in less than 15 min. The first step of this procedure involves the generation of solid composites of CNTs or graphite with small molecule selectors—designed to interact with specific classes of gaseous analytes—by solvent-free mechanical mixing in a ball mill and subsequent compression. The second step involves deposition of chemiresistive sensors by mechanical abrasion of these solid composites onto the surface of paper. Parallel fabrication of multiple chemiresistors from diverse composites rapidly generates cross-reactive arrays capable of sensing and differentiating gases and volatile organic compounds at part-per-million and part-per-thousand concentrations. PMID:23942132

Damage to the microbial cell membrane during pyrolytic sugar utilization and strategies for increasing resistance.

PubMed

Jin, Tao; Rover, Marjorie R; Petersen, Elspeth M; Chi, Zhanyou; Smith, Ryan G; Brown, Robert C; Wen, Zhiyou; Jarboe, Laura R

2017-09-01

Lignocellulosic biomass is an appealing feedstock for the production of biorenewable fuels and chemicals, and thermochemical processing is a promising method for depolymerizing it into sugars. However, trace compounds in this pyrolytic sugar syrup are inhibitory to microbial biocatalysts. This study demonstrates that hydrophobic inhibitors damage the cell membrane of ethanologenic Escherichia coli KO11+lgk. Adaptive evolution was employed to identify design strategies for improving pyrolytic sugar tolerance and utilization. Characterization of the resulting evolved strain indicates that increased resistance to the membrane-damaging effects of the pyrolytic sugars can be attributed to a glutamine to leucine mutation at position 29 of carbon storage regulator CsrA. This single amino acid change is sufficient for decreasing EPS protein production and increasing membrane integrity when exposed to pyrolytic sugars.

Destruction Chemistry of Mustard Simulants

DTIC Science & Technology

2008-07-04

organosulfur compounds under both pyrolytic and oxidative conditions. We focus on the destruction of alkyl sulfides that are surrogates for chemical...destruction chemistry of organosulfur compounds under both pyrolytic and oxidative conditions. We focus on the destruction of alkyl sulfides that are...ACCOMPLISHMENTS ABSTRACT This study investigates the destruction chemistry of organosulfur compounds under both pyrolytic and oxidative conditions. We

Studies of Reduced Graphene Oxide and Graphite Oxide in the Aspect of Their Possible Application in Gas Sensors

PubMed Central

Drewniak, Sabina; Muzyka, Roksana; Stolarczyk, Agnieszka; Pustelny, Tadeusz; Kotyczka-Morańska, Michalina; Setkiewicz, Maciej

2016-01-01

The paper presents the results of investigations on resistance structures based on graphite oxide (GRO) and graphene oxide (rGO). The subject matter of the investigations was thaw the sensitivity of the tested structures was affected by hydrogen, nitrogen dioxide and carbon dioxide. The experiments were performed at a temperature range from 30 °C to 150 °C in two carrier gases: nitrogen and synthetic air. The measurements were also aimed at characterization of the graphite oxide and graphene oxide. In our measurements we used (among others) techniques such as: Atomic Force Microscopy (AFM); Scanning Electron Microscopy (SEM); Raman Spectroscopy (RS); Fourier Transform Infrared Spectroscopy (FT-IR) and X-ray Photoelectron Microscopy (XPS). The data resulting from the characterizations of graphite oxide and graphene oxide have made it possible to interpret the obtained results from the point of view of physicochemical changes occurring in these structures. PMID:26784198

Structure of a peptide adsorbed on graphene and graphite.

PubMed

Katoch, Jyoti; Kim, Sang Nyon; Kuang, Zhifeng; Farmer, Barry L; Naik, Rajesh R; Tatulian, Suren A; Ishigami, Masa

2012-05-09

Noncovalent functionalization of graphene using peptides is a promising method for producing novel sensors with high sensitivity and selectivity. Here we perform atomic force microscopy, Raman spectroscopy, infrared spectroscopy, and molecular dynamics simulations to investigate peptide-binding behavior to graphene and graphite. We studied a dodecamer peptide identified with phage display to possess affinity for graphite. Optical spectroscopy reveals that the peptide forms secondary structures both in powder form and in an aqueous medium. The dominant structure in the powder form is α-helix, which undergoes a transition to a distorted helical structure in aqueous solution. The peptide forms a complex reticular structure upon adsorption on graphene and graphite, having a helical conformation different from α-helix due to its interaction with the surface. Our observation is consistent with our molecular dynamics calculations, and our study paves the way for rational functionalization of graphene using biomolecules with defined structures and, therefore, functionalities.

Studies of Reduced Graphene Oxide and Graphite Oxide in the Aspect of Their Possible Application in Gas Sensors.

PubMed

Drewniak, Sabina; Muzyka, Roksana; Stolarczyk, Agnieszka; Pustelny, Tadeusz; Kotyczka-Morańska, Michalina; Setkiewicz, Maciej

2016-01-15

The paper presents the results of investigations on resistance structures based on graphite oxide (GRO) and graphene oxide (rGO). The subject matter of the investigations was thaw the sensitivity of the tested structures was affected by hydrogen, nitrogen dioxide and carbon dioxide. The experiments were performed at a temperature range from 30 °C to 150 °C in two carrier gases: nitrogen and synthetic air. The measurements were also aimed at characterization of the graphite oxide and graphene oxide. In our measurements we used (among others) techniques such as: Atomic Force Microscopy (AFM); Scanning Electron Microscopy (SEM); Raman Spectroscopy (RS); Fourier Transform Infrared Spectroscopy (FT-IR) and X-ray Photoelectron Microscopy (XPS). The data resulting from the characterizations of graphite oxide and graphene oxide have made it possible to interpret the obtained results from the point of view of physicochemical changes occurring in these structures.

Deducing 2D Crystal Structure at the Solid/Liquid Interface with Atomic Resolution by Combined STM and SFG Study

NASA Astrophysics Data System (ADS)

McClelland, Arthur; Ahn, Seokhoon; Matzger, Adam J.; Chen, Zhan

2009-03-01

Supplemented by computed models, Scanning Tunneling Microscopy (STM) can provide detailed structure of 2D crystals formed at the liquid/solid interface with atomic resolution. However, some structural information such as functional group orientations in such 2D crystals needs to be tested experimentally to ensure the accuracy of the deduced structures. Due to the limited sensitivity, many other experimental techniques such as Raman and infrared spectroscopy have not been allowed to provide such structural information of 2D crystals. Here we showed that Sum Frequency Generation Vibrational Spectroscopy (SFG) can measure average orientation of functional groups in such 2D crystals, or physisorbed monolayers, providing key experimental data to aid in the modeling and interpretation of the STM images. The usefulness of combining these two techniques is demonstrated with a phthalate diesters monolayer formed at the 1-phenyloctane/ highly oriented pyrolytic graphite (HOPG) interface. The spatial orientation of the ester C=O of the monolayer was successfully determined using SFG.

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

Liscio, A.; CNISM and Dipartimento di Fisica, Universita di Roma Tre, Via Vasca Navale 84, 00146 Roma; Ruocco, A.

This paper deals with the mechanism of grazing incidence (e,2e) events from surfaces. Two different approaches are considered. In both cases, elastic scattering with the crystal lattice assists the inelastic collision; these two steps are coupled either coherently or incoherently. Experimental evidence is given that the 'coherent' approach reproduces better the cross section dependence on momentum transfer in the specific case of asymmetric kinematics at moderate electron energies. This model has allowed us to map out the band dispersion of the outermost valence states of highly oriented pyrolytic graphite and to measure the momentum distribution of {pi}-electron states without invokingmore » the contribution of reciprocal lattice vectors in the momentum conservation. Agreement between theory and experiment is satisfactory, though the presence of events where crystal momentum is reconstructed cannot be ruled out. These results, obtained with a significant reduction of the experiment duration by an implemented apparatus, show that reflection (e,2e) can be used to build up a momentum spectroscopy with high surface sensitivity.« less

Determination of the Wetting Angle of Germanium and Germanium-Silicon Melts on Different Substrate Materials

NASA Technical Reports Server (NTRS)

Kaiser, Natalie; Croell, Arne; Szofran, F. R.; Cobb. S. D.; Dold, P.; Benz, K. W.

1999-01-01

During Bridgman growth of semiconductors detachment of the crystal and the melt meniscus has occasionally been observed, mainly under microgravity (microg) conditions. An important factor for detached growth is the wetting angle of the melt with the crucible material. High contact angles are more likely to result in detachment of the growing crystal from the ampoule wall. In order to achieve detached growth of germanium (Ge) and germanium-silicon (GeSi) crystals under 1g and microg conditions, sessile drop measurements were performed to determine the most suitable ampoule material as well as temperature dependence of the surface tension for GeSi. Sapphire, fused quartz, glassy carbon, graphite, SiC, pyrolytic Boron Nitride (pBN), AIN, and diamond were used as substrates. Furthermore, different cleaning procedures and surface treatments (etching, sandblasting, etc.) of the same substrate material and their effect on the wetting behavior were studied during these experiments. pBN and AIN substrates exhibited the highest contact angles with values around 170 deg.

Addressing individual metal ion centers in supramolecules by STS

NASA Astrophysics Data System (ADS)

Alam, M. S.; Ako, A. M.; Ruben, M.; Thompson, L. K.; Lehn, J.-M.

2005-03-01

As the information of STM measurements arises from electronic structure, separating information on the topography is not straightforward for complex molecules. Scanning tunneling spectroscopy (STS) measurements give information about the molecular energy levels, which are next to the molecules Fermi level. Using a home built STM working under ambient conditions, we succeeded to combine high resolution topography mapping with simultaneous current-voltage characteristics (STS) measurements on single molecules deposited on highly oriented pyrolytic graphite surfaces. We present our recent results on grid-type molecules [Co4L4] (L=4,6-bis(2',2''-bipyridyl-6-yl)pyrimidine) and [Mn9L6] (L=2POAP-2H) as well as on ring-shaped Fe ion chains [Fe6Cl6L6] (L=1-Ecosyliminodiethanol). Small, regular molecule clusters as well as separated single molecules were observed. We found a rather large contrast at the expected location of the metal centers in our molecules, i.e. the location of the individual metal ions in their organic matrix is directly addressable by STS.

Space processing of composite materials

NASA Technical Reports Server (NTRS)

Steurer, W. H.; Kaye, S.

1975-01-01

Materials and processes for the testing of aluminum-base fiber and particle composites, and of metal foams under extended-time low-g conditions were investigated. A wetting and dispersion technique was developed, based on the theory that under the absence of a gas phase all solids are wetted by liquids. The process is characterized by a high vacuum environment and a high temperature cycle. Successful wetting and dispersion experiments were carried out with sapphire fibers, whiskers and particles, and with fibers of silicon carbide, pyrolytic graphite and tungsten. The developed process and facilities permit the preparation of a precomposite which serves as sample material for flight experiments. Low-g processing consists then merely in the uniform redistribution of the reinforcements during a melting cycle. For the preparation of metal foams, gas generation by means of a thermally decomposing compound was found most adaptable to flight experiments. For flight experiments, the use of compacted mixture of the component materials limits low-g processing to a simple melt cycle.

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

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

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

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

Metastable nanobubbles at the solid-liquid interface due to contact angle hysteresis.

PubMed

Nishiyama, Takashi; Yamada, Yutaka; Ikuta, Tatsuya; Takahashi, Koji; Takata, Yasuyuki

2015-01-27

Nanobubbles exist at solid-liquid interfaces between pure water and hydrophobic surfaces with very high stability, lasting in certain cases up to several days. Not only semispherical but also other shapes, such as micropancakes, are known to exist at such interfaces. However, doubt has been raised as to whether or not the nanobubbles are gas-phase entities. In this study, surface nanobubbles at a pure water-highly ordered pyrolytic graphite (HOPG) interface were investigated by peak force quantitative nanomechanics (PF-QNM). Multiple isolated nanobubbles generated by the solvent-exchange method were present on the terraced areas, avoiding the steps of the HOPG surface. Adjacent nanobubbles coalesced and formed metastable nanobubbles. Coalescence was enhanced by the PF-QNM measurement. We determined that nanobubbles can exist for a long time because of nanoscale contact angle hysteresis at the water-HOPG interface. Moreover, the hydrophilic steps of HOPG were avoided during coalescence, providing evidence that the nanobubbles are truly gas phase.

Surface rearrangement of water-immersed hydrophobic solids by gaseous nanobubbles.

PubMed

Tarábková, Hana; Bastl, Zdeněk; Janda, Pavel

2014-12-09

Interactions of gaseous (ambient) nanobubbles (10-100 nm diameter) with different hydrophobic materials-Teflon, polystyrene, paraffin, and basal plane highly ordered pyrolytic graphite (HOPG)-are studied by AFM in situ and ex situ. Exactly identical surface locations are examined before and after exposure to ambient gas nanobubbles in deionized water and compared for nanomorphological changes. While freely flooded/immersed surfaces, regularly occupied by nanobubbles, do not exhibit resolvable alterations, significant surface rearrangement is found on whole flooded area after mild pressure drop (10 kPa) applied on the solid-liquid interface. Nanopattern and its characteristic dimension appear to be material specific and solely reflect surface-nanobubble interaction. Mild, nonswelling, noncorrosive conditions (20 °C, deionized water) prevent intervention of chemical reaction and high-energy-demanding processes. Experimental results, in accordance with the presented model, indicate that the mild pressure drop triggers expansion of pinned nanobubbles, imposing local tensile stress on the solid surface. Consequently, nanobubbles should be considered as large-area nanoscale patterning elements.

Septipyridines as conformationally controlled substitutes for inaccessible bis(terpyridine)-derived oligopyridines in two-dimensional self-assembly

PubMed Central

Caterbow, Daniel; Künzel, Daniela; Mavros, Michael G; Groß, Axel; Landfester, Katharina

2011-01-01

Summary The position of the peripheral nitrogen atoms in bis(terpyridine)-derived oligopyridines (BTPs) has a strong impact on their self-assembly behavior at the liquid/HOPG (highly oriented pyrolytic graphite) interface. The intermolecular hydrogen bonding interactions in these peripheral pyridine units show specific 2D structures for each BTP isomer. From nine possible constitutional isomers only four have been described in the literature. The synthesis and self-assembling behavior of an additional isomer is presented here, but the remaining four members of the series are synthetically inaccessible. The self-assembling properties of three of the missing four BTP isomers can be mimicked by making use of the energetically preferred N–C–C–N transoid conformation between 2,2'-bipyridine subunits in a new class of so-called septipyridines. The structures are investigated by scanning tunneling microscopy (STM) and a combination of force-field and first-principles electronic structure calculations. PMID:22003448

Diffraction based method to reconstruct the spectrum of the Thomson scattering x-ray source

NASA Astrophysics Data System (ADS)

Chi, Zhijun; Yan, Lixin; Zhang, Zhen; Zhou, Zheng; Zheng, Lianmin; Wang, Dong; Tian, Qili; Wang, Wei; Nie, Zan; Zhang, Jie; Du, Yingchao; Hua, Jianfei; Shi, Jiaru; Pai, Chihao; Lu, Wei; Huang, Wenhui; Chen, Huaibi; Tang, Chuanxiang

2017-04-01

As Thomson scattering x-ray sources based on the collision of intense laser and relativistic electrons have drawn much attention in various scientific fields, there is an increasing demand for the effective methods to reconstruct the spectrum information of the ultra-short and high-intensity x-ray pulses. In this paper, a precise spectrum measurement method for the Thomson scattering x-ray sources was proposed with the diffraction of a Highly Oriented Pyrolytic Graphite (HOPG) crystal and was demonstrated at the Tsinghua Thomson scattering X-ray source. The x-ray pulse is diffracted by a 15 mm (L) ×15 mm (H)× 1 mm (D) HOPG crystal with 1° mosaic spread. By analyzing the diffraction pattern, both x-ray peak energies and energy spectral bandwidths at different polar angles can be reconstructed, which agree well with the theoretical value and simulation. The higher integral reflectivity of the HOPG crystal makes this method possible for single-shot measurement.

Diffraction based method to reconstruct the spectrum of the Thomson scattering x-ray source.

PubMed

Chi, Zhijun; Yan, Lixin; Zhang, Zhen; Zhou, Zheng; Zheng, Lianmin; Wang, Dong; Tian, Qili; Wang, Wei; Nie, Zan; Zhang, Jie; Du, Yingchao; Hua, Jianfei; Shi, Jiaru; Pai, Chihao; Lu, Wei; Huang, Wenhui; Chen, Huaibi; Tang, Chuanxiang

2017-04-01

As Thomson scattering x-ray sources based on the collision of intense laser and relativistic electrons have drawn much attention in various scientific fields, there is an increasing demand for the effective methods to reconstruct the spectrum information of the ultra-short and high-intensity x-ray pulses. In this paper, a precise spectrum measurement method for the Thomson scattering x-ray sources was proposed with the diffraction of a Highly Oriented Pyrolytic Graphite (HOPG) crystal and was demonstrated at the Tsinghua Thomson scattering X-ray source. The x-ray pulse is diffracted by a 15 mm (L) ×15 mm (H)× 1 mm (D) HOPG crystal with 1° mosaic spread. By analyzing the diffraction pattern, both x-ray peak energies and energy spectral bandwidths at different polar angles can be reconstructed, which agree well with the theoretical value and simulation. The higher integral reflectivity of the HOPG crystal makes this method possible for single-shot measurement.

A priori calculations of the free energy of formation from solution of polymorphic self-assembled monolayers.

PubMed

Reimers, Jeffrey R; Panduwinata, Dwi; Visser, Johan; Chin, Yiing; Tang, Chunguang; Goerigk, Lars; Ford, Michael J; Sintic, Maxine; Sum, Tze-Jing; Coenen, Michiel J J; Hendriksen, Bas L M; Elemans, Johannes A A W; Hush, Noel S; Crossley, Maxwell J

2015-11-10

Modern quantum chemical electronic structure methods typically applied to localized chemical bonding are developed to predict atomic structures and free energies for meso-tetraalkylporphyrin self-assembled monolayer (SAM) polymorph formation from organic solution on highly ordered pyrolytic graphite surfaces. Large polymorph-dependent dispersion-induced substrate-molecule interactions (e.g., -100 kcal mol(-1) to -150 kcal mol(-1) for tetratrisdecylporphyrin) are found to drive SAM formation, opposed nearly completely by large polymorph-dependent dispersion-induced solvent interactions (70-110 kcal mol(-1)) and entropy effects (25-40 kcal mol(-1) at 298 K) favoring dissolution. Dielectric continuum models of the solvent are used, facilitating consideration of many possible SAM polymorphs, along with quantum mechanical/molecular mechanical and dispersion-corrected density functional theory calculations. These predict and interpret newly measured and existing high-resolution scanning tunnelling microscopy images of SAM structure, rationalizing polymorph formation conditions. A wide range of molecular condensed matter properties at room temperature now appear suitable for prediction and analysis using electronic structure calculations.

Electrodeposition of Si from an Ionic Liquid Bath at Room Temperature in the Presence of Water.

PubMed

Shah, Nisarg K; Pati, Ranjan Kumar; Ray, Abhijit; Mukhopadhyay, Indrajit

2017-02-21

The electrochemical deposition of Si has been carried out in an ionic liquid medium in the presence of water in a limited dry nitrogen environment on highly oriented pyrolytic graphite (HOPG) at room temperature. It has been found that the presence of water in ionic liquids does not affect the available effective potential window to a large extent. Silicon has been successfully deposited electrochemically in the overpotential regime in two different ionic liquids, namely, BMImTf 2 N and BMImPF 6 , in the presence of water. Although a Si thin film has been obtained from BMImTf 2 N; only distinguished Si crystals protected in ionic liquid droplets have been observed from BMImPF 6 . The most important observation of the present investigation is that the Si precursor, SiCl 4 , instead of undergoing hydrolysis, even in the presence of water, coexisted with ionic liquids, and elemental Si has been successfully electrodeposited.

Simultaneous voltammetric determination of prednisone and prednisolone in human body fluids.

PubMed

Goyal, Rajendra N; Bishnoi, Sunita

2009-08-15

A sensitive, rapid and reliable electrochemical method based on voltammetry at single wall carbon nanotube (SWNT) modified edge plane pyrolytic graphite electrode (EPPGE) is proposed for the simultaneous determination of prednisolone and prednisone in human body fluids and pharmaceutical preparations. The electrochemical response of both the drugs was evaluated by osteryoung square wave voltammetry (OSWV) in phosphate buffer medium of pH 7.2. The modified electrode exhibited good electrocatalytic properties towards prednisone and prednisolone reduction with a peak potential of approximately -1230 and approximately -1332 mV respectively. The concentration versus peak current plots were linear for both the analytes in the range 0.01-100 microM and the detection limit (3 sigma/slope) observed for prednisone and prednisolone were 0.45 x 10(-8), 0.90 x 10(-8)M, respectively. The results of the quantitative estimation of prednisone and prednisolone in biological fluids were also compared with HPLC and the results were in good agreement.

Monochromatic X-ray sources based on a mechanism of real and virtual photon diffraction in crystals

NASA Astrophysics Data System (ADS)

Wagner, A. R.; Kuznetsov, S. I.; Potylitsyn, A. P.; Razin, S. V.; Uglov, S. R.; Zabaev, V. N.

2008-09-01

A source of monochromatic X-ray radiation is wanted in industry, science, medicine and so on. Many ways of making such a source are known. The present work describes two mechanisms for the creation of a monochromatic X-ray beam, which are parametric X-ray radiation (PXR) and bremsstrahlung diffraction (DBS). Both the experiments were carried out using an electron beam at a microtron. During the first experiment, the DBS process was investigated as a scattering of the Bremsstrahlung (BS) beam on the crystallographic surfaces of tungsten and pyrolytic graphite crystals. The second experiment consisted in the registration of the PXR and DBS yield during the passage of the electrons through the same crystals as in the first experiment. The spectral and orientation radiation characteristics and simulation results obtained for the DBS and PXR processes are presented. It is shown that the usage of mosaic crystalline targets is rather useful in order to obtain a monochromatic X-ray source based on bremsstrahlung diffraction from moderately relativistic electrons.

Study of Drug Metabolism by Xanthine Oxidase

PubMed Central

Zhao, Jing; He, Xiaolin; Yang, Nana; Sun, Lizhou; Li, Genxi

2012-01-01

In this work, we report the studies of drug metabolism by xanthine oxidase (XOD) with electrochemical techniques. Firstly, a pair of stable, well-defined and quasi-reversible oxidation/reduction peaks is obtained with the formal potential at −413.1 mV (vs. SCE) after embedding XOD in salmon sperm DNA membrane on the surface of pyrolytic graphite electrode. Then, a new steady peak can be observed at −730 mV (vs. SCE) upon the addition of 6-mercaptopurine (6-MP) to the electrochemical system, indicating the metabolism of 6-MP by XOD. Furthermore, the chronoamperometric response shows that the current of the catalytic peak located at −730 mV increases with addition of 6-MP in a concentration-dependent manner, and the increase of the chronoamperometric current can be inhibited by an XOD inhibitor, quercetin. Therefore, our results prove that XOD/DNA modified electrode can be efficiently used to study the metabolism of 6-MP, which may provide a convenient approach for in vitro studies on enzyme-catalyzed drug metabolism. PMID:22606015

Substrate Selection for Fundamental Studies of Electrocatalysts and Photoelectrodes: Inert Potential Windows in Acidic, Neutral, and Basic Electrolyte

PubMed Central

Gorlin, Yelena; Jaramillo, Thomas F.

2014-01-01

The selection of an appropriate substrate is an important initial step for many studies of electrochemically active materials. In order to help researchers with the substrate selection process, we employ a consistent experimental methodology to evaluate the electrochemical reactivity and stability of seven potential substrate materials for electrocatalyst and photoelectrode evaluation. Using cyclic voltammetry with a progressively increased scan range, we characterize three transparent conducting oxides (indium tin oxide, fluorine-doped tin oxide, and aluminum-doped zinc oxide) and four opaque conductors (gold, stainless steel 304, glassy carbon, and highly oriented pyrolytic graphite) in three different electrolytes (sulfuric acid, sodium acetate, and sodium hydroxide). We determine the inert potential window for each substrate/electrolyte combination and make recommendations about which materials may be most suitable for application under different experimental conditions. Furthermore, the testing methodology provides a framework for other researchers to evaluate and report the baseline activity of other substrates of interest to the broader community. PMID:25357131

Enzyme electrokinetics: hydrogen evolution and oxidation by Allochromatium vinosum [NiFe]-hydrogenase.

PubMed

Léger, Christophe; Jones, Anne K; Roseboom, Winfried; Albracht, Simon P J; Armstrong, Fraser A

2002-12-31

The mechanism of catalytic hydrogen evolution and oxidation by Allochromatium vinosum [NiFe]-hydrogenase has been studied by protein film voltammetry (PFV) with the enzyme adsorbed at a pyrolytic graphite edge electrode. By analyzing the entire shapes of catalytic voltammograms, the energetics of the catalytic cycles (reduction potentials and acidity constants of the active states), including the detailed profiles of activity against pH and the sequences of proton and electron transfers, have been determined, and these are discussed with respect to the mechanism. PFV, which probes rates as a continuous function of the electrochemical potential (i.e., in the "potential domain"), is proven to be an invaluable tool for determining the redox properties of an active site in the presence of its substrate, at room temperature, and during turnover. This is especially relevant in the case of the active states of hydrogenase, since one of its substrates (the proton) is always present at significant levels in the titration medium at physiological pH values.

Size-dependent electrocatalytic activity of gold nanoparticles on HOPG and highly boron-doped diamond surfaces.

PubMed

Brülle, Tine; Ju, Wenbo; Niedermayr, Philipp; Denisenko, Andrej; Paschos, Odysseas; Schneider, Oliver; Stimming, Ulrich

2011-12-06

Gold nanoparticles were prepared by electrochemical deposition on highly oriented pyrolytic graphite (HOPG) and boron-doped, epitaxial 100-oriented diamond layers. Using a potentiostatic double pulse technique, the average particle size was varied in the range from 5 nm to 30 nm in the case of HOPG as a support and between < 1 nm and 15 nm on diamond surfaces, while keeping the particle density constant. The distribution of particle sizes was very narrow, with standard deviations of around 20% on HOPG and around 30% on diamond. The electrocatalytic activity towards hydrogen evolution and oxygen reduction of these carbon supported gold nanoparticles in dependence of the particle sizes was investigated using cyclic voltammetry. For oxygen reduction the current density normalized to the gold surface (specific current density) increased for decreasing particle size. In contrast, the specific current density of hydrogen evolution showed no dependence on particle size. For both reactions, no effect of the different carbon supports on electrocatalytic activity was observed.

Absorber for wakefield interference management at the entrance of the wiggler of a free electron laser

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

Marchlik, Matthew; Biallas, George Herman

A method for managing the broad band microwave and TeraHertz (THz) radiation in a free electron laser (FEL) having a wiggler producing power in the electromagnetic spectrum. The method includes placement of broadband microwave and TeraHertz (THz) radiation absorbers on the upstream end of the wiggler. The absorbers dampen the bounced back, broad band microwave and THz radiation returning from the surfaces outside the nose of the cookie-cutter and thus preventing broadening of the electron beam pulse's narrow longitudinal energy distribution. Broadening diminishes the ultimate laser power from the wiggler. The broadband microwave and THz radiation absorbers are placed onmore » either side of the slot in the cookie-cutter that shapes the wake field wave of the electron pulse to the slot shape of the wiggler chamber aperture. The broad band microwave and THz radiation absorber is preferably a non-porous pyrolytic grade of graphite with small grain size.« less

Effect of thermal behavior of β-lactoglobulin on the oxidative stability of menhaden oil-in-water emulsions.

PubMed

Phoon, Pui Yeu; Narsimhan, Ganesan; San Martin-Gonzalez, Maria Fernanda

2013-02-27

This study reports how emulsion oxidative stability was affected by the interfacial structure of β-lactoglobulin due to different heat treatments. Four percent (v/v) menhaden oil-in-water emulsions, stabilized by 1% (w/v) β-lactoglobulin at pH 7, were prepared by homogenization under different thermal conditions. Oxidative stability was monitored by the ferric thiocyanate peroxide value assay. Higher oxidative stability was attained by β-lactoglobulin in the molten globule state than in the native or denatured state. From atomic force microscopy of β-lactoglobulin adsorbed onto highly ordered pyrolytic graphite in buffer, native β-lactoglobulin formed a relatively smooth interfacial layer of 1.2 GPa in Young's modulus, whereas additional aggregates of similar stiffness were found when β-lactoglobulin was preheated to the molten globule state. For denatured β-lactoglobulin, although aggregates were also observed, they were larger and softer (Young's modulus = 0.45 GPa), suggesting increased porosity and thus an offset in the advantage of increased layer coverage on oxidative stability.

Fabrication of bi-layer graphene and theoretical simulation for its possible application in thin film solar cell.

PubMed

Behura, Sanjay K; Mahala, Pramila; Nayak, Sasmita; Yang, Qiaoqin; Mukhopadhyay, Indrajit; Janil, Omkar

2014-04-01

High quality graphene film is fabricated using mechanical exfoliation of highly-oriented pyrolytic graphite. The graphene films on glass substrates are characterized using field-emission scanning electron microscopy, atomic force microscopy, Raman spectroscopy, UV-vis spectroscopy and Fourier transform infrared spectroscopy. A very high intensity ratio of 2D to G-band (to approximately 1.67) and narrow 2D-band full-width at half maximum (to approximately 40 cm(-1)) correspond to the bi-layer graphene formation. The bi-layer graphene/p-GaN/n-InGaN/n-GaN/GaN/sAl2O3 system is studied theoretically using TCAD Silvaco software, in which the properties of exfoliated bi-layer graphene are used as transparent and conductive film, and the device exhibits an efficiency of 15.24% compared to 13.63% for ITO/p-GaN/n-InGaN/n-GaN/GaN/Al2O3 system.

Production of sp3 hybridization by swift heavy ion irradiation of HOPG

NASA Astrophysics Data System (ADS)

Zeng, J.; Zhai, P. F.; Liu, J.; Yao, H. J.; Duan, J. L.; Hou, M. D.; Sun, Y. M.; Li, G. P.

2013-07-01

Highly oriented pyrolytic graphite (HOPG) samples were irradiated by swift heavy ions (86Kr, 209Bi and 238U) with the fluence of 1011-1013 ions/cm2 at room temperature. The production of sp3 hybridization by the irradiation process has been confirmed directly by X-ray photoelectron spectroscopy (XPS). In this work, both irradiated and pristine HOPG samples were investigated by XPS and Raman spectroscopy. The existence of sp3 component is confirmed on the surface of the irradiated HOPG samples. XPS result shows that the acreage ratio Isp3/Isp2 increases with the ion fluence and saturates at a higher value of irradiation. It is found that the amount of hybridization (Isp3/Isp2) strongly depends on the electronic energy loss in the sample. Raman spectra of the irradiated samples show the increasing of acreage ratio ID/IG with the ion fluence, which indicates the change of the atomic structure and the phase transition from sp2 to sp3.

Interfacial assembly structures and nanotribological properties of saccharic acids.

PubMed

Shi, Hongyu; Liu, Yuhong; Zeng, Qingdao; Yang, Yanlian; Wang, Chen; Lu, Xinchun

2017-01-04

Saccharides have been recognized as potential bio-lubricants because of their good hydration ability. However, the interfacial structures of saccharides and their derivatives are rarely studied and the molecular details of interaction mechanisms have not been well understood. In this paper, the supramolecular assembly structures of saccharic acids (including galactaric acid and lactobionic acid), mediated by hydrogen bonds O-HN and O-HO, were successfully constructed on a highly oriented pyrolytic graphite (HOPG) surface by introducing pyridine modulators and were explicitly revealed by using scanning tunneling microscopy (STM). Furthermore, friction forces were measured in the saccharic acid/pyridine co-assembled system by atomic force microscopy (AFM), revealing a larger value than a pristine saccharic acid system, which could be attributed to the stronger tip-assembled molecule interactions that lead to the higher potential energy barrier needed to overcome. The effort on saccharide-related supramolecular self-assembly and nanotribological behavior could provide a novel and promising pathway to explore the interaction mechanisms underlying friction and reveal the structure-property relationship at the molecular level.

A scanning tunneling microscope for a dilution refrigerator.

PubMed

Marz, M; Goll, G; Löhneysen, H v

2010-04-01

We present the main features of a home-built scanning tunneling microscope that has been attached to the mixing chamber of a dilution refrigerator. It allows scanning tunneling microscopy and spectroscopy measurements down to the base temperature of the cryostat, T approximately 30 mK, and in applied magnetic fields up to 13 T. The topography of both highly ordered pyrolytic graphite and the dichalcogenide superconductor NbSe(2) has been imaged with atomic resolution down to T approximately 50 mK as determined from a resistance thermometer adjacent to the sample. As a test for a successful operation in magnetic fields, the flux-line lattice of superconducting NbSe(2) in low magnetic fields has been studied. The lattice constant of the Abrikosov lattice shows the expected field dependence proportional to 1/square root of B and measurements in the scanning tunneling spectroscopy mode clearly show the superconductive density of states with Andreev bound states in the vortex core.

Poly(ethylene oxide) surfactant polymers.

PubMed

Vacheethasanee, Katanchalee; Wang, Shuwu; Qiu, Yongxing; Marchant, Roger E

2004-01-01

We report on a series of structurally well-defined surfactant polymers that undergo surface-induced self-assembly on hydrophobic biomaterial surfaces. The surfactant polymers consist of a poly(vinyl amine) backbone with poly(ethylene oxide) and hexanal pendant groups. The poly(vinyl amine) (PVAm) was synthesized by hydrolysis of poly(N-vinyl formamide) following free radical polymerization of N-vinyl formamide. Hexanal and aldehyde-terminated poly(ethylene oxide) (PEO) were simultaneously attached to PVAm via reductive amination. Surfactant polymers with different PEO:hexanal ratios and hydrophilic/hydrophobic balances were prepared, and characterized by FT-IR, 1H-NMR and XPS spectroscopies. Surface active properties at the air/water interface were determined by surface tension measurements. Surface activity at a solid surface/water interface was demonstrated by atomic force microscopy, showing epitaxially molecular alignment for surfactant polymers adsorbed on highly oriented pyrolytic graphite. The surfactant polymers described in this report can be adapted for simple non-covalent surface modification of biomaterials and hydrophobic surfaces to provide highly hydrated interfaces.

Cluster formation in laser-induced ablation and evaporation of solids observed by laser ionization time-of-flight mass spectrometry and scanning tunneling microscopy

NASA Astrophysics Data System (ADS)

Tench, R. J.; Balooch, M.; Bernardez, L.; Allen, Mike J.; Siekhaus, W. J.; Olander, D. R.; Wang, W.

1990-04-01

Laser ionization time-of-flight mass analysis (LIMA) used pulses (5ns) of a frequency-quadrupled Nd-YAG laser (266 nm) focused onto spots of 4 to 100 microns diameter to ablate material, and a reflectron time of flight tube to mass-analyze the plume. The observed mass spectra for Si, Pt, SiC, and UO 2 varied in the distribution of ablation products among atoms, molecules and clusters, depending on laser power density and target material. Cleaved surfaces of highly oriented pyrolytic graphite (HOPG) positioned at room temperature either 10 cm away from materials ablated at 10(exp -5) Torr by 1 to 3 excimer laser (308 nm) pulses of 20 ns duration or 1 m away from materials vaporized at 10(exp -8) Torr by 10 Nd-Glass laser pulses of 1 ms duration were analyzed by Scanning Tunneling Microscopy (STM) in air with angstrom resolution. Clusters up to 30 A in diameter were observed.

Substrate Selection for Fundamental Studies of Electrocatalysts and Photoelectrodes: Inert Potential Windows in Acidic, Neutral, and Basic Electrolyte

DOE PAGES

Benck, Jesse D.; Pinaud, Blaise A.; Gorlin, Yelena; ...

2014-10-30

The selection of an appropriate substrate is an important initial step for many studies of electrochemically active materials. In order to help researchers with the substrate selection process, we employ a consistent experimental methodology to evaluate the electrochemical reactivity and stability of seven potential substrate materials for electrocatalyst and photoelectrode evaluation. Using cyclic voltammetry with a progressively increased scan range, we characterize three transparent conducting oxides (indium tin oxide, fluorine-doped tin oxide, and aluminum-doped zinc oxide) and four opaque conductors (gold, stainless steel 304, glassy carbon, and highly oriented pyrolytic graphite) in three different electrolytes (sulfuric acid, sodium acetate, andmore » sodium hydroxide). Here, we determine the inert potential window for each substrate/electrolyte combination and make recommendations about which materials may be most suitable for application under different experimental conditions. Furthermore, the testing methodology provides a framework for other researchers to evaluate and report the baseline activity of other substrates of interest to the broader community.« less

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

NASA Astrophysics Data System (ADS)

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

2014-10-01

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

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

PubMed

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

2014-10-28

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

Bent crystal spectrometer for both frequency and wavenumber resolved x-ray scattering at a seeded free-electron laser.

PubMed

Zastrau, Ulf; Fletcher, Luke B; Förster, Eckhart; Galtier, Eric Ch; Gamboa, Eliseo; Glenzer, Siegfried H; Heimann, Philipp; Marschner, Heike; Nagler, Bob; Schropp, Andreas; Wehrhan, Ortrud; Lee, Hae Ja

2014-09-01

We present a cylindrically curved GaAs x-ray spectrometer with energy resolution ΔE/E = 1.1 × 10(-4) and wave-number resolution of Δk/k = 3 × 10(-3), allowing plasmon scattering at the resolution limits of the Linac Coherent Light Source (LCLS) x-ray free-electron laser. It spans scattering wavenumbers of 3.6 to 5.2/Å in 100 separate bins, with only 0.34% wavenumber blurring. The dispersion of 0.418 eV/13.5 μm agrees with predictions within 1.3%. The reflection homogeneity over the entire wavenumber range was measured and used to normalize the amplitude of scattering spectra. The proposed spectrometer is superior to a mosaic highly annealed pyrolytic graphite spectrometer when the energy resolution needs to be comparable to the LCLS seeded bandwidth of 1 eV and a significant range of wavenumbers must be covered in one exposure.

High translational energy release in H2 (D2) associative desorption from H (D) chemisorbed on C(0001).

PubMed

Baouche, S; Gamborg, G; Petrunin, V V; Luntz, A C; Baurichter, A; Hornekaer, L

2006-08-28

Highly energetic translational energy distributions are reported for hydrogen and deuterium molecules desorbing associatively from the atomic chemisorption states on highly oriented pyrolytic graphite (HOPG). Laser assisted associative desorption is used to measure the time of flight of molecules desorbing from a hydrogen (deuterium) saturated HOPG surface produced by atomic exposure from a thermal atom source at around 2100 K. The translational energy distributions normal to the surface are very broad, from approximately 0.5 to approximately 3 eV, with a peak at approximately 1.3 eV. The highest translational energy measured is close to the theoretically predicted barrier height. The angular distribution of the desorbing molecules is sharply peaked along the surface normal and is consistent with thermal broadening contributing to energy release parallel to the surface. All results are in qualitative agreement with recent density functional theory calculations suggesting a lowest energy para-type dimer recombination path.

Self-assembly of (perfluoroalkyl)alkanes on a substrate surface from solutions in supercritical carbon dioxide.

PubMed

Gallyamov, Marat O; Mourran, Ahmed; Tartsch, Bernd; Vinokur, Rostislav A; Nikitin, Lev N; Khokhlov, Alexei R; Schaumburg, Kjeld; Möller, Martin

2006-06-14

Toroidal self-assembled structures of perfluorododecylnonadecane and perfluorotetradecyloctadecane have been deposited on mica and highly oriented pyrolytic graphite surfaces by exposure of the substrates to solutions of the (pefluoroalkyl)alkanes in supercritical carbon dioxide. Scanning force microscopy (SFM) images have displayed a high degree of regularity of these self-assembled nanoobjects regarding size, shape, and packing in a monolayer. Analysis of SFM images allowed us to estimate that each toroidal domain has an outer diameter of about 50 nm and consists of several thousands of molecules. We propose a simple model explaining the clustering of the molecules to objects with a finite size. The model based on the close-packing principles predicts formation of toroids, whose size is determined by the molecular geometry. Here, we consider the amphiphilic nature of the (perfluoroalkyl)alkane molecules in combination with incommensurable packing parameters of the alkyl- and the perfluoralkyl-segments to be a key factor for such a self-assembly.

Waste-to-Energy Systems

DTIC Science & Technology

2009-04-01

at hospitals, at schools,” or wherever there are people creating masses of trash.5 Pyrolytic Gasification Pyrolytic gasification is not a new...prevalent with both. Gasification is . . . the chemical reaction and molecular breakdown or degradation of materials. The first pyrolytic gasification...dealing with about 2 tons of mixed solid waste per day, will destroy wood, paper card, food, plastics, and sanitary, clinical, and oil waste and

Time dependent wettability of graphite upon ambient exposure: The role of water adsorption

NASA Astrophysics Data System (ADS)

Amadei, Carlo A.; Lai, Chia-Yun; Heskes, Daan; Chiesa, Matteo

2014-08-01

We report the temporal evolution of the wettability of highly ordered pyrolytic graphite (HOPG) exposed to environmental conditions. Macroscopic wettability is investigated by static and dynamic contact angles (SCA and DCA) obtaining values comparable to the ones presented in the literature. SCA increases from ˜68° to ˜90° during the first hour of exposure after cleaving, whereas DCA is characterized by longer-scale (24 h) time evolution. We interpret these results in light of Fourier transform infrared spectroscopy, which indicates that the evolution of the HOPG wettability is due to adsorption of molecules from the surrounding atmosphere. This hypothesis is further confirmed by nanoscopic observations obtained by atomic force microscope (AFM)-based force spectroscopy, which monitor the evolution of surface properties with a spatial resolution superior to macroscopic experiments. Moreover, we observe that the results of macro- and nanoscale measurements evolve in similar fashion with time and we propose a quantitative correlation between SCA and AFM measurements. Our results suggest that the cause of the transition in the wettability of HOPG is due to the adsorption of hydrocarbon contaminations and water molecules from the environment. This is corroborated by annealing the HOPG is vacuum conditions at 150°, allowing the desorption of molecules on the surface, and thus re-establishing the initial macro and nano surface properties. Our findings can be used in the interpretation of the wettability of more complicated systems derived from HOPG (i.e., graphene).

Voltammetric studies of Azathioprine on the surface of graphite electrode modified with graphene nanosheets decorated with Ag nanoparticles.

PubMed

Asadian, Elham; Iraji Zad, Azam; Shahrokhian, Saeed

2016-01-01

By using graphene nanosheets decorated with Ag nanoparticles (AgNPs-G) as an effective approach for the surface modification of pyrolytic graphite electrode (PGE), a sensing platform was fabricated for the sensitive voltammetric determination of Azathioprine (Aza). The prepared AgNPs-G nanosheets were characterized using transmission electron microscopy (TEM), X-ray diffraction (XRD), UV-vis and Raman spectroscopy techniques. The electrochemical behavior of Aza was investigated by means of cyclic voltammetry. Comparing to the bare PGE, a remarkable enhancement was observed in the response characteristics of Aza on the surface of the modified electrode (AgNPs-G/PGE) as well as a noticeable decrease in its reduction overpotential. These results can be attributed to the incredible enlargement in the microscopic surface area of the electrode due to the presence of graphene nanosheets together with strong adsorption of Aza on its surface. The effect of experimental parameters such as accumulation time, the amount of modifier suspension and pH of the supporting electrolyte were also optimized toward obtaining the maximum sensitivity. Under the optimum conditions, the calibration curve studies demonstrated that the peak current increased linearly with Aza concentrations in the range of 7 × 10(-7) to 1 × 10(-4)mol L(-1) with the detection limit of 68 nM. Further experiments revealed that the modified electrode can be successfully applied for the accurate determination of Aza in pharmaceutical preparations. Copyright © 2015 Elsevier B.V. All rights reserved.

Time dependent wettability of graphite upon ambient exposure: The role of water adsorption

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

Amadei, Carlo A.; Lai, Chia-Yun; Heskes, Daan

We report the temporal evolution of the wettability of highly ordered pyrolytic graphite (HOPG) exposed to environmental conditions. Macroscopic wettability is investigated by static and dynamic contact angles (SCA and DCA) obtaining values comparable to the ones presented in the literature. SCA increases from ∼68° to ∼90° during the first hour of exposure after cleaving, whereas DCA is characterized by longer-scale (24 h) time evolution. We interpret these results in light of Fourier transform infrared spectroscopy, which indicates that the evolution of the HOPG wettability is due to adsorption of molecules from the surrounding atmosphere. This hypothesis is further confirmedmore » by nanoscopic observations obtained by atomic force microscope (AFM)-based force spectroscopy, which monitor the evolution of surface properties with a spatial resolution superior to macroscopic experiments. Moreover, we observe that the results of macro- and nanoscale measurements evolve in similar fashion with time and we propose a quantitative correlation between SCA and AFM measurements. Our results suggest that the cause of the transition in the wettability of HOPG is due to the adsorption of hydrocarbon contaminations and water molecules from the environment. This is corroborated by annealing the HOPG is vacuum conditions at 150°, allowing the desorption of molecules on the surface, and thus re-establishing the initial macro and nano surface properties. Our findings can be used in the interpretation of the wettability of more complicated systems derived from HOPG (i.e., graphene)« less

Detailed line shape analysis of the C KVV Auger peak of two carbon allotropes measured using a time of flight positron annihilation induced Auger electron spectrometer

NASA Astrophysics Data System (ADS)

Fairchild, A. J.; Chirayath, V. A.; Chrysler, M. D.; Gladen, R. W.; Imam, S. K.; Koymen, A. R.; Weiss, A. H.

We report a detailed line shape analysis of the positron induced C KVV Auger line shape from highly oriented pyrolytic graphite (HOPG) and a single layer of graphene grown on polycrystalline Cu. A model consisting of the self-fold of the one-electron density of states including terms for hole-hole interactions, charge screening effects, and intrinsic loss mechanisms is compared to experimental C KVV line shapes measured using a positron induced Auger electron spectrometer (PAES). In traditional Auger spectroscopies which use an electron or photon to initiate the Auger process, extracting the relatively small Auger signal from the large secondary background can be quite difficult. Using a very low energy positron beam to create the core hole through an anti-matter matter annihilation entirely eliminates this background. Additionally, PAES has sensitivity to the top most atomic layer since the positron becomes trapped in an image potential well at the surface before annihilation. Therefore, the PAES signal from a single layer of graphene on polycrystalline Cu is primarily from the graphene overlayer with small contributions from the Cu substrate while the PAES signal from HOPG can be viewed as a single graphene layer with a graphite substrate. The influence of these two substrates on C KVV line shape is discussed. This work was supported by NSF Grant No. DMR 1508719 and DMR 1338130.

Graphite nanocomposites sensor for multiplex detection of antioxidants in food.

PubMed

Ng, Khan Loon; Tan, Guan Huat; Khor, Sook Mei

2017-12-15

Butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT), and tert-butylhydroquinone (TBHQ) are synthetic antioxidants used in the food industry. Herein, we describe the development of a novel graphite nanocomposite-based electrochemical sensor for the multiplex detection and measurement of BHA, BHT, and TBHQ levels in complex food samples using a linear sweep voltammetry technique. Moreover, our newly established analytical method exhibited good sensitivity, limit of detection, limit of quantitation, and selectivity. The accuracy and reliability of analytical results were challenged by method validation and comparison with the results of the liquid chromatography method, where a linear correlation of more than 0.99 was achieved. The addition of sodium dodecyl sulfate as supporting additive further enhanced the LSV response (anodic peak current, I pa ) of BHA and BHT by 2- and 20-times, respectively. Copyright © 2017 Elsevier Ltd. All rights reserved.

Dielectric properties of novel polyurethane-PZT-graphite foam composites

NASA Astrophysics Data System (ADS)

Tolvanen, Jarkko; Hannu, Jari; Nelo, Mikko; Juuti, Jari; Jantunen, Heli

2016-09-01

Flexible foam composite materials offer multiple benefits to future electronic applications as the rapid development of the electronics industry requires smaller, more efficient, and lighter materials to further develop foldable and wearable applications. The aims of this work were to examine the electrical properties of three- and four-phase novel foam composites in different conditions, find the optimal mixture for four-phase foam composites, and study the combined effects of lead zirconate titanate (PZT) and graphite fillers. The flexible and highly compressible foams were prepared in a room-temperature mixing process using polyurethane, PZT, and graphite components as well as their combinations, in which air acted as one phase. In three-phase foams the amount of PZT varied between 20 and 80 wt% and the amount of graphite, between 1 and 15 wt%. The four-phase foams were formed by adding 40 wt% of PZT while the amount of graphite ranged between 1 and 15 wt%. The presented results and materials could be utilized to develop new flexible and soft sensor applications by means of material technology.

RESEARCH ON PHYSICAL AND CHEMICAL PRINCIPLES AFFECTING HIGH TEMPERATURE MATERIALS FOR ROCKET NOZZLES. Quarterly Progress Report, April 1, 1963-June 30, 1963

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

Lowrie, R.

1963-10-31

The development and properties of refractory materials are described. Corrosion of zirconium carbide, niobium carbide, and niobium carbide-zirconium carbide systems by carbon dioxide and hydrochloric acid at 2250 deg C is reported. Corrosion of silver-tungsten alloys by carbon dioxide and oxygen at 2150 to 2440 deg K is summarized. Measurements of pyrolytic and ZTA graphite corrosion by carbon dioxide and oxygen at 2100 to 2800 deg K are shown. At 2300 deg C the rate of formation of methane from graphite and hydrogen is greatly reduced by the addition of helium, at constant hydrogen pressure. Up to 2000 deg Cmore » the effect of helium is small. The pyrolysis of methane on graphite at 2000 deg C is tabulated. Oxidation of tungsten to form WO/sub 2/ and WO/sub 3/ is reported. Vaporization of hafnium borides at 2297 to 2538 deg K is analyzed. The lattice parameters of ZrB/sub 2/ at of TiN/sub 0.6/ and TiN/sub 0.75/ are discussed. Powder metallurgical techniques are used to prepare TiB/sub 2/, ZrB/sub 2/, HfB/ sub 2/, NbB/sub 2/, a nd TaB/sub 2/ for detailed x-ray characterization. The electric conductivity of NbC-ZrC systems is reported. General descriptions are given of analytical techniques for free carbon in carbides and spectrographic methods for metallic impurities in carbides and borides. Preliminary roomtemperature measurements are reported of the elastic properties of polycrystalline ZrB/sub 2/. Titanium carbide is brazed to tungsten with a platinum-boron system. A largegrained polycrystalline specimen of ZrC is plastically deformed in creep at 2134 deg C. Metallographic and x-ray examinations of polycrystalline TiC specimens deformed in creep reveal an increasing development with deformation of subgrains having preferred orientation. (N.W.R.)« less

Nucleation, aggregative growth and detachment of metal nanoparticles during electrodeposition at electrode surfaces† †Electronic supplementary information (ESI) available: S1 Scharifker–Hills model, S2 tapping mode-atomic force microscopy (TM-AFM) image of AM grade HOPG, after exposure to a droplet of 50 mM KNO3, S3 distribution of induction times, S4 results of the modified Cottrell fits at different potentials, S5 FE-SEM images of HOPG after control tip breaking, S6 extended current–time trace. See DOI: 10.1039/c4sc02792b Click here for additional data file.

PubMed Central

Lazenby, Robert A.; Kirkman, Paul M.

2015-01-01

The nucleation and growth of metal nanoparticles (NPs) on surfaces is of considerable interest with regard to creating functional interfaces with myriad applications. Yet, key features of these processes remain elusive and are undergoing revision. Here, the mechanism of the electrodeposition of silver on basal plane highly oriented pyrolytic graphite (HOPG) is investigated as a model system at a wide range of length scales, spanning electrochemical measurements from the macroscale to the nanoscale using scanning electrochemical cell microscopy (SECCM), a pipette-based approach. The macroscale measurements show that the nucleation process cannot be modelled as either truly instantaneous or progressive, and that step edge sites of HOPG do not play a dominant role in nucleation events compared to the HOPG basal plane, as has been widely proposed. Moreover, nucleation numbers extracted from electrochemical analysis do not match those determined by atomic force microscopy (AFM). The high time and spatial resolution of the nanoscale pipette set-up reveals individual nucleation and growth events at the graphite basal surface that are resolved and analysed in detail. Based on these results, corroborated with complementary microscopy measurements, we propose that a nucleation-aggregative growth-detachment mechanism is an important feature of the electrodeposition of silver NPs on HOPG. These findings have major implications for NP electrodeposition and for understanding electrochemical processes at graphitic materials generally. PMID:29560200

Thermal and catalytic slow pyrolysis of Calophyllum inophyllum fruit shell.

PubMed

Alagu, R M; Sundaram, E Ganapathy; Natarajan, E

2015-10-01

Pyrolysis of Calophyllum inophyllum shell was performed in a fixed bed pyrolyser to produce pyrolytic oil. Both thermal (without catalysts) and catalytic pyrolysis process were conducted to investigate the effect of catalysts on pyrolysis yield and pyrolysis oil characteristics. The yield of pyrolytic oil through thermal pyrolysis was maximum (41% wt) at 425 °C for particle size of 1.18 mm and heating rate of 40 °C/min. In catalytic pyrolysis the pyrolytic oil yield was maximum (45% wt) with both zeolite and kaolin catalysts followed by Al2O3 catalyst (44% wt). The functional groups and chemical components present in the pyrolytic oil are identified by Fourier Transform Infrared Spectroscopy (FT-IR) and Gas Chromatography-Mass Spectrometry (GC-MS) techniques. This study found that C. inophyllum shell is a potential new green energy source and that the catalytic pyrolysis process using zeolite catalyst improves the calorific value and acidity of the pyrolytic oil. Copyright © 2015 Elsevier Ltd. All rights reserved.

A comparison of thermal behaviors of raw biomass, pyrolytic biochar and their blends with lignite.

PubMed

Liu, Zhengang; Balasubramanian, Rajasekhar

2013-10-01

In this study, thermal characteristics of raw biomass, corresponding pyrolytic biochars and their blends with lignite were investigated. The results showed that pyrolytic biochars had better fuel qualities than their parent biomass. In comparison to raw biomass, the combustion of the biochars shifted towards higher temperature and occurred at continuous temperature zones. The biochar addition in lignite increased the reactivities of the blends. Obvious interactions were observed between biomass/biochar and lignite and resulted in increased total burnout, shortened combustion time and increased maximum weight loss rate, indicating increased combustion efficiencies than that of lignite combustion alone. Regarding ash-related problems, the tendency to form slagging and fouling increased, when pyrolytic biochars were co-combusted with coal. This present study demonstrated that the pyrolytic biochars were more suitable than raw biomass to be co-combusted with lignite for energy generation in existing coal-fired power plants. Copyright © 2013 Elsevier Ltd. All rights reserved.

Cyclic voltammetry deposition of copper nanostructure on MWCNTs modified pencil graphite electrode: An ultra-sensitive hydrazine sensor.

PubMed

Heydari, Hamid; Gholivand, Mohammad B; Abdolmaleki, Abbas

2016-09-01

In this study, Copper (Cu) nanostructures (CuNS) were electrochemically deposited on a film of multiwall carbon nanotubes (MWCNTs) modified pencil graphite electrode (MWCNTs/PGE) by cyclic voltammetry method to fabricate a CuNS-MWCNTs composite sensor (CuNS-MWCNT/PGE) for hydrazine detection. Scanning electron microscopy (SEM) and Energy-dispersive X-ray spectroscopy (EDX) were used for the characterization of CuNS on the MWCNTs matrix. The composite of CuNS-MWCNTs was characterized with cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The preliminary studies showed that the proposed sensor have a synergistic electrocatalytic activity for the oxidation of hydrazine in phosphate buffer. The catalytic currents of square wave voltammetry had a linear correlation with the hydrazine concentration in the range of 0.1 to 800μM with a low detection limit of 70nM. Moreover, the amperometric oxidation current exhibited a linear correlation with hydrazine concentration in the concentration range of 50-800μM with the detection limit of 4.3μM. The proposed electrode was used for the determination of hydrazine in real samples and the results were promising. Empirical results also indicated that the sensor had good reproducibility, long-term stability, and the response of the sensor to hydrazine was free from interferences. Moreover, the proposed sensor benefits from simple preparation, low cost, outstanding sensitivity, selectivity, and reproducibility for hydrazine determination. Copyright © 2016. Published by Elsevier B.V.

Polycyclic aromatic hydrocarbons (PAHs) and volatile organic compounds (VOCs) mitigation in the pyrolysis process of waste tires using CO₂ as a reaction medium.

PubMed

Kwon, Eilhann E; Oh, Jeong-Ik; Kim, Ki-Hyun

2015-09-01

Our work reported the CO2-assisted mitigation of PAHs and VOCs in the thermo-chemical process (i.e., pyrolysis). To investigate the pyrolysis of used tires to recover energy and chemical products, the experiments were conducted using a laboratory-scale batch-type reactor. In particular, to examine the influence of the CO2 in pyrolysis of a tire, the pyrolytic products including C1-5-hydrocarbons (HCs), volatile organic carbons (VOCs), and polycyclic aromatic hydrocarbons (PAHs) were evaluated qualitatively by gas chromatography (GC) with mass spectroscopy (MS) as well as with a thermal conductivity detector (TCD). The mass balance of the pyrolytic products under various pyrolytic conditions was established on the basis of their weight fractions of the pyrolytic products. Our experimental work experimentally validated that the amount of gaseous pyrolytic products increased when using CO2 as a pyrolysis medium, while substantially altering the production of pyrolytic oil in absolute content (7.3-17.2%) and in relative composition (including PAHs and VOCs). Thus, the co-feeding of CO2 in the pyrolysis process can be considered an environmentally benign and energy efficient process. Copyright © 2015 Elsevier Ltd. All rights reserved.

Preparation of β-cyclodextrin entrapped graphite composite for sensitive detection of dopamine.

PubMed

Palanisamy, Selvakumar; Sakthinathan, S; Chen, Shen-Ming; Thirumalraj, Balamurugan; Wu, Tsung-Han; Lou, Bih-Show; Liu, Xiaoheng

2016-01-01

A simple dopamine (DA) electrochemical sensor was developed based on a screen-printed carbon electrode (SPCE) modified with β-cyclodextrin entrapped graphite (GR/β-CD) composite for the first time. The polar hydroxyl groups on the β-CD rims interact with polar groups of edges of GR sheets resulting into the high dispersion ability of GR in β-CD solution. The GR/β-CD modified electrode exhibited a higher electrochemical response to DA with a lower oxidation potential (0.224V) than that of bare/β-CD (0.38V) and GR (0.525V) modified SPCEs, revealing an excellent electro-oxidation behavior of GR/β-CD composite toward DA. Under optimum conditions, the fabricated sensor detects the DA in the linear concentration range from 0.1 to 58.5μM with a limit of detection of 0.011μM and the sensitivity of 1.27±0.02μAμM(-1)cm(-2). The fabricated sensor also exhibits the excellent repeatability, practicality, reproducibility, storage stability along with acceptable selectivity. Copyright © 2015 Elsevier Ltd. All rights reserved.

A Stretchable and Screen-Printed Electrochemical Sensor for Glucose Determination in Human Perspiration

PubMed Central

Abellán-Llobregat, A.; Jeerapan, I.; Bandodkar, A.; Vidal, L.; Canals, A.; Wang, J.; Morallón, E.

2017-01-01

Here we present two types of all-printable, highly stretchable, and inexpensive devices based on platinum (Pt)-decorated graphite for glucose determination in physiological fluids. Said devices are: a non-enzymatic sensor and an enzymatic biosensor, the latter showing promising results. Glucose has been quantified by measuring hydrogen peroxide (H2O2) reduction by chronoamperometry at -0.35 V (vs pseudo-Ag/AgCl) using glucose-oxidase immobilized on Pt-decorated graphite. The sensor performs well for the quantification of glucose in phosphate buffer solution (0.25 M PBS, pH 7.0), with a working range between 33 μM and 0.9 mM, high sensitivity and selectivity, and a low limit of detection (LOD). Thus it provides an alternative non-invasive and on-body quantification of glucose levels in human perspiration. This biosensor has been successfully applied on real human perspiration samples and results also show a significant correlation between glucose concentration in perspiration and glucose concentration in blood measured by a commercial glucose meter. PMID:28167366

A facile photoelectrochemical sensor for high sensitive ROS and AA detection based on graphitic carbon nitride nanosheets.

PubMed

Motaghed Mazhabi, Robabeh; Ge, Liqin; Jiang, Hui; Wang, Xuemei

2018-06-01

Photoactive material is one of the main challenges for fabrication of sensitive and selective photoelectrochemical (PEC) sensor. Herein, a facile PEC sensor is constructed using graphitic carbon nitride nanosheets (g-C 3 N 4 NSs) coated on the surface of ITO electrode, where electron donor properties of potassium ferrocyanide and ascorbic acid is utilized for the tracing of hydrogen peroxide (H 2 O 2 ), hypochlorite (ClO - ), and ascorbic acid (AA). Our designed PEC sensor exhibits a good linear range to H 2 O 2 concentrations from 12.5 to 875 µM in pH = 7.4 and 2.5-400 µM in pH = 10, while that for AA is in the range from 0.25 to 100 µM in pH = 7.4, and with the same pH for ClO - concentrations in the range from 0.5 to 19 × 10 -3 % (V/V) in a bleach sample. Owing to the good responses towards the traces of H 2 O 2 , AA, and ClO - , our designed system may be used as H 2 O 2, ClO - , and AA sensor for outdoor applications with high specificity, long-time stability and good reproducibility. Copyright © 2018 Elsevier B.V. All rights reserved.

Advanced Heat Exchangers for Dry Cooling Systems, Phase II

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

Fortini, Arthur J.; Horwath, Joseph

Dry cooling systems are an option for industrial and utility power plants that cannot obtain permits for cooling water or where cooling water is unavailable. Currently available dry cooling systems are more expensive and less efficient than wet cooling systems, so significant improvements in efficiency are needed to make them economically viable. Previous attempts at using foams as cooling fin materials for power generating systems have focused on high thermal conductivity graphite foams made via the Oak Ridge process. Because these materials have high flow restrictions and hence low permeability with respect to air flow, their internal volume and surfacemore » area were not effectively used. Consequently, they performed poorly and offered no advantage over aluminum fins. A foam with a more open structure would provide increased permeability, enable greater airflow through the bulk material, increase the rate of heat transfer, and enable the material to outperform traditional fin structures. In this project, Ultramet designed, fabricated, and tested low flow restriction, high-efficiency foam-based heat exchangers. Calculations based on existing thermal and hydraulic data for Ultramet’s high-performance open-cell foams indicated that 65-ppi (pores per linear inch) pyrolytic graphite foam with a relative density of 15 vol%, produced by chemical vapor infiltration (CVI), would have an effectiveness significantly greater than that of a state-of-the-art Hamon/Balcke-Durr aluminum fin system and greater than that of the POCO graphite foams previously tested for the DOE National Energy Technology Laboratory. Using the same chevron design, test setup, and run conditions as were used with the Hamon/Balcke-Durr fin system and the POCO foams, Ultramet tested graphite foams with air flow velocities of 0.07–3.2 m/sec and pressure drops of 0.03–9.7 inH2O. The best-performing graphite foam architectures had air velocities in excess of 2.5 m/sec when the pressure drop was 1 inH2O. Because a foam-based system is more efficient than a fin-based system, a smaller heat exchanger installation can be used, significantly reducing the installation cost. Furthermore, because the foam-based system is physically smaller with no increase in flow restriction, less electrical power is needed to run the fans to drive the air through the condenser. The result is a decrease in both the installation and operating costs, which in turn will decrease the overall life cycle cost of the system.« less

Pyrolysis of de-oiled seed cake of Jatropha Curcas and catalytic steam reforming of pyrolytic bio-oil to hydrogen.

PubMed

Renny, Andrew; Santhosh, Viswanathan; Somkuwar, Nitin; Gokak, D T; Sharma, Pankaj; Bhargava, Sanjay

2016-11-01

The aim of this work was to study the pyrolysis of de-oiled seed cake of Jatropha Curcas and catalytic steam reforming of pyrolytic bio-oil to hydrogen. As per literature, presence of heavy nitrogenous and oxygenated compounds leads to catalyst deactivation. Here, an attempt has been made to tune pyrolytic reactions to optimize the N and O content of the pyrolytic bio-oil. Bio-oil conversion and hydrogen yield decreased as reaction progressed, which attributes to temporary loss of catalytic activity by blockage of catalyst pores by carbon deposition. Further, retention of steam reforming activity after repetitive steam activation suggests long-term catalyst usage. Copyright © 2016 Elsevier Ltd. All rights reserved.

Halo current diagnostic system of experimental advanced superconducting tokamak

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

Chen, D. L.; Shen, B.; Sun, Y.

2015-10-15

The design, calibration, and installation of disruption halo current sensors for the Experimental Advanced Superconducting Tokamak are described in this article. All the sensors are Rogowski coils that surround conducting structures, and all the signals are analog integrated. Coils with two different cross-section sizes have been fabricated, and their mutual inductances are calibrated. Sensors have been installed to measure halo currents in several different parts of both the upper divertor (tungsten) and lower divertor (graphite) at several toroidal locations. Initial measurements from disruptions show that the halo current diagnostics are working well.

Mechanical Drawing of Gas Sensors on Paper

PubMed Central

Mirica, Katherine A.; Weis, Jonathan G.; Schnorr, Jan M.; Esser, Birgit

2012-01-01

This communication describes a simple solvent-free method for fabricating chemoresistive gas sensors on the surface of paper. The method involves mechanical abrasion of compressed powders of sensing materials on the fibers of cellulose. We illustrate this approach by depositing conductive layers of several forms of carbon (e.g., single-walled carbon nanotubes [SWCNTs], multi-walled carbon nanotubes, and graphite) on the surface of different papers (Figure 1, Figure S1). The resulting sensors based on SWCNTs are capable of detecting NH3 gas at concentrations as low as 0.5 part-per-million. PMID:23037938

Design and fabrication of a fixed-bed batch type pyrolysis reactor for pilot scale pyrolytic oil production in Bangladesh

NASA Astrophysics Data System (ADS)

Aziz, Mohammad Abdul; Al-khulaidi, Rami Ali; Rashid, MM; Islam, M. R.; Rashid, MAN

2017-03-01

In this research, a development and performance test of a fixed-bed batch type pyrolysis reactor for pilot scale pyrolysis oil production was successfully completed. The characteristics of the pyrolysis oil were compared to other experimental results. A solid horizontal condenser, a burner for furnace heating and a reactor shield were designed. Due to the pilot scale pyrolytic oil production encountered numerous problems during the plant’s operation. This fixed-bed batch type pyrolysis reactor method will demonstrate the energy saving concept of solid waste tire by creating energy stability. From this experiment, product yields (wt. %) for liquid or pyrolytic oil were 49%, char 38.3 % and pyrolytic gas 12.7% with an operation running time of 185 minutes.

Inventory Control.

ERIC Educational Resources Information Center

Byrum, David L., Ed.

1984-01-01

Presents three ideas to help hold costs down in purchasing and using science equipment. These include (1) use of pencils and other graphite rods as sensors in potentiometric titrations, (2) rubber bulb modification for pipetting, and (3) a heater for a glassware bath. (JM)

Surface modification of amine-functionalised graphite for preparation of cobalt hexacyanoferrate (CoHCF)-modified electrode: an amperometric sensor for determination of butylated hydroxyanisole (BHA).

PubMed

Prabakar, S J Richard; Narayanan, S Sriman

2006-12-01

A cobalt hexacyanoferrate (CoHCF)-modified graphite paraffin wax composite electrode was prepared by a new approach. An amine-functionalised graphite powder was used for the fabrication of the electrode. A functionalised graphite paraffin wax composite electrode was prepared and the surface of the electrode was modified with a thin film of CoHCF. Various parameters that influence the electrochemical behaviour of the modified electrode were studied by varying the background electrolytes, scan rates and pH. The modified electrode showed good electrocatalytic activity towards the oxidation of butylated hydroxyanisole (BHA) under optimal conditions and showed a linear response over the range from 7.9 x 10(-7) to 1.9 x 10(-4) M of BHA with a correlation coefficient of 0.9988. The limit of detection was 1.9 x 10(-7) M. Electrocatalytic oxidation of BHA was effective at the modified electrode at a significantly reduced potential and at a broader pH range. The utility of the modified electrode as an amperometric sensor for the determination of BHA in flow systems was evaluated by carrying out hydrodynamic and chronoamperometric experiments. The modified electrode showed very good stability and a longer shelf life. The modified electrode was applied for the determination of BHA in spiked samples of chewing gum and edible sunflower oil. The advantage of this method is the ease of electrode fabrication, good stability, longer shelf life, low cost and its diverse application for BHA determination.

Deformation sensor based on polymer-supported discontinuous graphene multi-layer coatings

NASA Astrophysics Data System (ADS)

Carotenuto, G.; Schiavo, L.; Romeo, V.; Nicolais, L.

2014-05-01

Graphene can be conveniently used in the modification of polymer surfaces. Graphene macromolecules are perfectly transparent to the visible light and electrically conductive, consequently these two properties can be simultaneously provided to polymeric substrates by surface coating with thin graphene layers. In addition, such coating process provides the substrates of: water-repellence, higher surface hardness, low-friction, self-lubrication, gas-barrier properties, and many other functionalities. Polyolefins have a non-polar nature and therefore graphene strongly sticks on their surface. Nano-crystalline graphite can be used as graphene precursor in some chemical processes (e.g., graphite oxide synthesis by the Hummer method), in addition it can be directly applied to the surface of a polyolefin substrate (e.g., polyethylene) to cover it by a thin graphene multilayer. In particular, the nano-crystalline graphite perfectly exfoliate under the application of a combination of shear and friction forces and the produced graphene single-layers perfectly spread and adhere on the polyethylene substrate surface. Such polymeric materials can be used as ITO (indium-tin oxide) substitute and in the fabrication of different electronic devices. Here the fabrication of transparent resistive deformation sensors based on low-density polyethylene films coated by graphene multilayers is described. Such devices are very sensible and show a high reversible and reproducible behavior.

Effects of Prior Aging at Elevated Temperature in Air and in Argon Environments on Creep Response of PMR-15 Neat Resin at 288 deg C

DTIC Science & Technology

2007-03-01

either inert gases or air to distinguish between the pyrolytic and oxidative degradation mechanisms. This exposure is commonly called “aging” of...and performance under use conditions. 4 This thesis explores the effects of both pyrolytic and thermal oxidative degradation on the mechanical...fatigue. A third assumption is that the mechanical properties of the pyrolytically aged samples will approximate the mechanical properties of the inner

Secondary-electron-emission losses in multistage depressed collectors and traveling-wave-tube efficiency improvements with carbon collector electrode surfaces

NASA Technical Reports Server (NTRS)

Ramins, P.; Ebihara, B. T.

1986-01-01

Secondary-electron-emission losses in multistage depressed collectors (MDC's) and their effects on overall traveling-wave-tube (TWT) efficiency were investigated. Two representative TWT's and several computer-modeled MDC's were used. The experimental techniques provide the measurement of both the TWT overall and the collector efficiencies. The TWT-MDC performance was optimized and measured over a wide range of operating conditions, with geometrically identical collectors, which utilized different electrode surface materials. Comparisons of the performance of copper electrodes to that of various forms of carbon, including pyrolytic and iisotropic graphites, were stressed. The results indicate that: (1) a significant improvement in the TWT overall efficiency was obtained in all cases by the use of carbon, rather than copper electrodes, and (2) that the extent of this efficiency enhancement depended on the characteristics of the TWT, the TWT operating point, the MDC design, and collector voltages. Ion textured graphite was found to be particularly effective in minimizing the secondary-electron-emission losses. Experimental and analytical results, however, indicate that it is at least as important to provide a maximum amount of electrostatic suppression of secondary electrons by proper MDC design. Such suppression, which is obtained by ensuring that a substantial suppressing electric field exists over the regions of the electrodes where most of the current is incident, was found to be very effective. Experimental results indicate that, with proper MDC design and the use of electrode surfaces with low secondary-electron yield, degradation of the collector efficiency can be limited to a few percent.

Salt melt synthesis of curved nitrogen-doped carbon nanostructures: ORR kinetics boost

NASA Astrophysics Data System (ADS)

Rybarczyk, Maria K.; Gontarek, Emilia; Lieder, Marek; Titirici, Maria-Magdalena

2018-03-01

Implementing metal-free electrocatalysts for the oxygen reduction reaction (ORR) and revealing crucial chemical or topographical parameters driving their activity are vital for the development of power cells. The carbon-based catalysts are very often synthesized through carbonization of biopolymers, in particular, those one containing nitrogen groups such as chitosan. Unfortunately, the resulting carbonaceous materials usually lack specific porosity and exhibit low catalytic activity. Here, we demonstrate that pyrolysis of chitosan in a ZnCl2 melt assisted by the presence of LiCl results not only in a highly porous activated carbon material with a specific surface area of 1317.97 m2/g and the total nitrogen content of 6.5%, but also induces unexpected curvature in the grown graphitic layers. This is the first work that shows curved graphene layers obtained from a biopolymer precursor by its pyrolytic decomposition in the melted salt media. On the other hand, a carbonaceous material obtained from chitosan but without the salts has very low specific surface area of 7.8 m2/g, possesses no specific structural features, and contains 4.7% of nitrogen. The electrochemical studies show, that the former material is highly active towards four-electron pathway of the ORR in terms of an onset potential (0.89 V vs RHE) and the turnover frequency (TOFmax = 0.095 e site-1 s-1). We attribute this high catalytic performance to the presence of the pyridinic and pyrrolic sites in the structure. The ORR kinetics is probably further promoted by curvature in the graphitic layers.

Thermometry of the system “heat-resistant sample - incident plasma stream”

NASA Astrophysics Data System (ADS)

Sargsyan, M. A.; Chinnov, V. F.; Kavyrshin, D. I.; Gadzhiev, M. Kh; Khromov, M. A.; Chistolinov, A. V.; Senchenko, V. N.

2017-11-01

To study the interacting system “heat-resistant sample - an incident plasma stream” a setup of synchronized measurement equipment was developed and tested that recorded the main parameters of such interaction. Heat resistance tests were carried out on the samples of MPG-6 grade isotropic graphite, and samples of pyrolytic graphite that were subjected to a long (60 … 100 s) exposure to nitrogen, argon and air plasma streams at atmospheric pressure. As plasma generators a series of plasma torches with a vortex stabilization of the stream and an expanding anode channels was used. The temperature and composition of the plasma in the jet and near the sample were determined using two AvaSpec2048 and AvaSpec3648 scanning optical spectrometers and the MS5402i spectrograph with the Andor matrix at its outlet. The surface temperature of the sample was determined in real time using three independent ways: two pyrometric systems - a high-speed micro-pyrometer FMP1001 and a two-position visualization of the heated sample by high-speed Motion Pro X3 and VS-FAST cameras, and the spectral analysis of the wide-range thermal radiation of the samples. The main method for determining the rate of material loss during the action of a plasma jet on it was to analyze a two-position synchronous visualization of the “jet-sample” system. When a crater was formed on the surface of the sample under the “dagger” effect of a plasma jet, a video recording system of the crater zone was used, backlit using the “laser knife” method.

Auto-assembly of nanometer thick, water soluble layers of plasmid DNA complexed with diamines and basic amino acids on graphite: Greatest DNA protection is obtained with arginine.

PubMed

Khalil, T T; Boulanouar, O; Heintz, O; Fromm, M

2017-02-01

We have investigated the ability of diamines as well as basic amino acids to condense DNA onto highly ordered pyrolytic graphite with minimum damage after re-dissolution in water. Based on a bibliographic survey we briefly summarize DNA binding properties with diamines as compared to basic amino acids. Thus, solutions of DNA complexed with these linkers were drop-cast in order to deposit ultra-thin layers on the surface of HOPG in the absence or presence of Tris buffer. Atomic Force Microscopy analyses showed that, at a fixed ligand-DNA mixing ratio of 16, the mean thickness of the layers can be statistically predicted to lie in the range 0-50nm with a maximum standard deviation ±6nm, using a simple linear law depending on the DNA concentration. The morphology of the layers appears to be ligand-dependent. While the layers containing diamines present holes, those formed in the presence of basic amino acids, except for lysine, are much more compact and dense. X-ray Photoelectron Spectroscopy measurements provide compositional information indicating that, compared to the maximum number of DNA sites to which the ligands may bind, the basic amino acids Arg and His are present in large excess. Conservation of the supercoiled topology of the DNA plasmids was studied after recovery of the complex layers in water. Remarkably, arginine has the best protection capabilities whether Tris was present or not in the initial solution. Copyright © 2016 Elsevier B.V. All rights reserved.

Influence of alkyl chain length and anion species on ionic liquid structure at the graphite interface as a function of applied potential

NASA Astrophysics Data System (ADS)

Li, Hua; Wood, Ross J.; Endres, Frank; Atkin, Rob

2014-07-01

Atomic force microscopy (AFM) force measurements elucidate the effect of cation alkyl chain length and the anion species on ionic liquid (IL) interfacial structure at highly ordered pyrolytic graphite (HOPG) surfaces as a function of potential. Three ILs are examined: 1-hexyl-3-methylimidazolium tris(pentafluoroethyl)trifluorophosphate ([HMIM] FAP), 1-ethyl-3-methylimidazolium tris(pentafluoroethyl)trifluorophosphate ([EMIM] FAP), and 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide ([EMIM] TFSA). The step-wise force-distance profiles indicate the ILs adopt a multilayered morphology near the surface. When the surface is biased positively or negatively versus Pt quasireference electrode, both the number of steps, and the force required to rupture each step increase, indicating stronger interfacial structure. At all potentials, push-through forces for [HMIM] FAP are the highest, because the long alkyl chain results in strong cohesive interactions between cations, leading to well-formed layers that resist the AFM tip. The most layers are observed for [EMIM] FAP, because the C2 chains are relatively rigid and the dimensions of the cation and anion are similar, facilitating neat packing. [EMIM] TFSA has the smallest push-through forces and fewest layers, and thus the weakest interfacial structure. Surface-tip attractive forces are measured for all ILs. At the same potential, the attractions are the strongest for [EMIM] TFSA and the weakest for [HMIM] FAP because the interfacial layers are better formed for the longer alkyl chain cation. This means interfacial forces are stronger, which masks the weak attractive forces.

Gas sensors based on carbon nanoflake/tin oxide composites for ammonia detection.

PubMed

Lee, Soo-Keun; Chang, Daeic; Kim, Sang Wook

2014-03-15

Carbon nanoflake (CNFL) was obtained from graphite pencil by using the electrochemical method and the CNFL/SnO2 composite material assessed its potential as an ammonia gas sensor. A thin film resistive gas sensor using the composite material was manufactured by the drop casting method, and the sensor was evaluated to test in various ammonia concentrations and operating temperatures. Physical and chemical characteristics of the composite material were assessed using SEM, TEM, SAED, EDS and Raman spectroscopy. The composite material having 10% of SnO2 showed 3 times higher sensor response and better repeatability than the gas sensor using pristine SnO2 nano-particle at the optimal temperature of 350°C. Copyright © 2013 Elsevier B.V. All rights reserved.

Graphite Screen-Printed Electrodes Applied for the Accurate and Reagentless Sensing of pH.

PubMed

Galdino, Flávia E; Smith, Jamie P; Kwamou, Sophie I; Kampouris, Dimitrios K; Iniesta, Jesus; Smith, Graham C; Bonacin, Juliano A; Banks, Craig E

2015-12-01

A reagentless pH sensor based upon disposable and economical graphite screen-printed electrodes (GSPEs) is demonstrated for the first time. The voltammetric pH sensor utilizes GSPEs which are chemically pretreated to form surface immobilized oxygenated species that, when their redox behavior is monitored, give a Nernstian response over a large pH range (1-13). An excellent experimental correlation is observed between the voltammetric potential and pH over the entire pH range of 1-13 providing a simple approach with which to monitor solution pH. Such a linear response over this dynamic pH range is not usually expected but rather deviation from linearity is encountered at alkaline pH values; absence of this has previously been attributed to a change in the pKa value of surface immobilized groups from that of solution phase species. This non-deviation, which is observed here in the case of our facile produced reagentless pH sensor and also reported in the literature for pH sensitive compounds immobilized upon carbon electrodes/surfaces, where a linear response is observed over the entire pH range, is explained alternatively for the first time. The performance of the GSPE pH sensor is also directly compared with a glass pH probe and applied to the measurement of pH in "real" unbuffered samples where an excellent correlation between the two protocols is observed validating the proposed GSPE pH sensor.

Role of oxygen-containing functional groups in forest fire-generated and pyrolytic chars for immobilization of copper and nickel.

PubMed

Esfandbod, Maryam; Merritt, Christopher R; Rashti, Mehran Rezaei; Singh, Balwant; Boyd, Sue E; Srivastava, Prashant; Brown, Christopher L; Butler, Orpheus M; Kookana, Rai S; Chen, Chengrong

2017-01-01

Char as a carbon-rich material, can be produced under pyrolytic conditions, wildfires or prescribed burn offs for fire management. The objective of this study was to elucidate mechanistic interactions of copper (Cu 2+ ) and nickel (Ni 2+ ) with different chars produced by pyrolysis (green waste, GW; blue-Mallee, BM) and forest fires (fresh-burnt by prescribed fire, FC; aged char produced by wild fire, AC). The pyrolytic chars were more effective sorbents of Cu 2+ (∼11 times) and Ni 2+ (∼5 times) compared with the forest fire chars. Both cross-polarization (CPMAS-NMR) and Bloch decay (BDMAS-NMR) 13 C NMR spectroscopies showed that forest fire chars have higher woody components (aromatic functional groups) and lower polar groups (e.g. O-alkyl C) compared with the pyrolytic chars. The polarity index was greater in the pyrolytic chars (0.99-1.34) than in the fire-generated chars (0.98-1.15), while aromaticity was lower in the former than in the latter. Fourier transform infrared (FTIR) and Raman spectroscopies indicated the binding of carbonate and phosphate with both Cu 2+ and Ni 2+ in all chars, but with a greater extent in pyrolytic than forest fire-generated chars. These findings have demonstrated the key role of char's oxygen-containing functional groups in determining their sorption capacity for the Cu 2+ and Ni 2+ in contaminated lands. Copyright © 2016 Elsevier Ltd. All rights reserved.

A simple preparation of graphite/gelatin composite for electrochemical detection of dopamine.

PubMed

Rajkumar, Chellakannu; Thirumalraj, Balamurugan; Chen, Shen-Ming; Chen, His-An

2017-02-01

In this study, we demonstrate a simple preparation of graphite (GR) sheets assisted with gelatin (GLN) polypeptide composite was developed for sensitive detection of dopamine (DA) sensor. The GR/GLN composite was prepared by GR powder in GLN solution (5mg/mL) via sonication process. The prepared GR/GLN composite displays well dispersion ability in biopolymer matrix and characterized via scanning electron microscope (SEM), Fourier transform infrared (FTIR) spectroscopy and electrochemical impedance spectroscopy (EIS) studies. The GR/GLN modified electrode showed an excellent electrocatalytic activity toward the oxidation of DA, suggesting that the successful formation of GR sheets crosslinked with the functional groups of GLN polypeptide. In addition, the GR/GLN modified electrode achieved a wide linear response ranging from 0.05 to 79.5μM with a detection limit of 0.0045μM. The calculated analytical sensitivity of the sensor was 1.36±0.02μAμM -1 cm -2 . Conversely, the modified electrode demonstrates a good storage stability, reproducibility and repeatability. In addition, the sensor manifests the determination of DA in human serum and urine samples for practical applications. Copyright © 2016 Elsevier Inc. All rights reserved.

Uncondensed Graphitic Carbon Nitride on Reduced Graphene Oxide for Oxygen Sensing via a Photoredox Mechanism

DOE PAGES

Ellis, James E.; Sorescu, Dan C.; Burkert, Seth C.; ...

2017-07-24

Melon, a polymeric, uncondensed graphitic carbon nitride with a two-dimensional structure, has been coupled with reduced graphene oxide (rGO) to create an oxygen chemiresistor sensor that is active under UV photoactivation. Oxygen gas is an important sensor target in a variety of areas including industrial safety, combustion process monitoring, as well as environmental and biomedical fields. Because of the intimate electrical interface formed between melon and rGO, charge transfer of photoexcited electrons occurs between the two materials when under UV (λ = 365 nm) irradiation. A photoredox mechanism wherein oxygen is reduced on the rGO surface provides the basis formore » sensing oxygen gas in the concentration range 300–100 000 ppm. The sensor response was found to be logarithmically proportional to oxygen gas concentration. DFT calculations of a melon-oxidized graphene composite found that slight protonation of melon leads to charge accumulation on the rGO layer and a corresponding charge depletion on the melon layer. As a result, this work provides an example of a metal-free system for solid–gas interface sensing via a photoredox mechanism.« less

Uncondensed Graphitic Carbon Nitride on Reduced Graphene Oxide for Oxygen Sensing via a Photoredox Mechanism

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

Ellis, James E.; Sorescu, Dan C.; Burkert, Seth C.

Melon, a polymeric, uncondensed graphitic carbon nitride with a two-dimensional structure, has been coupled with reduced graphene oxide (rGO) to create an oxygen chemiresistor sensor that is active under UV photoactivation. Oxygen gas is an important sensor target in a variety of areas including industrial safety, combustion process monitoring, as well as environmental and biomedical fields. Because of the intimate electrical interface formed between melon and rGO, charge transfer of photoexcited electrons occurs between the two materials when under UV (λ = 365 nm) irradiation. A photoredox mechanism wherein oxygen is reduced on the rGO surface provides the basis formore » sensing oxygen gas in the concentration range 300–100 000 ppm. The sensor response was found to be logarithmically proportional to oxygen gas concentration. DFT calculations of a melon-oxidized graphene composite found that slight protonation of melon leads to charge accumulation on the rGO layer and a corresponding charge depletion on the melon layer. As a result, this work provides an example of a metal-free system for solid–gas interface sensing via a photoredox mechanism.« less

Dinuclear copper(II) octaazamacrocyclic complex in a PVC coated GCE and graphite as a voltammetric sensor for determination of gallic acid and antioxidant capacity of wine samples.

PubMed

Petković, B B; Stanković, D; Milčić, M; Sovilj, S P; Manojlović, D

2015-01-01

A novel efficient differential pulse voltammetric (DPV) method for determination gallic acid (GA) was developed by using an electrochemical sensor based on [Cu2tpmc](ClO4)4 immobilized in PVC matrix and coated on graphite (CGE) or classy carbon rod (CGCE). The proposed method is based on the gallic acid oxidation process at formed [Cu2tpmcGA](3+) complex at the electrode surface. The complexation was explored by molecular modeling and DFT calculations. Voltammograms for both sensors, recorded in a HNO3 as a supporting electrolyte at pH 2 and measured in 2.5×10(-7) to 1.0×10(-4) M of GA, resulted with two linear calibration curves (for higher and lower GA concentration range). The detection limit at CGE was 1.48×10(-7) M, while at CGCE was 4.6×10(-6) M. CGE was successfully applied for the determination of the antioxidant capacity based on GA equivalents for white, rosé and red wine samples. Copyright © 2014 Elsevier B.V. All rights reserved.

2D nanosheet molybdenum disulphide (MoS2) modified electrodes explored towards the hydrogen evolution reaction

NASA Astrophysics Data System (ADS)

Rowley-Neale, Samuel J.; Brownson, Dale A. C.; Smith, Graham C.; Sawtell, David A. G.; Kelly, Peter J.; Banks, Craig E.

2015-10-01

We explore the use of two-dimensional (2D) MoS2 nanosheets as an electrocatalyst for the Hydrogen Evolution Reaction (HER). Using four commonly employed commercially available carbon based electrode support materials, namely edge plane pyrolytic graphite (EPPG), glassy carbon (GC), boron-doped diamond (BDD) and screen-printed graphite electrodes (SPE), we critically evaluate the reported electrocatalytic performance of unmodified and MoS2 modified electrodes towards the HER. Surprisingly, current literature focuses almost exclusively on the use of GC as an underlying support electrode upon which HER materials are immobilised. 2D MoS2 nanosheet modified electrodes are found to exhibit a coverage dependant electrocatalytic effect towards the HER. Modification of the supporting electrode surface with an optimal mass of 2D MoS2 nanosheets results in a lowering of the HER onset potential by ca. 0.33, 0.57, 0.29 and 0.31 V at EPPG, GC, SPE and BDD electrodes compared to their unmodified counterparts respectively. The lowering of the HER onset potential is associated with each supporting electrode's individual electron transfer kinetics/properties and is thus distinct. The effect of MoS2 coverage is also explored. We reveal that its ability to catalyse the HER is dependent on the mass deposited until a critical mass of 2D MoS2 nanosheets is achieved, after which its electrocatalytic benefits and/or surface stability curtail. The active surface site density and turn over frequency for the 2D MoS2 nanosheets is determined, characterised and found to be dependent on both the coverage of 2D MoS2 nanosheets and the underlying/supporting substrate. This work is essential for those designing, fabricating and consequently electrochemically testing 2D nanosheet materials for the HER.We explore the use of two-dimensional (2D) MoS2 nanosheets as an electrocatalyst for the Hydrogen Evolution Reaction (HER). Using four commonly employed commercially available carbon based electrode support materials, namely edge plane pyrolytic graphite (EPPG), glassy carbon (GC), boron-doped diamond (BDD) and screen-printed graphite electrodes (SPE), we critically evaluate the reported electrocatalytic performance of unmodified and MoS2 modified electrodes towards the HER. Surprisingly, current literature focuses almost exclusively on the use of GC as an underlying support electrode upon which HER materials are immobilised. 2D MoS2 nanosheet modified electrodes are found to exhibit a coverage dependant electrocatalytic effect towards the HER. Modification of the supporting electrode surface with an optimal mass of 2D MoS2 nanosheets results in a lowering of the HER onset potential by ca. 0.33, 0.57, 0.29 and 0.31 V at EPPG, GC, SPE and BDD electrodes compared to their unmodified counterparts respectively. The lowering of the HER onset potential is associated with each supporting electrode's individual electron transfer kinetics/properties and is thus distinct. The effect of MoS2 coverage is also explored. We reveal that its ability to catalyse the HER is dependent on the mass deposited until a critical mass of 2D MoS2 nanosheets is achieved, after which its electrocatalytic benefits and/or surface stability curtail. The active surface site density and turn over frequency for the 2D MoS2 nanosheets is determined, characterised and found to be dependent on both the coverage of 2D MoS2 nanosheets and the underlying/supporting substrate. This work is essential for those designing, fabricating and consequently electrochemically testing 2D nanosheet materials for the HER. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr05164a|ART

Toxic Effect of Cadmium Assay in Contaminated Soil Earthworm Cell Using Modified Sensor

PubMed Central

Kyung, Lee; Kim, Chae Hwa; Seo, Roma; Lee, Soo Youn; Kim, Lina; Chae, Su min; Choi, Sung Wook; Kim, Ji Yoon

2015-01-01

A voltammetric toxic metal of cadmium detection was studied using a fluorine doped graphite pencil electrode (FPE) in a seawater electrolyte. In this study, square wave (SW) stripping and chronoamerometry were used for determination of Cd(II) in seawater. Affordable pencils and an auxiliary electrode were used as reference. All experiments in this study could be performed at reasonable cost by using graphite pencil. The application was performed on the tissue of contaminated soil earthworm. The results show that the method can be applicable for vegetables and in vivo fluid or medicinal diagnosis. PMID:26191388

Mechanically robust, electrically conductive ultralow-density carbon nanotube-based aerogels

DOEpatents

Worsley, Marcus A.; Baumann, Theodore F.; Satcher, Jr., Joe H.

2016-10-04

Disclosed here is a device comprising a porous carbon aerogel or composite thereof as an energy storage material, catalyst support, sensor or adsorbent, wherein the porous carbon aerogel comprises a network of interconnected struts comprising carbon nanotube bundles covalently crosslinked by graphitic carbon nanoparticles, wherein the carbon nanotubes account for 5 to 95 wt. % of the aerogel and the graphitic carbon nanoparticles account for 5 to 95 wt. % of the aerogel, and wherein the aerogel has an electrical conductivity of at least 10 S/m and is capable of withstanding strains of more than 10% before fracture.

Covering surface nanobubbles with a NaCl nanoblanket.

PubMed

Berkelaar, Robin P; Zandvliet, Harold J W; Lohse, Detlef

2013-09-10

By letting a NaCl aqueous solution of low (0.01 M) concentration evaporate on a highly oriented pyrolytic graphite (HOPG) surface, it is possible to form a thin film of salt. However, pre-existing surface nanobubbles prevent the homogeneous coverage of the surface with the salt, keeping the footprint areas on the substrate pristine. Comparing the surface nanobubbles in the salt solution with their associated footprint after drying, provides information on the shrinkage of nanobubbles during the hours-long process of drying the liquid film. At a slightly higher NaCl concentration and thus salt layer thickness, the nanobubbles are covered with a thin blanket of salt. Once the liquid film has evaporated until a water film remains that is smaller than the height of the nanobubbles, the blanket of salt cracks and unfolds into a flower-like pattern of salt flakes that is located at the rim of the nanobubble footprint. The formation of a blanket of salt covering the nanobubbles is likely to considerably or even completely block the gas out-flux from the nanobubble, partially stabilizing the nanobubbles against dissolution.

Evolution of elastic x-ray scattering in laser-shocked warm dense lithium.

PubMed

Kugland, N L; Gregori, G; Bandyopadhyay, S; Brenner, C M; Brown, C R D; Constantin, C; Glenzer, S H; Khattak, F Y; Kritcher, A L; Niemann, C; Otten, A; Pasley, J; Pelka, A; Roth, M; Spindloe, C; Riley, D

2009-12-01

We have studied the dynamics of warm dense Li with near-elastic x-ray scattering. Li foils were heated and compressed using shock waves driven by 4-ns-long laser pulses. Separate 1-ns-long laser pulses were used to generate a bright source of 2.96 keV Cl Ly- alpha photons for x-ray scattering, and the spectrum of scattered photons was recorded at a scattering angle of 120 degrees using a highly oriented pyrolytic graphite crystal operated in the von Hamos geometry. A variable delay between the heater and backlighter laser beams measured the scattering time evolution. Comparison with radiation-hydrodynamics simulations shows that the plasma is highly coupled during the first several nanoseconds, then relaxes to a moderate coupling state at later times. Near-elastic scattering amplitudes have been successfully simulated using the screened one-component plasma model. Our main finding is that the near-elastic scattering amplitudes are quite sensitive to the mean ionization state Z[over ] and by extension to the choice of ionization model in the radiation-hydrodynamics simulations used to predict plasma properties within the shocked Li.

A priori calculations of the free energy of formation from solution of polymorphic self-assembled monolayers

PubMed Central

Reimers, Jeffrey R.; Panduwinata, Dwi; Visser, Johan; Chin, Yiing; Tang, Chunguang; Goerigk, Lars; Ford, Michael J.; Sintic, Maxine; Sum, Tze-Jing; Coenen, Michiel J. J.; Hendriksen, Bas L. M.; Elemans, Johannes A. A. W.; Hush, Noel S.; Crossley, Maxwell J.

2015-01-01

Modern quantum chemical electronic structure methods typically applied to localized chemical bonding are developed to predict atomic structures and free energies for meso-tetraalkylporphyrin self-assembled monolayer (SAM) polymorph formation from organic solution on highly ordered pyrolytic graphite surfaces. Large polymorph-dependent dispersion-induced substrate−molecule interactions (e.g., −100 kcal mol−1 to −150 kcal mol−1 for tetratrisdecylporphyrin) are found to drive SAM formation, opposed nearly completely by large polymorph-dependent dispersion-induced solvent interactions (70–110 kcal mol−1) and entropy effects (25–40 kcal mol−1 at 298 K) favoring dissolution. Dielectric continuum models of the solvent are used, facilitating consideration of many possible SAM polymorphs, along with quantum mechanical/molecular mechanical and dispersion-corrected density functional theory calculations. These predict and interpret newly measured and existing high-resolution scanning tunnelling microscopy images of SAM structure, rationalizing polymorph formation conditions. A wide range of molecular condensed matter properties at room temperature now appear suitable for prediction and analysis using electronic structure calculations. PMID:26512115

Thrombin-Binding Aptamer Quadruplex Formation: AFM and Voltammetric Characterization

PubMed Central

Diculescu, Victor Constantin; Chiorcea-Paquim, Ana-Maria; Eritja, Ramon; Oliveira-Brett, Ana Maria

2010-01-01

The adsorption and the redox behaviour of thrombin-binding aptamer (TBA) and extended TBA (eTBA) were studied using atomic force microscopy and voltammetry at highly oriented pyrolytic graphite and glassy carbon. The different adsorption patterns and degree of surface coverage were correlated with the sequence base composition, presence/absence of K+, and voltammetric behaviour of TBA and eTBA. In the presence of K+, only a few single-stranded sequences present adsorption, while the majority of the molecules forms stable and rigid quadruplexes with no adsorption. Both TBA and eTBA are oxidized and the only anodic peak corresponds to guanine oxidation. Upon addition of K+ ions, TBA and eTBA fold into a quadruplex, causing the decrease of guanine oxidation peak and occurrence of a new peak at a higher potential due to the oxidation of G-quartets. The higher oxidation potential of G-quartets is due to the greater difficulty of electron transfer from the inside of the quadruplex to the electrode surface than electron transfer from the more flexible single strands. PMID:20798847

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

Han, Yong; Lii-Rosales, A.; Zhou, Y.

Theory and stochastic lattice-gas modeling is developed for the formation of intercalated metal islands in the gallery between the top layer and the underlying layer at the surface of layered materials. Our model for this process involves deposition of atoms, some fraction of which then enter the gallery through well-separated pointlike defects in the top layer. Subsequently, these atoms diffuse within the subsurface gallery leading to nucleation and growth of intercalated islands nearby the defect point source. For the case of a single point defect, continuum diffusion equation analysis provides insight into the nucleation kinetics. However, complementary tailored lattice-gas modelingmore » produces a more comprehensive and quantitative characterization. We analyze the large spread in nucleation times and positions relative to the defect for the first nucleated island. We also consider the formation of subsequent islands and the evolution of island growth shapes. The shapes reflect in part our natural adoption of a hexagonal close-packed island structure. As a result, motivation and support for the model is provided by scanning tunneling microscopy observations of the formation of intercalated metal islands in highly-ordered pyrolytic graphite at higher temperatures.« less

Enzyme-linked electrochemical DNA ligation assay using magnetic beads.

PubMed

Stejskalová, Eva; Horáková, Petra; Vacek, Jan; Bowater, Richard P; Fojta, Miroslav

2014-07-01

DNA ligases are essential enzymes in all cells and have been proposed as targets for novel antibiotics. Efficient DNA ligase activity assays are thus required for applications in biomedical research. Here we present an enzyme-linked electrochemical assay based on two terminally tagged probes forming a nicked junction upon hybridization with a template DNA. Nicked DNA bearing a 5' biotin tag is immobilized on the surface of streptavidin-coated magnetic beads, and ligated product is detected via a 3' digoxigenin tag recognized by monoclonal antibody-alkaline phosphatase conjugate. Enzymatic conversion of napht-1-yl phosphate to napht-1-ol enables sensitive detection of the voltammetric signal on a pyrolytic graphite electrode. The technique was tested under optimal conditions and various situations limiting or precluding the ligation reaction (such as DNA substrates lacking 5'-phosphate or containing a base mismatch at the nick junction, or application of incompatible cofactor), and utilized for the analysis of the nick-joining activity of a range of recombinant Escherichia coli DNA ligase constructs. The novel technique provides a fast, versatile, specific, and sensitive electrochemical assay of DNA ligase activity.

Comprehensive Adsorption Studies of Doxycycline and Ciprofloxacin Antibiotics by Biochars Prepared at Different Temperatures

PubMed Central

Zeng, Zhi-wei; Tan, Xiao-fei; Liu, Yun-guo; Tian, Si-rong; Zeng, Guang-ming; Jiang, Lu-hua; Liu, Shao-bo; Li, Jiang; Liu, Ni; Yin, Zhi-hong

2018-01-01

This paper comparatively investigated the removal efficiency and mechanisms of rice straw biochars prepared under three pyrolytic temperatures for two kinds of tetracycline and quinolone antibiotics (doxycycline and ciprofloxacin). The influencing factors of antibiotic adsorption (including biochar dosage, pH, background electrolytes, humic acid, initial antibiotics concentration, contact time, and temperature) were comprehensively studied. The results suggest that biochars produced at high-temperature [i.e., 700°C (BC700)], have higher adsorption capacity for the two antibiotics than low-temperature (i.e., 300–500°C) biochars (BC300 and BC500). Higher surface area gives rise to greater volume of micropores and mesopores, and higher graphitic surfaces of the BC700 contributed to its higher functionality. The maximum adsorption capacity was found to be in the following order: DOX > CIP. The π-π EDA interaction and hydrogen bonding might be the predominant adsorption mechanisms. Findings in this study highlight the important roles of high-temperature biochars in controlling the contamination of tetracycline and quinolone antibiotics in the environment. PMID:29637067

Effect of intermolecular dipole-dipole interactions on interfacial supramolecular structures of C3-symmetric hexa-peri-hexabenzocoronene derivatives.

PubMed

Mu, Zhongcheng; Shao, Qi; Ye, Jun; Zeng, Zebing; Zhao, Yang; Hng, Huey Hoon; Boey, Freddy Yin Chiang; Wu, Jishan; Chen, Xiaodong

2011-02-15

Two-dimensional (2D) supramolecular assemblies of a series of novel C(3)-symmetric hexa-peri-hexabenzocoronene (HBC) derivatives bearing different substituents adsorbed on highly oriented pyrolytic graphite were studied by using scanning tunneling microscopy at a solid-liquid interface. It was found that the intermolecular dipole-dipole interactions play a critical role in controlling the interfacial supramolecular assembly of these C(3)-symmetric HBC derivatives at the solid-liquid interface. The HBC molecule bearing three -CF(3) groups could form 2D honeycomb structures because of antiparallel dipole-dipole interactions, whereas HBC molecules bearing three -CN or -NO(2) groups could form hexagonal superstructures because of a special trimeric arrangement induced by dipole-dipole interactions and weak hydrogen bonding interactions ([C-H···NC-] or [C-H···O(2)N-]). Molecular mechanics and dynamics simulations were performed to reveal the physics behind the 2D structures as well as detailed functional group interactions. This work provides an example of how intermolecular dipole-dipole interactions could enable fine control over the self-assembly of disklike π-conjugated molecules.

Imaging nanoclusters in the constant height mode of the dynamic SFM.

PubMed

Barth, Clemens; Pakarinen, Olli H; Foster, Adam S; Henry, Claude R

2006-04-14

For the first time, high quality images of metal nanoclusters which were recorded in the constant height mode of a dynamic scanning force microscope (dynamic SFM) are shown. Surfaces of highly ordered pyrolytic graphite (HOPG) were used as a test substrate since metal nanoclusters with well defined and symmetric shapes can be created by epitaxial growth. We performed imaging of gold clusters with sizes between 5 and 15 nm in both scanning modes, constant Δf mode and constant height mode, and compared the image contrast. We notice that clusters in constant height images appear much sharper, and exhibit more reasonable lateral shapes and sizes in comparison to images recorded in the constant Δf mode. With the help of numerical simulations we show that only a microscopically small part of the tip apex (nanotip) is probably the main contributor for the image contrast formation. In principle, the constant height mode can be used for imaging surfaces of any material, e.g. ionic crystals, as shown for the system Au/NaCl(001).

Kinetics of solvent supported tubule formation of Lotus (Nelumbo nucifera) wax on highly oriented pyrolytic graphite (HOPG) investigated by atomic force microscopy

PubMed Central

Koch, Kerstin; Barthlott, Wilhelm; Wandelt, Klaus

2018-01-01

The time dependence of the formation of lotus wax tubules after recrystallization from various chloroform-based solutions on an HOPG surface at room temperature was studied by atomic force microscopy (magnetic AC mode) taking series of consecutive images of the formation process. The growth of the tubules oriented in an upright fashion follows a sequential rodlet→ring→tubule behavior. The influence of a number of factors, e.g., different wax concentration in chloroform, the additional presence of water, or salts [(NH4)2SO4, NH4NO3] or a mixture of salt/water in the solution on the growth rate and orientation of the tubules is also investigated. Different wax concentrations were found to have no effect on the growth rate or the orientation of tubules in none of the solutions. The presence of water, however, considerably increased the growth rate of tubule formation, while the presence of salt was again found to have no effect on growth rate or orientation of tubules. PMID:29515959

The HB-2D Polarized Neutron Development Beamline at the High Flux Isotope Reactor

NASA Astrophysics Data System (ADS)

Crow, Lowell; Hamilton, WA; Zhao, JK; Robertson, JL

2016-09-01

The Polarized Neutron Development beamline, recently commissioned at the HB-2D position on the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory, provides a tool for development and testing of polarizers, polarized neutron devices, and prototyping of polarized neutron techniques. With available monochromators including pyrolytic graphite and polarizing enriched Fe-57 (Si), the instrument has operated at 4.25 and 2.6 Å wavelengths, using crystal, supermirror, or He-3 polarizers and analyzers in various configurations. The Neutron Optics and Development Team has used the beamline for testing of He-3 polarizers for use at other HFIR and Spallation Neutron Source (SNS) instruments, as well as a variety of flipper devices. Recently, we have acquired new supermirror polarizers which have improved the instrument performance. The team and collaborators also have continuing demonstration experiments of spin-echo focusing techniques, and plans to conduct polarized diffraction measurements. The beamline is also used to support a growing use of polarization techniques at present and future instruments at SNS and HFIR.

Direct electrochemistry of nitrate reductase from the fungus Neurospora crassa.

PubMed

Kalimuthu, Palraj; Ringel, Phillip; Kruse, Tobias; Bernhardt, Paul V

2016-09-01

We report the first direct (unmediated) catalytic electrochemistry of a eukaryotic nitrate reductase (NR). NR from the filamentous fungus Neurospora crassa, is a member of the mononuclear molybdenum enzyme family and contains a Mo, heme and FAD cofactor which are involved in electron transfer from NAD(P)H to the (Mo) active site where reduction of nitrate to nitrite takes place. NR was adsorbed on an edge plane pyrolytic graphite (EPG) working electrode. Non-turnover redox responses were observed in the absence of nitrate from holo NR and three variants lacking the FAD, heme or Mo cofactor. The FAD response is due to dissociated cofactor in all cases. In the presence of nitrate, NR shows a pronounced cathodic catalytic wave with an apparent Michaelis constant (KM) of 39μM (pH7). The catalytic cathodic current increases with temperature from 5 to 35°C and an activation enthalpy of 26kJmol(-1) was determined. In spite of dissociation of the FAD cofactor, catalytically activity is maintained. Copyright © 2016. Published by Elsevier B.V.

Comprehensive adsorption studies of doxycycline and ciprofloxacin antibiotics by biochars prepared at different temperatures

NASA Astrophysics Data System (ADS)

Zeng, Zhi-wei; Tan, Xiao-fei; Liu, Yun-guo; Tian, Si-rong; Zeng, Guang-ming; Jiang, Lu-hua; Liu, Shao-bo; Li, Jiang; Liu, Ni; Yin, Zhi-hong

2018-03-01

This paper comparatively investigated the removal efficiency and mechanisms of rice straw biochars prepared under three pyrolytic temperatures for two kinds of tetracycline and quinolone antibiotics (doxycycline and ciprofloxacin). The influencing factors of antibiotic adsorption (including biochar dosage, pH, background electrolytes, humic acid, initial antibiotics concentration, contact time, and temperature) were comprehensively studied. The results suggest that biochars produced at high-temperature (i.e., 700°C (BC700)), have higher adsorption capacity for the two antibiotics than low-temperature (i.e., 300-500°C) biochars (BC300 and BC500). Higher surface area gives rise to greater volume of micropores and mesopores, and higher graphitic surfaces of the BC700 contributed to its higher functionality. The maximum adsorption capacity was found to be in the following order: DOX > CIP. The π-π EDA interaction and hydrogen bonding might be the predominant adsorption mechanisms. Findings in this study highlight the important roles of high-temperature biochars in controlling the contamination of tetracycline and quinolone antibiotics in the environment.

Transport of energy by ultraintense laser-generated electrons in nail-wire targets

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

Ma, T.; Lawrence Livermore National Laboratory, Livermore, California 94550; Key, M. H.

2009-11-15

Nail-wire targets (20 {mu}m diameter copper wires with 80 {mu}m hemispherical head) were used to investigate energy transport by relativistic fast electrons generated in intense laser-plasma interactions. The targets were irradiated using the 300 J, 1 ps, and 2x10{sup 20} W{center_dot}cm{sup -2} Vulcan laser at the Rutherford Appleton Laboratory. A spherically bent crystal imager, a highly ordered pyrolytic graphite spectrometer, and single photon counting charge-coupled device gave absolute Cu K{alpha} measurements. Results show a concentration of energy deposition in the head and an approximately exponential fall-off along the wire with about 60 {mu}m 1/e decay length due to resistive inhibition.more » The coupling efficiency to the wire was 3.3{+-}1.7% with an average hot electron temperature of 620{+-}125 keV. Extreme ultraviolet images (68 and 256 eV) indicate additional heating of a thin surface layer of the wire. Modeling using the hybrid E-PLAS code has been compared with the experimental data, showing evidence of resistive heating, magnetic trapping, and surface transport.« less

Insitu measurement and control of processing properties of composite resins in a production tool

NASA Technical Reports Server (NTRS)

Kranbuehl, D.; Hoff, M.; Haverty, P.; Loos, A.; Freeman, T.

1988-01-01

An in situ measuring technique for use in automated composite processing and quality control is discussed. Frequency dependent electromagnetic sensors are used to measure processing parameters at four ply positions inside a thick section 192-ply graphite-epoxy composite during cure in an 8 x 4 in. autoclave. Viscosity measurements obtained using the sensors are compared with the viscosities calculated using the Loos-Springer cure process model. Good overall agreement is obtained. In a subsequent autoclave run, the output from the four sensors was used to control the autoclave temperature. Using the 'closed loop' sensor controlled autoclave temperature resulted in a more uniform and more rapid cure cycle.

Void forming pyrolytic carbon coating process

DOEpatents

Beatty, Ronald L.; Cook, Jackie L.

2000-01-01

A pyrolytic carbon coated nuclear fuel particle and method of making it. The fuel particle has a core composed of a refractory compound of an actinide metal. The pyrolytic carbon coating surrounds the core so as to provide a void volume therebetween. The coating has an initial density of no greater than 1.45 grams/cm.sup.3 and an anisotropy factor than 3.0 and a final density upon heat treatment above about 2000.degree. C. of greater than 1.7 grams/cm.sup.3 and an anisotropy factor greater than 5.

Pyrolytic Characteristics and Kinetics of Phragmites australis

PubMed Central

Zhao, Hui; Yan, Huaxiao; Zhang, Congwang; Liu, Xiaodong; Xue, Yanhui; Qiao, Yingyun; Tian, Yuanyu; Qin, Song

2011-01-01

The pyrolytic kinetics of Phragmites australis was investigated using thermogravimetric analysis (TGA) method with linear temperature programming process under an inert atmosphere. Kinetic expressions for the degradation rate in devolatilization and combustion steps have been obtained for P. australis with Dollimore method. The values of apparent activation energy, the most probable mechanism functions, and the corresponding preexponential factor were determined. The results show that the model agrees well with the experimental data and provide useful information for the design of pyrolytic processing system using P. australis as feedstock to produce biofuel. PMID:22007256

Pyrolysis characteristics of integrated circuit boards at various particle sizes and temperatures.

PubMed

Chiang, Hung-Lung; Lin, Kuo-Hsiung; Lai, Mei-Hsiu; Chen, Ting-Chien; Ma, Sen-Yi

2007-10-01

A pyrolysis method was employed to recycle the metals and brominated compounds blended into printed circuit boards. This research investigated the effect of particle size and process temperature on the element composition of IC boards and pyrolytic residues, liquid products, and water-soluble ionic species in the exhaust, with the overall goal being to identify the pyrolysis conditions that will have the least impact on the environment. Integrated circuit (IC) boards were crushed into 5-40 mesh (0.71-4.4mm), and the crushed particles were pyrolyzed at temperatures ranging from 200 to 500 degrees C. The thermal decomposition kinetics were measured by a thermogravimetric (TG) analyzer. The composition of pyrolytic residues was analyzed by Energy Dispersive X-ray Spectrometer (EDS), Inductively Coupled Plasma Atomic Emission Spectrometer (ICP-AES) and Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). In addition, the element compositions of liquid products were analyzed by ICP-AES and ICP-MS. Pyrolytic exhaust was collected by a water-absorption system in an ice-bath cooler, and IC analysis showed that the absorbed solution comprised 11 ionic species. Based on the pyrolytic kinetic parameters of TG analysis and pyrolytic residues at various temperatures for 30 min, the effect of particle size was insignificant in this study, and temperature was the key factor for the IC board pyrolysis. Two stages of decomposition were found for IC board pyrolysis under nitrogen atmosphere. The activation energy was 38-47 kcal/mol for the first-stage reaction and 5.2-9.4 kcal/mol for the second-stage reaction. Metal content was low in the liquid by-product of the IC board pyrolysis process, which is an advantage in that the liquid product could be used as a fuel. Brominate and ammonium were the main water-soluble ionic species of the pyrolytic exhaust. A plan for their safe and effective disposal must be developed if the pyrolytic recycling process is to be applied to IC boards.

Electronic structure of multi-walled carbon fullerenes

NASA Astrophysics Data System (ADS)

Doore, Keith; Cook, Matthew; Clausen, Eric; Lukashev, Pavel V.; Kidd, Tim E.; Stollenwerk, Andrew J.

2017-02-01

Despite an enormous amount of research on carbon based nanostructures, relatively little is known about the electronic structure of multi-walled carbon fullerenes, also known as carbon onions. In part, this is due to the very high computational expense involved in estimating electronic structure of large molecules. At the same time, experimentally, the exact crystal structure of the carbon onion is usually unknown, and therefore one relies on qualitative arguments only. In this work we present the results of a computational study on a series of multi-walled fullerenes and compare their electronic structures to experimental data. Experimentally, the carbon onions were fabricated using ultrasonic agitation of isopropanol alcohol and deposited onto the surface of highly ordered pyrolytic graphite using a drop cast method. Scanning tunneling microscopy images indicate that the carbon onions produced using this technique are ellipsoidal with dimensions on the order of 10 nm. The majority of differential tunneling spectra acquired on individual carbon onions are similar to that of graphite with the addition of molecular-like peaks, indicating that these particles span the transition between molecules and bulk crystals. A smaller, yet sizable number exhibited a semiconducting gap between the highest occupied molecular orbital (HOMO) and the lowest unoccupied molecular orbital (LUMO) levels. These results are compared with the electronic structure of different carbon onion configurations calculated using first-principles. Similar to the experimental results, the majority of these configurations are metallic with a minority behaving as semiconductors. Analysis of the configurations investigated here reveals that each carbon onion exhibiting an energy band gap consisted only of non-metallic fullerene layers, indicating that the interlayer interaction is not significant enough to affect the total density of states in these structures.

Determination of cadmium in coal using solid sampling graphite furnace high-resolution continuum source atomic absorption spectrometry.

PubMed

da Silva, Alessandra Furtado; Borges, Daniel L G; Lepri, Fábio Grandis; Welz, Bernhard; Curtius, Adilson J; Heitmann, Uwe

2005-08-01

This work describes the development of a method to determine cadmium in coal, in which iridium is used as a permanent chemical modifier and calibration is performed against aqueous standards by high-resolution continuum source atomic absorption spectrometry (HR-CS AAS). This new instrumental concept makes the whole spectral environment in the vicinity of the analytical line accessible, providing a lot more data than just the change in absorbance over time available from conventional instruments. The application of Ir (400 microg) as a permanent chemical modifier, thermally deposited on the pyrolytic graphite platform surface, allowed pyrolysis temperatures of 700 degrees C to be used, which was sufficiently high to significantly reduce the continuous background that occurred before the analyte signal at pyrolysis temperatures <700 degrees C. Structured background absorption also occurred after the analyte signal when atomization temperatures of >1600 degrees C were used, which arose from the electron-excitation spectrum (with rotational fine structure) of a diatomic molecule. Under optimized conditions (pyrolysis at 700 degrees C and atomization at 1500 degrees C), interference-free determination of cadmium in seven certified coal reference materials and two real samples was achieved by direct solid sampling and calibrating against aqueous standards, resulting in good agreement with the certified values (where available) at the 95% confidence level. A characteristic mass of 0.4 pg and a detection limit of 2 ng g(-1), calculated for a sample mass of 1.0 mg coal, was obtained. A precision (expressed as the relative standard deviation, RSD) of <10% was typically obtained when coal samples in the mass range 0.6-1.2 mg were analyzed.

Study of Copper and Purine-Copper Complexes on Modified Carbon Electrodes by Cyclic and Elimination Voltammetry

PubMed Central

Trnkova, Libuse; Zerzankova, Lenka; Dycka, Filip; Mikelova, Radka; Jelen, Frantisek

2008-01-01

Using a paraffin impregnated graphite electrode (PIGE) and mercury-modified pyrolytic graphite electrode with basal orientation (Hg-PGEb) copper(II) and Cu(II)-DNA purine base solutions have been studied by cyclic (CV) and linear sweep voltammetry (LSV) in connection with elimination voltammetry with linear scan (EVLS). In chloride and bromide solutions (pH 6), the redox process of Cu(II) proceeded on PIGE with two cathodic and two anodic potentially separated signals. According to the elimination function E4, the first cathodic peak corresponds to the reduction Cu(II) + e- → Cu(I) with the possibility of fast disproportionation 2Cu(I) → Cu(II)+ Cu(0). The E4 of the second cathodic peak signalized an electrode process controlled by a surface reaction. The electrode system of Cu(II) on Hg-PGEb in borate buffer (pH 9.2) was characterized by one cathodic and one anodic peak. Anodic stripping voltammetry (ASV) on PIGE and cathodic stripping voltammetry (CSV) on Hg-PGEb were carried out at potentials where the reduction of copper ions took place and Cu(I)-purine complexes were formed. By using ASV and CSV in combination with EVLS, the sensitivity of Cu(I)-purine complex detection was enhanced relative to either ASV or CSV alone, resulting in higher peak currents of more than one order of magnitude. The statistical treatment of CE data was used to determine the reproducibility of measurements. Our results show that EVLS in connection with the stripping procedure is useful for both qualitative and quantitative microanalysis of purine derivatives and can also reveal details of studied electrode processes. PMID:27879715

2D nanosheet molybdenum disulphide (MoS2) modified electrodes explored towards the hydrogen evolution reaction.

PubMed

Rowley-Neale, Samuel J; Brownson, Dale A C; Smith, Graham C; Sawtell, David A G; Kelly, Peter J; Banks, Craig E

2015-11-21

We explore the use of two-dimensional (2D) MoS2 nanosheets as an electrocatalyst for the Hydrogen Evolution Reaction (HER). Using four commonly employed commercially available carbon based electrode support materials, namely edge plane pyrolytic graphite (EPPG), glassy carbon (GC), boron-doped diamond (BDD) and screen-printed graphite electrodes (SPE), we critically evaluate the reported electrocatalytic performance of unmodified and MoS2 modified electrodes towards the HER. Surprisingly, current literature focuses almost exclusively on the use of GC as an underlying support electrode upon which HER materials are immobilised. 2D MoS2 nanosheet modified electrodes are found to exhibit a coverage dependant electrocatalytic effect towards the HER. Modification of the supporting electrode surface with an optimal mass of 2D MoS2 nanosheets results in a lowering of the HER onset potential by ca. 0.33, 0.57, 0.29 and 0.31 V at EPPG, GC, SPE and BDD electrodes compared to their unmodified counterparts respectively. The lowering of the HER onset potential is associated with each supporting electrode's individual electron transfer kinetics/properties and is thus distinct. The effect of MoS2 coverage is also explored. We reveal that its ability to catalyse the HER is dependent on the mass deposited until a critical mass of 2D MoS2 nanosheets is achieved, after which its electrocatalytic benefits and/or surface stability curtail. The active surface site density and turn over frequency for the 2D MoS2 nanosheets is determined, characterised and found to be dependent on both the coverage of 2D MoS2 nanosheets and the underlying/supporting substrate. This work is essential for those designing, fabricating and consequently electrochemically testing 2D nanosheet materials for the HER.

Modified Au nanoparticles-imprinted sol-gel, multiwall carbon nanotubes pencil graphite electrode used as a sensor for ranitidine determination.

PubMed

Rezaei, B; Lotfi-Forushani, H; Ensafi, A A

2014-04-01

A new, simple, and disposable molecularly imprinted electrochemical sensor for the determination of ranitidine was developed on pencil graphite electrode (PGE) via cyclic voltammetry (CV). The PGEs were coated with MWCNTs containing the carboxylic functional group (f-MWCNTs), imprinted with sol-gel and Au nanoparticle (AuNPs) layers (AuNP/MIP-sol-gel/f-MWCNT/PGE), respectively, to enhance the electrode's electrical transmission and sensitivity. The thin film of molecularly imprinted sol-gel polymers with specific binding sites for ranitidine was cast on modified PGE by electrochemical deposition. The AuNP/MIP-sol-gel/f-MWCNT/PGE thus developed was characterized by electrochemical impedance spectroscopy (EIS) and CV. The interaction between the imprinted sensor and the target molecule was also observed on the electrode by measuring the current response of 5.0mMK3[Fe(CN)6] solution as an electrochemical probe. The pick currents of ranitidine increased linearly with concentration in the ranges of 0.05 to 2.0μM, with a detection limit of (S/N=3) 0.02μM. Finally, the modified electrode was successfully employed to determine ranitidine in human urine samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Aromatics extraction from pyrolytic sugars using ionic liquid to enhance sugar fermentability.

PubMed

Li, Xiaohua; Luque-Moreno, Luis C; Oudenhoven, Stijn R G; Rehmann, Lars; Kersten, Sascha R A; Schuur, Boelo

2016-09-01

Fermentative bioethanol production from pyrolytic sugars was improved via aromatics removal by liquid-liquid extraction. As solvents, the ionic liquid (IL) trihexyltetradecylphosphonium dicyanamide (P666,14[N(CN)2]) and ethyl acetate (EA) were compared. Two pyrolytic sugar solutions were created from acid-leached and untreated pinewood, with levoglucosan contents (most abundant sugar) of 29.0% and 8.3% (w/w), respectively. In a single stage extraction, 70% of the aromatics were effectively removed by P666,14[N(CN)2] and 50% by EA, while no levoglucosan was extracted. The IL was regenerated by vacuum evaporation (100mbar) at 220°C, followed by extraction of aromatics from fresh pyrolytic sugar solutions. Regenerated IL extracted aromatics with similar extraction efficiency as the fresh IL, and the purified sugar fraction from pretreated pinewood was hydrolyzed to glucose and fermented to ethanol, yielding 0.46g ethanol/(g glucose), close to the theoretical maximum yield. Copyright © 2016 The Authors. Published by Elsevier Ltd.. All rights reserved.

Program for the development of high temperature electrical materials and components

NASA Technical Reports Server (NTRS)

Neff, W. S.; Lowry, L. R.

1972-01-01

Evaluation of high temperature, space-vacuum performance of selected electrical materials and components, high temperature capacitor development, and evaluation, construction, and endurance testing of compression sealed pyrolytic boron nitride slot insulation are described. The first subject above covered the aging evaluation of electrical devices constructed from selected electrical materials. Individual materials performances were also evaluated and reported. The second subject included study of methods of improving electrical performance of pyrolytic boron nitride capacitors. The third portion was conducted to evaluate the thermal and electrical performance of pyrolytic boron nitride as stator slot liner material under varied temperature and compressive loading. Conclusions and recommendations are presented.

Catalytic pyrolysis of car tire waste using expanded perlite.

PubMed

Kar, Y

2011-08-01

In this study, the non-catalytic and catalytic pyrolysis experiments were conducted on the sample of tire waste using expanded perlite as an additive material to determine especially the effect of temperature and catalyst-to-tire ratio on the products yields and the compositions and qualities of pyrolytic oils (NCPO and CPO). Non-catalytic studies, which were carried out under the certain conditions (a nitrogen flow of 100mL/min and a heating rate of 10°C/min), showed that the highest yield of pyrolytic oil (NCPO) was 60.02wt.% at 425°C. Then, the catalytic pyrolysis studies were carried out at catalyst-to-tire ratio range of 0.05-0.25 and the highest catalytic pyrolytic oil (CPO) yield was 65.11wt.% at the ratio of 0.10 with the yield increase of 8.48wt.% compared with the non-catalytic pyrolysis. Lastly, the pyrolytic oils were characterized with applying a various techniques such as elemental analyses and various chromatographic and spectroscopic techniques (GC-MS, (1)H NMR, FT-IR, etc.). The characterization results revealed that the pyrolytic oils which were complex mixtures of C(5)-C(15) organic compounds (predominantly aromatic compounds) and also the CPO compared to the NCPO was more similar to conventional fuels in view of the certain fuel properties. Copyright © 2011 Elsevier Ltd. All rights reserved.

Recent advances in graphite powder-based electrodes.

PubMed

Bellido-Milla, Dolores; Cubillana-Aguilera, Laura Ma; El Kaoutit, Mohammed; Hernández-Artiga, Ma Purificación; Hidalgo-Hidalgo de Cisneros, José Luis; Naranjo-Rodríguez, Ignacio; Palacios-Santander, José Ma

2013-04-01

Graphite powder-based electrodes have the electrochemical performance of quasi-noble metal electrodes with intrinsic advantages related to the possibility of modification to enhance selectivity and their easily renewable surface, with no need for hazardous acids or bases for their cleaning. In contrast with commercial electrodes, for example screen-printed or sputtered-chip electrodes, graphite powder-based electrodes can also be fabricated in any laboratory with the form and characteristics desired. They are also readily modified with advanced materials, with relatively high reproducibility. All these characteristics make them a very interesting option for obtaining a large variety of electrodes to resolve different kinds of analytical problems. This review summarizes the state-of-the-art, advantages, and disadvantages of graphite powder-based electrodes in electrochemical analysis in the 21st century. It includes recent trends in carbon paste electrodes, devoting special attention to the use of emergent materials as new binders and to the development of other composite electrodes. The most recent advances in the use of graphite powder-modified sol-gel electrodes are also described. The development of sonogel-carbon electrodes and their use in electrochemical sensors and biosensors is included. These materials extend the possibilities of applications, especially for industrial technology-transfer purposes, and their development could affect not only electroanalytical green chemistry but other interesting areas also, for example catalysis and energy conversion and storage.

Adjusting the thermoelectric properties of copper(I) oxide-graphite-polymer pastes and the applications of such flexible composites.

PubMed

Andrei, Virgil; Bethke, Kevin; Rademann, Klaus

2016-04-28

We present a facile alternative to other well known strategies for synthesizing flexible thermoelectric materials. Instead of printing thin active layers on flexible substrates or doping conductive polymers, we produce thermoelectric pastes, using a mixture of graphite, copper(I) oxide and polychlorotrifluoroethene. The Seebeck coefficient of the investigated pastes varies between 10 and 600 μV K(-1), while the electrical conductivity spans over an even wider range of 10(-4) to 10(2) S m(-1). Here, the influence of phenomena such as percolation on the electrical transport is revealed. The resulting power factor reaches 5.69 × 10(-4) ± 0.70 × 10(-4) μW m(-1) K(-2) for the graphite-polymer paste, with an unexpected minimum at a graphite molar fraction of approximately 0.4. The values are comparable to those of the powder mixtures, which are slightly higher, but less precisely tunable. Such compounds are further evaluated for practical applications. The graphite-polymer paste is used to exemplify, how a flexible thermoelectric sensor can be easily manufactured, step by step. Our results represent a proof of principle, that thermoelectric pastes are viable alternatives to current solutions. A further expansion of the scope for the composites can be achieved by using high performance thermoelectric materials and conductive polymers.

Pyrolytic carbon-coated nuclear fuel

DOEpatents

Lindemer, Terrence B.; Long, Jr., Ernest L.; Beatty, Ronald L.

1978-01-01

An improved nuclear fuel kernel having at least one pyrolytic carbon coating and a silicon carbon layer is provided in which extensive interaction of fission product lanthanides with the silicon carbon layer is avoided by providing sufficient UO.sub.2 to maintain the lanthanides as oxides during in-reactor use of said fuel.

Sensitive and selective determination of Cu2+ at D-penicillamine functionalized nano-cellulose modified pencil graphite electrode

NASA Astrophysics Data System (ADS)

Taheri, M.; Ahour, F.; Keshipour, S.

2018-06-01

A novel electrochemical sensor based on D-penicillamine anchored nano-cellulose (DPA-NC) modified pencil graphite electrode was fabricated and used for highly selective and sensitive determination of copper (II) ions in the picomolar concentration by square wave adsorptive stripping voltammetric (SWV) method. The modified electrode showed better and increased SWV response compared to the bare and NC modified electrodes which may be related to the porous structure of modifier along with formation of complex between Cu2+ ions and nitrogen or oxygen containing groups in DPA-NC. Optimization of various experimental parameters influence the performance of the sensor, were investigated. Under optimized condition, DPA-NC modified electrode was used for the analysis of Cu2+ in the concentration range from 0.2 to 50 pM, and a lower detection limit of 0.048 pM with good stability, repeatability, and selectivity. Finally, the practical applicability of DPA-NC-PGE was confirmed via measuring trace amount of Cu (II) in tap and river water samples.

Calibration of High Heat Flux Sensors at NIST

PubMed Central

Murthy, A. V.; Tsai, B. K.; Gibson, C. E.

1997-01-01

An ongoing program at the National Institute of Standards and Technology (NIST) is aimed at improving and standardizing heat-flux sensor calibration methods. The current calibration needs of U.S. science and industry exceed the current NIST capability of 40 kW/m2 irradiance. In achieving this goal, as well as meeting lower-level non-radiative heat flux calibration needs of science and industry, three different types of calibration facilities currently are under development at NIST: convection, conduction, and radiation. This paper describes the research activities associated with the NIST Radiation Calibration Facility. Two different techniques, transfer and absolute, are presented. The transfer calibration technique employs a transfer standard calibrated with reference to a radiometric standard for calibrating the sensors using a graphite tube blackbody. Plans for an absolute calibration facility include the use of a spherical blackbody and a cooled aperture and sensor-housing assembly to calibrate the sensors in a low convective environment. PMID:27805156

Solvent-free fabrication of biodegradable hot-film flow sensor for noninvasive respiratory monitoring

NASA Astrophysics Data System (ADS)

Dinh, Toan; Phan, Hoang-Phuong; Nguyen, Tuan-Khoa; Qamar, Afzaal; Woodfield, Peter; Zhu, Yong; Nguyen, Nam-Trung; Viet Dao, Dzung

2017-06-01

In this paper, we report on a low-cost, environment-friendly and wearable thermal flow sensor, which can be manufactured in-house using pencil graphite as a sensing hot film and biodegradable printing paper as a substrate, without using any toxic solvents or cleanroom facilities. The hot film flow sensor offers excellent performance such as high signal-to-noise ratio (≥slant 40 for an air flow velocity of 1 m s-1), high sensitivity to airflow (53.7 mV(m s-1)-0.8) and outstanding long-term stability (almost no drift in 24 h). The sensor can be comfortably affixed to the philtrum of patients and measures human respiration in realtime. The results indicate that the wearable thermal flow sensors fabricated by this solvent-free and user-friendly method could be employed in human respiratory monitoring.

Improved Blackbody Temperature Sensors for a Vacuum Furnace

NASA Technical Reports Server (NTRS)

Farmer, Jeff; Coppens, Chris; O'Dell, J. Scott; McKechnie, Timothy N.; Schofield, Elizabeth

2009-01-01

Some improvements have been made in the design and fabrication of blackbody sensors (BBSs) used to measure the temperature of a heater core in a vacuum furnace. Each BBS consists of a ring of thermally conductive, high-melting-temperature material with two tantalum-sheathed thermocouples attached at diametrically opposite points. The name "blackbody sensor" reflects the basic principle of operation. Heat is transferred between the ring and the furnace heater core primarily by blackbody radiation, heat is conducted through the ring to the thermocouples, and the temperature of the ring (and, hence, the temperature of the heater core) is measured by use of the thermocouples. Two main requirements have guided the development of these BBSs: (1) The rings should have as high an emissivity as possible in order to maximize the heat-transfer rate and thereby maximize temperature-monitoring performance and (2) the thermocouples must be joined to the rings in such a way as to ensure long-term, reliable intimate thermal contact. The problem of fabricating a BBS to satisfy these requirements is complicated by an application-specific prohibition against overheating and thereby damaging nearby instrumentation leads through the use of conventional furnace brazing or any other technique that involves heating the entire BBS and its surroundings. The problem is further complicated by another application-specific prohibition against damaging the thin tantalum thermocouple sheaths through the use of conventional welding to join the thermocouples to the ring. The first BBS rings were made of graphite. The tantalum-sheathed thermocouples were attached to the graphite rings by use of high-temperature graphite cements. The ring/thermocouple bonds thus formed were found to be weak and unreliable, and so graphite rings and graphite cements were abandoned. Now, each BBS ring is made from one of two materials: either tantalum or a molybdenum/titanium/zirconium alloy. The tantalum-sheathed thermocouples are bonded to the ring by laser brazing. The primary advantage of laser brazing over furnace brazing is that in laser brazing, it is possible to form a brazed connection locally, without heating nearby parts to the flow temperature of the brazing material. Hence, it is possible to comply with the prohibition against overheating nearby instrumentation leads. Also, in laser brazing, unlike in furnace brazing, it is possible to exert control over the thermal energy to such a high degree that it becomes possible to braze the thermocouples to the ring without burning through the thin tantalum sheaths on the thermocouples. The brazing material used in the laser brazing process is a titanium-boron paste. This brazing material can withstand use at temperatures up to about 1,400 C. In thermal-cycling tests performed thus far, no debonding between the rings and thermocouples has been observed. Emissivity coatings about 0.001 in. (.0.025 mm) thick applied to the interior surfaces of the rings have been found to improve the performance of the BBS sensors by raising the apparent emissivities of the rings. In thermal-cycling tests, the coatings were found to adhere well to the rings.

Method for applying pyrolytic carbon coatings to small particles

DOEpatents

Beatty, Ronald L.; Kiplinger, Dale V.; Chilcoat, Bill R.

1977-01-01

A method for coating small diameter, low density particles with pyrolytic carbon is provided by fluidizing a bed of particles wherein at least 50 per cent of the particles have a density and diameter of at least two times the remainder of the particles and thereafter recovering the small diameter and coated particles.

Performance and Vibration of 30 cm Pyrolytic Ion Thruster Optics

NASA Technical Reports Server (NTRS)

Haag, Thomas; Soulas, George C.

2004-01-01

Carbon has a sputter erosion rate about an order of magnitude less than that of molybdenum, over the voltages typically used in ion thruster applications. To explore its design potential, 30 cm pyrolytic carbon ion thruster optics have been fabricated geometrically similar to the molybdenum ion optics used on NSTAR. They were then installed on an NSTAR Engineering Model thruster, and experimentally evaluated over much of the original operating envelope. Ion beam currents ranged from 0.51 to 1.76 Angstroms, at total voltages up to 1280 V. The perveance, electron back-streaming limit, and screen-grid transparency were plotted for these operating points, and compared with previous data obtained with molybdenum. While thruster performance with pyrolytic carbon was quite similar to that with molybdenum, behavior variations can reasonably be explained by slight geometric differences. Following all performance measurements, the pyrolytic carbon ion optics assembly was subjected to an abbreviated vibration test. The thruster endured 9.2 g(sub rms) of random vibration along the thrust axis, similar to DS 1 acceptance levels. Despite significant grid clashing, there was no observable damage to the ion optics assembly.

Retrofitting hetrotrophically cultivated algae biomass as pyrolytic feedstock for biogas, bio-char and bio-oil production encompassing biorefinery.

PubMed

Sarkar, Omprakash; Agarwal, Manu; Naresh Kumar, A; Venkata Mohan, S

2015-02-01

Algal biomass grown hetrotrophically in domestic wastewater was evaluated as pyrolytic feedstock for harnessing biogas, bio-oil and bio-char. Freshly harvested microalgae (MA) and lipid extracted microalgae (LEMA) were pyrolysed in packed bed reactor in the presence and absence of sand as additive. MA (without sand additive) depicted higher biogas (420 ml/g; 800 °C; 3 h) and bio-oil (0.70 ml/g; 500 °C; 3 h). Sand addition enhanced biogas production (210 ml/g; 600 °C; 2 h) in LEMA operation. The composition of bio-gas and bio-oil was found to depend on the nature of feedstock as well as the process conditions viz., pyrolytic-temperature, retention time and presence of additive. Sand additive improved the H2 composition while pyrolytic temperature increment caused a decline in CO2 fraction. Bio-char productivity increased with increasing temperature specifically with LEMA. Integration of thermo-chemical process with microalgae cultivation showed to yield multiple resources and accounts for environmental sustainability in the bio-refinery framework. Copyright © 2014 Elsevier Ltd. All rights reserved.

Overliming detoxification of pyrolytic sugar syrup for direct fermentation of levoglucosan to ethanol.

PubMed

Chi, Zhanyou; Rover, Marjorie; Jun, Erin; Deaton, Mark; Johnston, Patrick; Brown, Robert C; Wen, Zhiyou; Jarboe, Laura R

2013-12-01

The application of pyrolytic sugars for biofuel production through fermentation is challenged by inhibitory contaminant compounds. Inhibition is so severe that only 0.25% sugar syrup can be used. In this study, overliming was tested as a simple detoxification method, using the Escherichia coli KO11+ lgk to directly convert levoglucosan into ethanol. After treatment with at least 14.8 g/L of Ca(OH)2, fermentation with 2% (w/v) pyrolytic sugar syrup was observed with no inhibition of ethanol production. Further investigation of treatment time and temperature showed that 8-16 h of treatment at 20°C, and 1-4 h of treatment at 60°C are necessary to obtain consistent ethanol production. The samples treated with 18.5 g/L Ca(OH)2 at 60°C for 4 h showed no inhibition at 2.5%. Multiple contaminants removed by the overliming treatment were identified. This study demonstrates that overliming is a promising method for detoxification of pyrolytic sugars for fermentation. Copyright © 2013 Elsevier Ltd. All rights reserved.

Influence of Inner Transducer Properties on EMF Response and Stability of Solid-Contact Anion Selective Membrane Electrodes Based on Metalloporphyrin Ionophores

PubMed Central

Górski, Łukasz; Matusevich, Alexey; Pietrzak, Mariusz; Wang, Lin; Meyerhoff, Mark E.; Malinowska, Elżbieta

2010-01-01

The performance of solid-contact/coated wire type electrodes with plasticized PVC membranes containing metalloporphyrins as anion selective ionophores is reported. The membranes are deposited on transducers based on graphite pastes and graphite rods. The hydrophobicity of the underlying conductive transducer surface is found to be a key factor that influences the formation of an aqueous layer beneath the polymer film. Elimination of this ill-defined water layer greatly improves the electrochemical properties of the ion-sensors, such as EMF stability and life-time. Only highly lipophilic electrode substrates, namely graphite paste with mineral oil, were shown to prevent the formation of aqueous layer underneath the ion-sensing membrane. The possibility of employing Co(III)-tetraphenylporphyrin both as NO2− selective ionophore and as electron/ion conducting species to ensure ion-to-electron translation was also discussed based on the results of preliminary experiments. PMID:20357903

High viscosity environments: an unexpected route to obtain true atomic resolution with atomic force microscopy.

PubMed

Weber, Stefan A L; Kilpatrick, Jason I; Brosnan, Timothy M; Jarvis, Suzanne P; Rodriguez, Brian J

2014-05-02

Atomic force microscopy (AFM) is widely used in liquid environments, where true atomic resolution at the solid-liquid interface can now be routinely achieved. It is generally expected that AFM operation in more viscous environments results in an increased noise contribution from the thermal motion of the cantilever, thereby reducing the signal-to-noise ratio (SNR). Thus, viscous fluids such as ionic and organic liquids have been generally avoided for high-resolution AFM studies despite their relevance to, e.g. energy applications. Here, we investigate the thermal noise limitations of dynamic AFM operation in both low and high viscosity environments theoretically, deriving expressions for the amplitude, phase and frequency noise resulting from the thermal motion of the cantilever, thereby defining the performance limits of amplitude modulation, phase modulation and frequency modulation AFM. We show that the assumption of a reduced SNR in viscous environments is not inherent to the technique and demonstrate that SNR values comparable to ultra-high vacuum systems can be obtained in high viscosity environments under certain conditions. Finally, we have obtained true atomic resolution images of highly ordered pyrolytic graphite and mica surfaces, thus revealing the potential of high-resolution imaging in high viscosity environments.

Ultraviolet photoelectron spectroscopy reveals energy-band dispersion for π-stacked 7,8,15,16-tetraazaterrylene thin films in a donor–acceptor bulk heterojunction

NASA Astrophysics Data System (ADS)

Aghdassi, Nabi; Wang, Qi; Ji, Ru-Ru; Wang, Bin; Fan, Jian; Duhm, Steffen

2018-05-01

7,8,15,16-tetraazaterrylene (TAT) thin films grown on highly oriented pyrolytic graphite (HOPG) substrates were studied extensively with regard to their intrinsic and interfacial electronic properties by means of ultraviolet photoelectron spectroscopy (UPS). Merely weak substrate–adsorbate interaction occurs at the TAT/HOPG interface, with interface energetics being only little affected by the nominal film thickness. Photon energy-dependent UPS performed perpendicular to the molecular planes of TAT multilayer films at room temperature clearly reveals band-like intermolecular dispersion of the TAT highest occupied molecular orbital (HOMO) energy. Based on a comparison with a tight-binding model, a relatively narrow bandwidth of 54 meV is derived, which points to the presence of an intermediate regime between hopping and band-like hole transport. Upon additional deposition of 2,2‧:5‧,2″:5″,2″‧-quaterthiophene (4T), a 4T:TAT donor–acceptor bulk heterojunction with a considerable HOMO-level offset at the donor–acceptor interface is formed. The 4T:TAT bulk heterojunction likewise exhibits intermolecular dispersion of the TAT HOMO energy, yet with a significant decreased bandwidth.

Development of Passive Fuel Cell Thermal Management Technology

NASA Technical Reports Server (NTRS)

Burke, Kenneth A.; Jakupca, Ian; Colozza, Anthony

2011-01-01

The NASA Glenn Research Center is developing advanced passive thermal management technology to reduce the mass and improve the reliability of space fuel cell systems for the NASA exploration program. The passive thermal management system relies on heat conduction within the cooling plate to move the heat from the central portion of the cell stack out to the edges of the fuel cell stack rather than using a pumped loop cooling system to convectively remove the heat. Using the passive approach eliminates the need for a coolant pump and other cooling loop components which reduces fuel cell system mass and improves overall system reliability. Previous analysis had identified that low density, ultra-high thermal conductivity materials would be needed for the cooling plates in order to achieve the desired reductions in mass and the highly uniform thermal heat sink for each cell within a fuel cell stack. A pyrolytic graphite material was identified and fabricated into a thin plate using different methods. Also a development project with Thermacore, Inc. resulted in a planar heat pipe. Thermal conductivity tests were done using these materials. The results indicated that lightweight passive fuel cell cooling is feasible.

Surface science approach to Pt/carbon model catalysts: XPS, STM and microreactor studies

NASA Astrophysics Data System (ADS)

Motin, Abdul Md.; Haunold, Thomas; Bukhtiyarov, Andrey V.; Bera, Abhijit; Rameshan, Christoph; Rupprechter, Günther

2018-05-01

Pt nanoparticles supported on carbon are an important technological catalyst. A corresponding model catalyst was prepared by physical vapor deposition (PVD) of Pt on sputtered HOPG (highly oriented pyrolytic graphite). The carbon substrate before and after sputtering as well as the Pt/HOPG system before and after Pt deposition and annealing were examined by XPS and STM. This yielded information on the surface density of defects, which serve as nucleation centres for Pt, and on the size distribution (mean size/height) of the Pt nanoparticles. Two different model catalysts were prepared with mean sizes of 2.0 and 3.6 nm, both turned out to be stable upon UHV-annealing to 300 °C. After transfer into a UHV-compatible flow microreactor and subsequent cleaning in UHV and under mbar pressure, the catalytic activity of the Pt/HOPG model system for ethylene hydrogenation was examined under atmospheric pressure flow conditions. This enabled to determine temperature-dependent conversion rates, turnover frequencies (TOFs) and activation energies. The catalytic results obtained are in line with the characteristics of technological Pt/C, demonstrating the validity of the current surface science based model catalyst approach.

Covalent Attachment of the Water-insoluble Ni(P Cy 2 N Phe 2 ) 2 Electrocatalyst to Electrodes Showing Reversible Catalysis in Aqueous Solution

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

Rodríguez-Maciá, Patricia; Priyadarshani, Nilusha; Dutta, Arnab

Hydrogenases are a diverse group of metalloenzymes which catalyze the reversible conversion between molecular hydrogen and protons at high rates. The catalytic activity of these enzymes does not require overpotential because their active site has been evolutionarily optimized to operate fast and efficiently. These enzymes have inspired the development of molecular catalysts, which have dramatically improved in efficiency in recent years, to the point that some synthetic catalysts even outperform hydrogenases under certain conditions. In this work, we use a reversible noble-metal-free homogeneous catalyst, the [Ni(PCy2NPhe2)2]2+ complex, and we covalently immobilize it on a functionalized highly oriented pyrolytic graphite “edge”more » (HOPGe) electrode surface. This catalyst is not water soluble, but once it is surface-confined on the electrode, it maintains its catalytic properties in aqueous solutions, showing reversibility for H2 oxidation/reduction. Immobilization of the [Ni(PCy2NPhe2)2]2+ complex onto a multi-walled carbon nanotubes coated electrode leads to even higher catalytic current densities and enhanced stability.« less

Field-assisted nanopatterning of metals, metal oxides and metal salts

NASA Astrophysics Data System (ADS)

Liu, Jun-Fu; Miller, Glen P.

2009-02-01

The tip-based nanofabrication method called field-assisted nanopatterning or FAN has now been extended to the transfer of metals, metal oxides and metal salts onto various receiving substrates including highly ordered pyrolytic graphite, passivated gold and indium-tin oxide. Standard atomic force microscope tips were first dip-coated using suspensions of inorganic compounds in solvent. The films prepared in this manner were non-uniform and contained inorganic nanoparticles. Tip-based nanopatterning on chosen substrates was conducted under high electric field conditions. The same tip was used for both nanofabrication and imaging. Arbitrary patterns were formed with dimensions that ranged from tens of microns to sub-20 nm and were controlled by tuning the tip bias during fabrication. Most tip-based nanopatterning techniques are limited in terms of the type of species that can be deposited and the type of substrates onto which the deposition occurs. With the successful deposition of inorganic species reported here, FAN is demonstrated to be a truly versatile tip-based nanofabrication technique that is useful for the deposition of a wide variety of both organic and inorganic species including small molecules, large molecules and polymers.

High viscosity environments: an unexpected route to obtain true atomic resolution with atomic force microscopy

NASA Astrophysics Data System (ADS)

Weber, Stefan A. L.; Kilpatrick, Jason I.; Brosnan, Timothy M.; Jarvis, Suzanne P.; Rodriguez, Brian J.

2014-05-01

Atomic force microscopy (AFM) is widely used in liquid environments, where true atomic resolution at the solid-liquid interface can now be routinely achieved. It is generally expected that AFM operation in more viscous environments results in an increased noise contribution from the thermal motion of the cantilever, thereby reducing the signal-to-noise ratio (SNR). Thus, viscous fluids such as ionic and organic liquids have been generally avoided for high-resolution AFM studies despite their relevance to, e.g. energy applications. Here, we investigate the thermal noise limitations of dynamic AFM operation in both low and high viscosity environments theoretically, deriving expressions for the amplitude, phase and frequency noise resulting from the thermal motion of the cantilever, thereby defining the performance limits of amplitude modulation, phase modulation and frequency modulation AFM. We show that the assumption of a reduced SNR in viscous environments is not inherent to the technique and demonstrate that SNR values comparable to ultra-high vacuum systems can be obtained in high viscosity environments under certain conditions. Finally, we have obtained true atomic resolution images of highly ordered pyrolytic graphite and mica surfaces, thus revealing the potential of high-resolution imaging in high viscosity environments.

Method of making carbon-carbon composites

DOEpatents

Engle, Glen B.

1991-01-01

A process for making a carbon-carbon composite having a combination of high crystallinity, high strength, high modulus and high thermal and electrical conductivity. High-modulus/high-strength mesophase derived carbon fibers are woven into a suitable cloth. Layers of this easily graphitizable woven cloth are covered with petroleum or coal tar pitch and pressed at a temperature a few degrees above the softening point of the pitch to form a green laminated composite. The green composite is restrained in a suitable fixture and heated slowly to carbonize the pitch binder. The carbonized composite is then impregnated several times with pitch by covering the composite with hot pitch under pressure. The composites are given a heat treatment between each impregnation step to crack up the infiltrated carbon and allow additional pitch to enter the microstructure during the next impregnation cycle. The impregnated composites are then given a final heat treatment in the range 2500.degree. to 3000.degree. C. to fully graphitize the fibers and the matrix carbon. The composites are then infiltrated with pyrolytic carbon by chemical vapor deposition in the range 1000.degree. to 1300.degree. C. at a reduced pressure for approximately one hundred and fifty (150) hours.

Preparation of monolayers of [MnIII 6CrIII]3+ single-molecule magnets on HOPG, mica and silicon surfaces and characterization by means of non-contact AFM

NASA Astrophysics Data System (ADS)

Gryzia, Aaron; Predatsch, Hans; Brechling, Armin; Hoeke, Veronika; Krickemeyer, Erich; Derks, Christine; Neumann, Manfred; Glaser, Thorsten; Heinzmann, Ulrich

2011-08-01

We report on the characterization of various salts of [ Mn III 6 Cr III ] 3+ complexes prepared on substrates such as highly oriented pyrolytic graphite (HOPG), mica, SiO2, and Si3N4. [ Mn III 6 Cr III ] 3+ is a single-molecule magnet, i.e., a superparamagnetic molecule, with a blocking temperature around 2 K. The three positive charges of [ Mn III 6 Cr III ] 3+ were electrically neutralized by use of various anions such as tetraphenylborate (BPh4 -), lactate (C3H5O3 -), or perchlorate (ClO4 -). The molecule was prepared on the substrates out of solution using the droplet technique. The main subject of investigation was how the anions and substrates influence the emerging surface topology during and after the preparation. Regarding HOPG and SiO2, flat island-like and hemispheric-shaped structures were created. We observed a strong correlation between the electronic properties of the substrate and the analyzed structures, especially in the case of mica where we observed a gradient in the analyzed structures across the surface.

Pectin-Lipid Self-Assembly: Influence on the Formation of Polyhydroxy Fatty Acids Nanoparticles

PubMed Central

Guzman-Puyol, Susana; Benítez, José Jesús; Domínguez, Eva; Bayer, Ilker Sefik; Cingolani, Roberto; Athanassiou, Athanassia; Heredia, Antonio; Heredia-Guerrero, José Alejandro

2015-01-01

Nanoparticles, named cutinsomes, have been prepared from aleuritic (9,10,16-trihidroxipalmitic) acid and tomato fruit cutin monomers (a mixture of mainly 9(10),16-dihydroxypalmitic acid (85%, w/w) and 16-hydroxyhexadecanoic acid (7.5%, w/w)) with pectin in aqueous solution. The process of formation of the nanoparticles of aleuritic acid plus pectin has been monitored by UV-Vis spectrophotometry, while their chemical and morphological characterization was analyzed by ATR-FTIR, TEM, and non-contact AFM. The structure of these nanoparticles can be described as a lipid core with a pectin shell. Pectin facilitated the formation of nanoparticles, by inducing their aggregation in branched chains and favoring the condensation between lipid monomers. Also, pectin determined the self-assembly of cutinsomes on highly ordered pyrolytic graphite (HOPG) surfaces, causing their opening and forming interconnected structures. In the case of cutin monomers, the nanoparticles are fused, and the condensation of the hydroxy fatty acids is strongly affected by the presence of the polysaccharide. The interaction of pectin with polyhydroxylated fatty acids could be related to an initial step in the formation of the plant biopolyester cutin. PMID:25915490

Ultraviolet photoelectron spectroscopy reveals energy-band dispersion for π-stacked 7,8,15,16-tetraazaterrylene thin films in a donor-acceptor bulk heterojunction.

PubMed

Aghdassi, Nabi; Wang, Qi; Ji, Ru-Ru; Wang, Bin; Fan, Jian; Duhm, Steffen

2018-05-11

7,8,15,16-tetraazaterrylene (TAT) thin films grown on highly oriented pyrolytic graphite (HOPG) substrates were studied extensively with regard to their intrinsic and interfacial electronic properties by means of ultraviolet photoelectron spectroscopy (UPS). Merely weak substrate-adsorbate interaction occurs at the TAT/HOPG interface, with interface energetics being only little affected by the nominal film thickness. Photon energy-dependent UPS performed perpendicular to the molecular planes of TAT multilayer films at room temperature clearly reveals band-like intermolecular dispersion of the TAT highest occupied molecular orbital (HOMO) energy. Based on a comparison with a tight-binding model, a relatively narrow bandwidth of 54 meV is derived, which points to the presence of an intermediate regime between hopping and band-like hole transport. Upon additional deposition of 2,2':5',2″:5″,2″'-quaterthiophene (4T), a 4T:TAT donor-acceptor bulk heterojunction with a considerable HOMO-level offset at the donor-acceptor interface is formed. The 4T:TAT bulk heterojunction likewise exhibits intermolecular dispersion of the TAT HOMO energy, yet with a significant decreased bandwidth.

MISSE 2 PEACE Polymers Experiment Atomic Oxygen Erosion Yield Error Analysis

NASA Technical Reports Server (NTRS)

McCarthy, Catherine E.; Banks, Bruce A.; deGroh, Kim, K.

2010-01-01

Atomic oxygen erosion of polymers in low Earth orbit (LEO) poses a serious threat to spacecraft performance and durability. To address this, 40 different polymer samples and a sample of pyrolytic graphite, collectively called the PEACE (Polymer Erosion and Contamination Experiment) Polymers, were exposed to the LEO space environment on the exterior of the International Space Station (ISS) for nearly 4 years as part of the Materials International Space Station Experiment 1 & 2 (MISSE 1 & 2). The purpose of the PEACE Polymers experiment was to obtain accurate mass loss measurements in space to combine with ground measurements in order to accurately calculate the atomic oxygen erosion yields of a wide variety of polymeric materials exposed to the LEO space environment for a long period of time. Error calculations were performed in order to determine the accuracy of the mass measurements and therefore of the erosion yield values. The standard deviation, or error, of each factor was incorporated into the fractional uncertainty of the erosion yield for each of three different situations, depending on the post-flight weighing procedure. The resulting error calculations showed the erosion yield values to be very accurate, with an average error of 3.30 percent.

Nucleation and growth kinetics for intercalated islands during deposition on layered materials with isolated pointlike surface defects

DOE PAGES

Han, Yong; Lii-Rosales, A.; Zhou, Y.; ...

2017-10-13

Theory and stochastic lattice-gas modeling is developed for the formation of intercalated metal islands in the gallery between the top layer and the underlying layer at the surface of layered materials. Our model for this process involves deposition of atoms, some fraction of which then enter the gallery through well-separated pointlike defects in the top layer. Subsequently, these atoms diffuse within the subsurface gallery leading to nucleation and growth of intercalated islands nearby the defect point source. For the case of a single point defect, continuum diffusion equation analysis provides insight into the nucleation kinetics. However, complementary tailored lattice-gas modelingmore » produces a more comprehensive and quantitative characterization. We analyze the large spread in nucleation times and positions relative to the defect for the first nucleated island. We also consider the formation of subsequent islands and the evolution of island growth shapes. The shapes reflect in part our natural adoption of a hexagonal close-packed island structure. As a result, motivation and support for the model is provided by scanning tunneling microscopy observations of the formation of intercalated metal islands in highly-ordered pyrolytic graphite at higher temperatures.« less

P(VDF/TrFE) morphologies and crystalline lamellae orientations dependence on substrates characterized by scanning probe microscopy

NASA Astrophysics Data System (ADS)

Lakbita, Imane; El-Hami, Khalil

2018-02-01

Ultra-thin films of the polyvinylidene fluoride and trifluoroethylene (P(VDF/TrFE)) copolymer were elaborated on various different substrates by the spin coating method. The purpose of this paper is to study the P(VDF/TrFE) morphologies and crystalline lamellae orientation dependence on substrates. We chose the potassium chloride (KCl), Sodium Chloride (NaCl) and Potassium Bromide (KBr) with the [110] direction and the highly ordered pyrolytic graphite (HOPG) substrates because they present different crystallographic structures. The atomic force microscopy is used for imaging P(VDF/TrFE) morphologies with nanometer resolution and determining the surface roughness. The analysis of the AFM topography images revealed that the P(VDF/TrFE) film has, almost, the same texture on KCl, NaCl or on KBr substrates and their crystalline lamellae had grown in two preferred orientations. Unlike the HOPG substrate, their crystalline lamellae were entangled, randomly oriented and positioned adjacent to each other. The growth texture of the P(VDF/TrFE) copolymer showed experimentally a strong dependence on substrate types. Since the P(VDF/TrFE) is ferroelectric, piezoelectric and pyroelectric, this finding may lead to potential applications.

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

Oloff, L.-P., E-mail: oloff@physik.uni-kiel.de; Hanff, K.; Stange, A.

With the advent of ultrashort-pulsed extreme ultraviolet sources, such as free-electron lasers or high-harmonic-generation (HHG) sources, a new research field for photoelectron spectroscopy has opened up in terms of femtosecond time-resolved pump-probe experiments. The impact of the high peak brilliance of these novel sources on photoemission spectra, so-called vacuum space-charge effects caused by the Coulomb interaction among the photoemitted probe electrons, has been studied extensively. However, possible distortions of the energy and momentum distributions of the probe photoelectrons caused by the low photon energy pump pulse due to the nonlinear emission of electrons have not been studied in detail yet.more » Here, we systematically investigate these pump laser-induced space-charge effects in a HHG-based experiment for the test case of highly oriented pyrolytic graphite. Specifically, we determine how the key parameters of the pump pulse—the excitation density, wavelength, spot size, and emitted electron energy distribution—affect the measured time-dependent energy and momentum distributions of the probe photoelectrons. The results are well reproduced by a simple mean-field model, which could open a path for the correction of pump laser-induced space-charge effects and thus toward probing ultrafast electron dynamics in strongly excited materials.« less

Nano-structured variable capacitor based on P(VDF-TrFE) copolymer and carbon nanotubes

NASA Astrophysics Data System (ADS)

Lakbita, I.; El-Hami, K.

2018-02-01

A newly organic capacitor was conceived with a variable capacitance using the inverse piezoelectric effect. The device consists of two parallel plates of carbon nanotubes (CNTs), known for their large surface area, high sensitivity and high electric conductivity, separated by a thin film of a dielectric layer of Polyinylidene fluoride and trifluoroehtylene (P(VDF-TrFE)) promising material for piezoelectric and ferroelectric properties. The obtained architecture is the CNT/PVDF-TrFE/CNT capacitor device. In this study, an ultra-thin film of P(VDF-TrFE) (54/46) with thickness of 20 nm was elaborated on highly oriented pyrolytic graphite (HOPG) by spin-coating. The morphology of the ultra-thin film and the mechanical behavior of CNT/P(VDF-TrFE)/CNT system were studied using the atomic force microscopy (AFM) combined with a lock-in amplifier in contact mode. All changes in applied voltage induce a change in thin film thickness according to the inverse piezoelectric effect that affect, consequently the capacitance. The results showed that the ratio of capacitance change ΔC to initial capacitance C0 is ΔC/C0=5%. This value is sufficient to use P(VDF-TrFE) as variable organic capacitor.

Fabrication and Evaluation of a Graphene Oxide-Based Capacitive Humidity Sensor.

PubMed

Feng, Jinfeng; Kang, Xiaoxu; Zuo, Qingyun; Yuan, Chao; Wang, Weijun; Zhao, Yuhang; Zhu, Limin; Lu, Hanwei; Chen, Juying

2016-03-01

In this study, a CMOS compatible capacitive humidity sensor structure was designed and fabricated on a 200 mm CMOS BEOL Line. A top Al interconnect layer was used as an electrode with a comb/serpent structure, and graphene oxide (GO) was used as sensing material. XRD analysis was done which shows that GO sensing material has a strong and sharp (002) peak at about 10.278°, whereas graphite has (002) peak at about 26°. Device level CV and IV curves were measured in mini-environments at different relative humidity (RH) level, and saturated salt solutions were used to build these mini-environments. To evaluate the potential value of GO material in humidity sensor applications, a prototype humidity sensor was designed and fabricated by integrating the sensor with a dedicated readout ASIC and display/calibration module. Measurements in different mini-environments show that the GO-based humidity sensor has higher sensitivity, faster recovery time and good linearity performance. Compared with a standard humidity sensor, the measured RH data of our prototype humidity sensor can match well that of the standard product.

An ultrasensitive electrochemiluminescent sensor based on a pencil graphite electrode modified with CdS nanorods for detection of chlorogenic acid in honeysuckle.

PubMed

Zheng, Ruijuan; Zhong, Jianhai; Zhao, Chenhao; Lang, Xiaoling; Hu, Zhibiao; Luo, Jiangshui

2017-08-01

In this paper, a novel and ultrasensitive electrochemiluminescent sensor employing a solvothermal-synthesized CdS nanorod-modified pencil graphite electrode (CdS/PGE) for the determination of chlorogenic acid (CA) is fabricated. In the first step, the PGE surface is modified using CdS nanorods. In the next step, the developed electrode is used to detect CA using a electrochemiluminescent (ECL) technique, in which potassium persulfate (K 2 S 2 O 8 ) served as a co-reactant. The possible ECL mechanism is investigated, and the influences of pH and cyclic voltammetric scanning rate on the signal response are studied. The ECL intensity decreases quantitatively in relation to the concentration of the target molecule. Under optimized conditions, the linear correlation between the quenched ECL intensity and the logarithm of CA concentration is observed in the range from 2 × 10 -9 to 8 × 10 -7  mol L -1 with a limit of detection of 1 × 10 -9  mol L -1 . This proposed method is applied to the analysis of CA in honeysuckle flower, giving recoveries of 99-107%. The experimental results demonstrate that this ECL sensor shows good stability and reproducibility. Copyright © 2016 John Wiley & Sons, Ltd.

Nanocarbon: Defect Architectures and Properties

NASA Astrophysics Data System (ADS)

Vuong, Amanda

The allotropes of carbon make its solid phases amongst the most diverse of any element. It can occur naturally as graphite and diamond, which have very different properties that make them suitable for a wide range of technological and commercial purposes. Recent developments in synthetic carbon include Highly Oriented Pyrolytic Graphite (HOPG) and nano-carbons, such as fullerenes, nanotubes and graphene. The main industrial application of bulk graphite is as an electrode material in steel production, but in purified nuclear graphite form, it is also used as a moderator in Advanced Gas-cooled Reactors across the United Kingdom. Both graphene and graphite are damaged over time when subjected to bombardment by electrons, neutrons or ions, and these have a wide range of effects on their physical and electrical properties, depending on the radiation flux and temperature. This research focuses on intrinsic defects in graphene and dimensional change in nuclear graphite. The method used here is computational chemistry, which complements physical experiments. Techniques used comprise of density functional theory (DFT) and molecular dynamics (MD), which are discussed in chapter 2 and chapter 3, respectively. The succeeding chapters describe the results of simulations performed to model defects in graphene and graphite. Chapter 4 presents the results of ab initio DFT calculations performed to investigate vacancy complexes that are formed in AA stacked bilayer graphene. In AB stacking, carbon atoms surrounding the lattice vacancies can form interlayer structures with sp2 bonding that are lower in energy compared to in-plane reconstructions. From the investigation of AA stacking, sp2 interlayer bonding of adjacent multivacancy defects in registry creates a type of stable sp2 bonded wormhole between the layers. Also, a new class of mezzanine structure characterised by sp3 interlayer bonding, resembling a prismatic vacancy loop has also been identified. The mezzanine, which is a V6 hexavacancy variant, where six sp3 carbon atoms sit midway between two carbon layers and bond to both, is substantially more stable than any other vacancy aggregate in AA stacked layers. Chapter 5 presents the results of ab initio DFT calculations performed to investigate the wormhole and mezzanine defect that were identified in chapter 4 and the ramp defect discovered by Trevethan et al.. DFT calculations were performed on these defects in twisted bilayer graphene. From the investigation of vacancy complexes in twisted bilayer graphene, it is found that vacancy complexes are unstable in the twisted region and are more favourable in formation energy when the stacking arrangement is close to AA or AB stacking. It has also been discovered that the ramp defect is more stable in the twisted bilayer graphene compared to the mezzanine defect. Chapter 6 presents the results of ab initio DFT calculations performed to investigate a form of extending defect, prismatic edge dislocation. Suarez-Martinez et al.'s research suggest the armchair core is disconnected from any other layer, whilst the zigzag core is connected. In the investigation here, the curvature of the mezzanine defect allows it to swing between the armchair, zigzag and Klein in the AA stacking. For the AB stacking configuration, the armchair and zigzag core are connected from any other layer. Chapter 7 present results of MD simulations using the adaptive intermolecular reactive empirical bond order (AIREBO) potential to investigate the dimensional change of graphite due to the formation of vacancies present in a single crystal. It has been identified that there is an expansion along the c-axis, whilst a contraction along the a- and b- axes due to the coalescence of vacancy forming in-plane and between the layers. The results here are in good agreement with experimental studies of low temperature irradiation. The final chapter gives conclusions to this work.

Comparative study on pyrolysis of lignocellulosic and algal biomass using pyrolysis-gas chromatography/mass spectrometry.

PubMed

Li, Kai; Zhang, Liqiang; Zhu, Liang; Zhu, Xifeng

2017-06-01

The cornstalk and chlorella were selected as the representative of lignocelulosic and algal biomass, and the pyrolysis experiments of them were carried out using pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS). The physicochemical properties of samples and the pyrolytic product distribution were presented. And then the compositional differences between the two kinds of pyrolytic products were studied, the relevant pyrolysis mechanisms were analyzed systematically. Pyrolytic vapor from lignocellulosic biomass contained more phenolic and carbonyl compounds while that from algal biomass contained more long-chain fatty acids, nitrogen-containing compounds and fewer carbonyl compounds. Maillard reaction is conducive to the conversion of carbonyl compounds to nitrogenous heterocyclic compounds with better thermal stability. Copyright © 2017 Elsevier Ltd. All rights reserved.

Multi-functional laser fabrication of diamond (Conference Presentation)

NASA Astrophysics Data System (ADS)

Salter, Patrick S.; Booth, Martin J.

2017-03-01

Ultrafast laser fabrication enables micro-structuring of diamond in 3D with a range of functionality. An ultrashort pulsed beam focused beneath the diamond surface induces structural modifications which are highly localised in three dimensions. At high pulse energy, the laser breaks down the diamond lattice at focus to form a graphitic phase. We demonstrate high resolution analysis of the structural changes revealing the graphitic phase to be formed of small clusters ( 100 nm in size) of amorphous sp2 bonded carbon accompanied by localised cracking of the diamond. When the laser focus is traced through the diamond, continuous graphitic wires are created which are electrically conductive. We have used such wires to fabricate large-area 3D radiation sensors which have been employed for the detection of high energy protons. Such graphitic wires have an associated stress field and a related localised modulation of the refractive index. We have recently written combinations of graphitic tracks in diamond to engineer stress fields to give a desired refractive index distribution and form an optical waveguide. Type III waveguides are demonstrated that allow guiding of both polarization states. We also show that by reducing the laser pulse energy, it is possible to avoid complete breakdown of the diamond lattice and simply introduce an ensemble of vacancies within the focal volume. This can be used to create single coherent NV centres in diamond isolated in 3D. All these processes are improved by processing at high numerical aperture (NA), for which adaptive optics aberration correction is essential.

Magnified fluorescence detection of silver(I) ion in aqueous solutions by using nano-graphite-DNA hybrid and DNase I.

PubMed

Wei, Yin; Li, Bianmiao; Wang, Xu; Duan, Yixiang

2014-08-15

This paper describes a novel approach utilizing nano-graphite-DNA hybrid and DNase I for the amplified detection of silver(I) ion in aqueous solutions for the first time. Nano-graphite can effectively quench the fluorescence of dye-labeled cytosine-rich single-stranded DNA due to its strong π-π stacking interactions; however, in the presence of Ag(+), C-Ag(+)-C coordination induces the probe to fold into a hairpin structure, which does not adsorb on the surface of nano-graphite and thus retains the dye fluorescence. Meanwhile, the hairpin structure can be cleaved by DNase I, and in such case Ag(+) is delivered from the complex. The released Ag(+) then binds other dye-labeled single-stranded DNA on the nano-graphite surface, and touches off another target recycling, resulting in the successive release of dye-labeled single-stranded DNA from the nano-graphite, which leads to significant amplification of the signal. The present magnification sensing system exhibits high sensitivity toward Ag(+) with a limit of detection of 0.3nM (S/N=3), which is much lower than the standard for Ag(+) in drinking water recommended by the Environmental Protection Agency (EPA). The selectivity of the sensor for Ag(+) against other biologically and environmentally related metal ions is outstanding due to the high specificity of C-Ag(+)-C formation. Moreover, the sensing system is used for the determination of Ag(+) in river water samples with satisfying results. The proposed assay is simple, cost-effective, and might open the door for the development of new assays for other metal ions or biomolecules. Copyright © 2014 Elsevier B.V. All rights reserved.

Molecular modeling of interactions in electronic nose sensors for environmental monitoring

NASA Technical Reports Server (NTRS)

Shevade, A. V.; Ryan, M. A.; Homer, M. L.; Manfreda, A. M.; Yen, S. -P. S.; Zhou, H.; Manatt, K.

2002-01-01

We report a study aimed at understanding analyte interactions with sensors made from polymer-carbon black composite films. The sensors are used in an Electronic Nose (ENose) which is used for monitoring the breathing air quality in human habitats. The model mimics the experimental conditions of the composite film deposition and formation and was developed using molecular modeling and simulation tools. The Dreiding 2.21 Force Field was used for the polymer and analyte molecules while graphite parameters were assigned to the carbon black atoms. The polymer considered for this work is methyl vinyl ether / maleic acid copolymer. The target analytes include both inorganic (NH3) and organic (methanol) types of compound. Results indicate different composite-analyte interaction behavior.

Graphene-like 2D nanomaterial-based biointerfaces for biosensing applications.

PubMed

Zhu, Chengzhou; Du, Dan; Lin, Yuehe

2017-03-15

Due to their unique structures and multifunctionalities, two-dimensional (2D) nanomaterials have aroused increasing interest in the construction of the novel biointerfaces for biosensing applications. Efforts in constructing novel biointerfaces led to exploit the more versatile and tunable graphene-like 2D nanomaterials (e.g. graphitic carbon nitride, boron nitride, transition metal dichalcogenides, and transition metal oxides) with various structural and compositional characteristics. This review highlights recent efforts in the design of graphene-like 2D nanomaterials and their derived biointerfaces and exploitation of their research on fluorescent sensors and a series of electrochemical sensors, including amperometric, electrochemiluminescence, photoelectrochemical and field-effect transistor sensors. Finally, we discuss some critical challenges and future perspectives in this field. Copyright © 2016. Published by Elsevier B.V.

Acoustic emission evaluation of reinforced concrete bridge beam with graphite composite laminate

NASA Astrophysics Data System (ADS)

Johnson, Dan E.; Shen, H. Warren; Finlayson, Richard D.

2001-07-01

A test was recently conducted on August 1, 2000 at the FHwA Non-Destructive Evaluation Validation Center, sponsored by The New York State DOT, to evaluate a graphite composite laminate as an effective form of retrofit for reinforced concrete bridge beam. One portion of this testing utilized Acoustic Emission Monitoring for Evaluation of the beam under test. Loading was applied to this beam using a two-point loading scheme at FHwA's facility. This load was applied in several incremental loadings until the failure of the graphite composite laminate took place. Each loading culminated by either visual crack location or large audible emissions from the beam. Between tests external cracks were located visually and highlighted and the graphite epoxy was checked for delamination. Acoustic Emission data was collected to locate cracking areas of the structure during the loading cycles. To collect this Acoustic Emission data, FHwA and NYSDOT utilized a Local Area Monitor, an Acoustic Emission instrument developed in a cooperative effort between FHwA and Physical Acoustics Corporation. Eight Acoustic Emission sensors were attached to the structure, with four on each side, in a symmetrical fashion. As testing progressed and culminated with beam failure, Acoustic Emission data was gathered and correlated against time and test load. This paper will discuss the analysis of this test data.

Pyrolytic-carbon coating in carbon nanotube foams for better performance in supercapacitors

NASA Astrophysics Data System (ADS)

He, Nanfei; Yildiz, Ozkan; Pan, Qin; Zhu, Jiadeng; Zhang, Xiangwu; Bradford, Philip D.; Gao, Wei

2017-03-01

Nowadays, the wide-spread adoption of supercapacitors has been hindered by their inferior energy density to that of batteries. Here we report the use of our pyrolytic-carbon-coated carbon nanotube foams as lightweight, compressible, porous, and highly conductive current collectors in supercapacitors, which are infiltrated with chemically-reduced graphene oxide and later compressed via mechanical and capillary forces to generate the active electrodes. The pyrolytic carbon coatings, introduced by chemical vapor infiltration, wrap around the CNT junctions and increase the surface roughness. When active materials are infiltrated, the pyrolytic-carbon coatings help prevent the π-stacking, enlarge the accessible surface area, and increase the electrical conductivity of the scaffold. Our best-performing device offers 48% and 57% higher gravimetric energy and power density, 14% and 23% higher volumetric energy and power density, respectively, and two times higher knee frequency, than the device with commercial current collectors, while the "true-performance metrics" are strictly followed in our measurements. We have further clarified the solution resistance, charge transfer resistance/capacitance, double-layer capacitance, and Warburg resistance in our system via comprehensive impedance analysis, which will shed light on the design and optimization of similar systems.

Formation of the reduced form of furaneol® (2,5-dimethyl-4-hydroxy-tetrahydrofuran-3-one) during the Maillard reaction through catalysis of amino acid metal salts.

PubMed

Nashalian, Ossanna; Wang, Xi; Yaylayan, Varoujan A

2016-11-01

Under pyrolytic conditions the acidity/basicity of Maillard reaction mixtures can be controlled through the use of hydrochloride or sodium salts of amino acids to generate a diversity of products. When the degradation of glucose was studied under pyrolytic conditions using excess sodium glycinate the reaction was found to generate a major unknown peak having a molecular ion at m/z 130. Subsequent in-depth isotope labelling studies indicated that acetol was an important precursor of this compound under pyrolytic and aqueous heating conditions. The dimerisation and cyclisation of acetol into 2,5-dimethyl-4-hydroxy-tetrahydrofuran-3-one was found to be catalysed by amino acid metal salts. Also, ESI/qTOF/MS studies indicated that the unknown peak has expected molecular formula of C6H10O3. Finally, a peak having the same retention time and mass spectrum was also generated pyrolytically when furaneol® was reduced with NaBH4 confirming the initial hypothesis regarding the unknown peak to be the reduced form of furaneol®. Copyright © 2016 Elsevier Ltd. All rights reserved.

Pyrolytic conversion of plastic and rubber waste to hydrocarbons with basic salt catalysts

DOEpatents

Wingfield, Jr., Robert C.; Braslaw, Jacob; Gealer, Roy L.

1985-01-01

The invention relates to a process for improving the pyrolytic conversion of waste selected from rubber and plastic to low molecular weight olefinic materials by employing basis salt catalysts in the waste mixture. The salts comprise alkali or alkaline earth compounds, particularly sodium carbonate, in an amount of greater than about 1 weight percent based on the waste feed.

Selective and sensitive determination of uric acid in the presence of ascorbic acid and dopamine by PDDA functionalized graphene/graphite composite electrode.

PubMed

Yu, Yanyan; Chen, Zuanguang; Zhang, Beibei; Li, Xinchun; Pan, Jianbin

2013-08-15

In this work, a facile electrochemical sensor based on poly(diallyldimethylammonium chloride) (PDDA) functionalized graphene (PDDA-G) and graphite was fabricated. The composite electrode exhibited excellent selectivity and sensitivity towards uric acid (UA), owing to the electrocatalytic effect of graphene nanosheets and the electrostatic attractions between PDDA-G and UA. The anodic peak current of UA obtained by cyclic voltammetry (CV) increased over 10-fold compared with bare carbon paste electrode (CPE). And the reversibility of the oxidation process was improved significantly. Differential pulse voltammetry (DPV) was used to determine UA in the presence of ascorbic acid (AA) and dopamine (DA). It was found that all of oxidation peaks of three species could be well resolved, and the peak current of UA was much stronger than the other two components. More importantly, considerable-amount of AA and DA showed negligible interference to UA assay. The calibration curve for UA ranged from 0.5 to 20 μmol L(-1) with a correlation coefficient of 0.9934. The constructed sensor has been employed to quantitatively determine UA in urine samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Nanoscale Electrochemistry of sp(2) Carbon Materials: From Graphite and Graphene to Carbon Nanotubes.

PubMed

Unwin, Patrick R; Güell, Aleix G; Zhang, Guohui

2016-09-20

Carbon materials have a long history of use as electrodes in electrochemistry, from (bio)electroanalysis to applications in energy technologies, such as batteries and fuel cells. With the advent of new forms of nanocarbon, particularly, carbon nanotubes and graphene, carbon electrode materials have taken on even greater significance for electrochemical studies, both in their own right and as components and supports in an array of functional composites. With the increasing prominence of carbon nanomaterials in electrochemistry comes a need to critically evaluate the experimental framework from which a microscopic understanding of electrochemical processes is best developed. This Account advocates the use of emerging electrochemical imaging techniques and confined electrochemical cell formats that have considerable potential to reveal major new perspectives on the intrinsic electrochemical activity of carbon materials, with unprecedented detail and spatial resolution. These techniques allow particular features on a surface to be targeted and models of structure-activity to be developed and tested on a wide range of length scales and time scales. When high resolution electrochemical imaging data are combined with information from other microscopy and spectroscopy techniques applied to the same area of an electrode surface, in a correlative-electrochemical microscopy approach, highly resolved and unambiguous pictures of electrode activity are revealed that provide new views of the electrochemical properties of carbon materials. With a focus on major sp(2) carbon materials, graphite, graphene, and single walled carbon nanotubes (SWNTs), this Account summarizes recent advances that have changed understanding of interfacial electrochemistry at carbon electrodes including: (i) Unequivocal evidence for the high activity of the basal surface of highly oriented pyrolytic graphite (HOPG), which is at least as active as noble metal electrodes (e.g., platinum) for outer-sphere redox processes. (ii) Demonstration of the high activity of basal plane HOPG toward other reactions, with no requirement for catalysis by step edges or defects, as exemplified by studies of proton-coupled electron transfer, redox transformations of adsorbed molecules, surface functionalization via diazonium electrochemistry, and metal electrodeposition. (iii) Rationalization of the complex interplay of different factors that determine electrochemistry at graphene, including the source (mechanical exfoliation from graphite vs chemical vapor deposition), number of graphene layers, edges, electronic structure, redox couple, and electrode history effects. (iv) New methodologies that allow nanoscale electrochemistry of 1D materials (SWNTs) to be related to their electronic characteristics (metallic vs semiconductor SWNTs), size, and quality, with high resolution imaging revealing the high activity of SWNT sidewalls and the importance of defects for some electrocatalytic reactions (e.g., the oxygen reduction reaction). The experimental approaches highlighted for carbon electrodes are generally applicable to other electrode materials and set a new framework and course for the study of electrochemical and interfacial processes.

Chemical preparation of graphene-based nanomaterials and their applications in chemical and biological sensors.

PubMed

Jiang, Hongji

2011-09-05

Graphene is a flat monolayer of carbon atoms packed tightly into a 2D honeycomb lattice that shows many intriguing properties meeting the key requirements for the implementation of highly excellent sensors, and all kinds of proof-of-concept sensors have been devised. To realize the potential sensor applications, the key is to synthesize graphene in a controlled way to achieve enhanced solution-processing capabilities, and at the same time to maintain or even improve the intrinsic properties of graphene. Several production techniques for graphene-based nanomaterials have been developed, ranging from the mechanical cleavage and chemical exfoliation of high-quality graphene to direct growth onto different substrates and the chemical routes using graphite oxide as a precusor to the newly developed bottom-up approach at the molecular level. The current review critically explores the recent progress on the chemical preparation of graphene-based nanomaterials and their applications in sensors. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Graphene oxide-silica nanohybrids as fillers for PA6 based nanocomposites

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

Maio, A.; Fucarino, R.; Khatibi, R.

Graphene oxide (GO) was prepared by oxidation of graphite flakes by a mixture of H{sub 2}SO{sub 4}/H{sub 3}PO{sub 4} and KMnO{sub 4} based on Marcano's method. Two different masterbatches containing GO (33.3%) and polyamide-6 (PA6) (66.7%) were prepared both via solvent casting in formic acid and by melt mixing in a mini-extruder (Haake). The two masterbatches were then used to prepare PA6-based nanocomposites with a content of 2% in GO. For comparison, a nanocomposite by direct mixing of PA6 and GO (2%) and PA6/graphite nanocomposites were prepared, too. The oxidation of graphite into GO was assessed by X-ray diffraction (XRD),more » Micro-Raman spectroscopy, scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) analyses. All these techniques demonstrated the effectiveness of the graphite modification, since the results put into evidence that, after the acid treatment, interlayer distance, oxygen content and defects increased. SEM micrographs carried out on the nanocomposites, showed GO layers totally surrounded by polyamide-6, this feature is likely due to the strong interaction between the hydrophilic moieties located both on GO and on PA6. On the contrary, no interactions were observed when graphite was used as filler. Mechanical characterization, carried out by tensile and dynamic-mechanical tests, marked an improvement of the mechanical properties observed. Photoluminescence and EPR measurements were carried out onto nanoparticles and nanocomposites to study the nature of the interactions and to assess the possibility to use this class of materials as semiconductors or optical sensors.« less

Graphene oxide-silica nanohybrids as fillers for PA6 based nanocomposites

NASA Astrophysics Data System (ADS)

Maio, A.; Fucarino, R.; Khatibi, R.; Botta, L.; Rosselli, S.; Bruno, M.; Scaffaro, R.

2014-05-01

Graphene oxide (GO) was prepared by oxidation of graphite flakes by a mixture of H2SO4/H3PO4 and KMnO4 based on Marcano's method. Two different masterbatches containing GO (33.3%) and polyamide-6 (PA6) (66.7%) were prepared both via solvent casting in formic acid and by melt mixing in a mini-extruder (Haake). The two masterbatches were then used to prepare PA6-based nanocomposites with a content of 2% in GO. For comparison, a nanocomposite by direct mixing of PA6 and GO (2%) and PA6/graphite nanocomposites were prepared, too. The oxidation of graphite into GO was assessed by X-ray diffraction (XRD), Micro-Raman spectroscopy, scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) analyses. All these techniques demonstrated the effectiveness of the graphite modification, since the results put into evidence that, after the acid treatment, interlayer distance, oxygen content and defects increased. SEM micrographs carried out on the nanocomposites, showed GO layers totally surrounded by polyamide-6, this feature is likely due to the strong interaction between the hydrophilic moieties located both on GO and on PA6. On the contrary, no interactions were observed when graphite was used as filler. Mechanical characterization, carried out by tensile and dynamic-mechanical tests, marked an improvement of the mechanical properties observed. Photoluminescence and EPR measurements were carried out onto nanoparticles and nanocomposites to study the nature of the interactions and to assess the possibility to use this class of materials as semiconductors or optical sensors.

Reversible temperature regulation of electrical and thermal conductivity using liquid–solid phase transitions

PubMed Central

Zheng, Ruiting; Gao, Jinwei; Wang, Jianjian; Chen, Gang

2011-01-01

Reversible temperature tuning of electrical and thermal conductivities of materials is of interest for many applications, including seasonal regulation of building temperature, thermal storage and sensors. Here we introduce a general strategy to achieve large contrasts in electrical and thermal conductivities using first-order phase transitions in percolated composite materials. Internal stress generated during a phase transition modulates the electrical and thermal contact resistances, leading to large contrasts in the electrical and thermal conductivities at the phase transition temperature. With graphite/hexadecane suspensions, the electrical conductivity changes 2 orders of magnitude and the thermal conductivity varies up to 3.2 times near 18 °C. The generality of the approach is also demonstrated in other materials such as graphite/water and carbon nanotube/hexadecane suspensions. PMID:21505445

Reversible temperature regulation of electrical and thermal conductivity using liquid-solid phase transitions.

PubMed

Zheng, Ruiting; Gao, Jinwei; Wang, Jianjian; Chen, Gang

2011-01-01

Reversible temperature tuning of electrical and thermal conductivities of materials is of interest for many applications, including seasonal regulation of building temperature, thermal storage and sensors. Here we introduce a general strategy to achieve large contrasts in electrical and thermal conductivities using first-order phase transitions in percolated composite materials. Internal stress generated during a phase transition modulates the electrical and thermal contact resistances, leading to large contrasts in the electrical and thermal conductivities at the phase transition temperature. With graphite/hexadecane suspensions, the electrical conductivity changes 2 orders of magnitude and the thermal conductivity varies up to 3.2 times near 18 °C. The generality of the approach is also demonstrated in other materials such as graphite/water and carbon nanotube/hexadecane suspensions.

Analysis of HEMCL Railgun Insulator Damage

DTIC Science & Technology

2006-06-01

pyrolytic epoxy degradation and glass fiber softening and liquification in the insulator, it is determined that rail-to-rail plasmas are present behind...produces epoxy decomposition products in the form of gases, oils , waxes and chars solid (heavily cross-linked residues) [4]. The nature of the... pyrolytic decomposition product (wax) of the epoxy as in the fired specimens. Figures 6 and 7 are typical examples of glass fiber softening and

Biological conversion of pyrolytic products to ethanol and lipids

NASA Astrophysics Data System (ADS)

Lian, Jieni

Pyrolysis is a promising technology that can convert up to 75 % of lignocellulosic biomass into crude bio-oil. However, due to the complex chemical compositions of bio-oil, its further refining into fuels and high value chemicals faces great challenges. This dissertation research proposed new technologies for biological conversion of pyrolytic products derived from cellulose and hemicellulose, such as anhydrosugars and carbolic acids to fuels and chemicals. First, the pyrolytic anhydrosugars (chiefly levoglucosan (LG)) were hydrolysed into glucose followed by neutralization, detoxification and fermentation to produce ethanol by ethanogenetic yeast and lipids by oleaginous yeasts. Second, a novel process for the conversion of C1-C4 pyrolytic products to lipid with oleaginous yeasts was investigated. Third, oleaginous yeasts that can directly convert LG to lipids were studied and a recombined yeast with LG kinase was constructed for the direct convertion of LG into lipids. This allowed a reduction of existing process for LG fermentation from four steps into two steps and eliminated the need for acids and bases as well as the disposal of chemicals. The development of genetic modified organisms with LG kinase opens a promising avenue for the direct LG fermentation to produce a wide range of fuels and chemicals. The simplification of LG utilization process would enhance the economic viability of this technology.

Determination of boron in blood, urine and bone by electrothermal atomic absorption spectrometry using zirconium and citric acid as modifiers

NASA Astrophysics Data System (ADS)

Burguera, Marcela; Burguera, José Luis; Rondón, Carlos; Carrero, Pablo

2001-10-01

A comparative study of various potential chemical modifiers (Au, Ba, Be, Ca, Cr, Ir, La, Lu, Mg, Ni, Pd, Pt, Rh, Ru, Sr, V, W, and Zr), and different 'coating' treatments (Zr, W, and W+Rh) of the pyrolytic graphite platform of a longitudinally heated graphite tube atomizer for thermal stabilization and determination of boron was undertaken. The use of Au, Ba, Be, Cr, Ir, Pt, Rh, Ru, Sr and V as modifiers, and of W+Rh coating produced erratic, and noisy signals, while the addition of La, Ni and Pd as modifiers, and the W coating had positive effects, but with too high background absorption signals, rendering their use unsuitable for boron determination even in aqueous solutions. The atomic absorption signal for boron was increased and stabilized when the platform was coated with Zr, and by the addition of Ca, Mg, Lu, W or Zr as modifiers. Only the addition of 10 μg of Zr as a modifier onto Zr-treated platforms allowed the use of a higher pyrolysis temperature without analyte losses. The memory effect was minimized by incorporating a cleaning step with 10 μl of 50 g l -1 NH 4F HF after every three boron measurements. The addition of 10 μl of 15 g l -1 citric acid together with Zr onto Zr-treated platforms significantly improved the characteristic mass to m0=282 pg, which is adequate for biological samples such as urine and bone, although the sensitivity was still inadequate for the determination of boron in blood of subjects without supplementary diet. Under optimized conditions, the detection limit (3σ) was 60 μg l -1. The amount of boron found in whole blood, urine and femur head samples from patients with osteoporosis was in agreement with values previously reported in the literature.

The role of mineral surface chemistry in modified dextrin adsorption.

PubMed

Beaussart, Audrey; Mierczynska-Vasilev, Agnieszka M; Harmer, Sarah L; Beattie, David A

2011-05-15

The adsorption of two modified dextrins (phenyl succinate dextrin--PS Dextrin; styrene oxide dextrin--SO Dextrin) on four different mineral surfaces has been studied using X-ray photoelectron spectroscopy (XPS), in situ atomic force microscopy (AFM) imaging, and captive bubble contact angle measurements. The four surfaces include highly orientated pyrolytic graphite (HOPG), freshly cleaved synthetic sphalerite (ZnS), and two surfaces produced through surface reactions of sphalerite: one oxidized in alkaline solution (pH 9, 1 h immersion); and one subjected to metal ion exchange between copper and zinc (i.e. copper activation: exposed to 1×10(-3) M CuSO(4) solution for 1 h). XPS measurements indicate that the different sphalerite surfaces contain varying amounts of sulfur, zinc, oxygen, and copper, producing substrates for polymer adsorption with a range of possible binding sites. AFM imaging has shown that the two polymers adsorb to a similar extent on HOPG, and that the two polymers display very different propensities for adsorption on the three sphalerite surface types, with freshly cleaved sphalerite encouraging the least adsorption, and copper activated and oxidized sphalerite encouraging significantly more adsorption. Contact angle measurements of the four surfaces indicate that synthetic sphalerite has a low contact angle upon fracture, and that oxidation on the timescale of one hour substantially alters the hydrophobicity. HOPG and copper-activated sphalerite were the most hydrophobic, as expected due to the carbon and di/poly-sulfide rich surfaces of the two samples, respectively. SO Dextrin is seen to have a significant impact on the wettability of HOPG and the surface reacted sphalerite samples, highlighting the difficulty in selectively separating sphalerite from carbonaceous unwanted minerals in flotation. PS Dextrin has the least effect on the hydrophobicity of the reacted sphalerite surfaces, whilst still significantly increasing the wettability of graphite, and thus has more potential for use as a polymer depressant in this separation. Copyright © 2011 Elsevier Inc. All rights reserved.

Surfactant exfoliated 2D hexagonal Boron Nitride (2D-hBN) explored as a potential electrochemical sensor for dopamine: surfactants significantly influence sensor capabilities.

PubMed

Khan, Aamar F; Brownson, Dale A C; Foster, Christopher W; Smith, Graham C; Banks, Craig E

2017-05-21

Surfactant exfoliated 2D hexagonal Boron Nitride (2D-hBN) nanosheets are explored as a potential electrochemical sensing platform and evaluated towards the electroanalytical sensing of dopamine (DA) in the presence of the common interferents, ascorbic acid (AA) and uric acid (UA). Surfactant exfoliated 2D-hBN nanosheets (2-4 layers) fabricated using sodium cholate in aqueous media are electrically wired via a drop-casting modification process onto disposable screen-printed graphite electrodes (SPEs). We critically evaluate the performance of these 2D-hBN modified SPEs and demonstrate the effect of 'mass coverage' towards the detection of DA, AA and UA. Previous studies utilising surfactant-free (pristine) 2D-hBN modified SPEs have shown a beneficial effect towards the detection of DA, AA and UA when compared to the underlying/unmodified graphite-based electrode. We show that the fabrication route utilised to prepare 2D-hBN is a vital experimental consideration, such that the beneficial effect previously reported is considerably reduced when surfactant exfoliated 2D-hBN is utilised. We demonstrate for the first time, through implementation of control experiments in the form of surfactant modified graphite electrodes, that sodium cholate is a major contributing factor to the aforementioned detrimental behaviour. The significance here is not in the material per se, but the fundamental knowledge of the surfactant and surface coverage changing the electrochemical properties of the material under investigation. Given the wide variety of ionic and non-ionic surfactants that are utilised in the manufacture of novel 2D materials, the control experiments reported herein need to be performed in order to de-convolute the electrochemical response and effectively evaluate the 'underlying surface/surfactant/2D materials' electrocatalytic contribution.

Oxygen reduction reaction activity and structural stability of Pt-Au nanoparticles prepared by arc-plasma deposition.

PubMed

Takahashi, Shuntaro; Chiba, Hiroshi; Kato, Takashi; Endo, Shota; Hayashi, Takehiro; Todoroki, Naoto; Wadayama, Toshimasa

2015-07-28

The oxygen reduction reaction (ORR) activity and durability of various Au(x)/Pt100 nanoparticles (where x is the atomic ratio of Au against Pt) are evaluated herein. The samples were fabricated on a highly-oriented pyrolytic graphite substrate at 773 K through sequential arc-plasma depositions of Pt and Au. The electrochemical hydrogen adsorption charges (electrochemical surface area), particularly the characteristic currents caused by the corner and edge sites of the Pt nanoparticles, decrease with increasing Au atomic ratio (x). In contrast, the specific ORR activities of the Au(x)/Pt100 samples were dependent on the atomic ratios of Pt and Au: the Au28/Pt100 sample showed the highest specific activity among all the investigated samples (x = 0-42). As for ORR durability evaluated by applying potential cycles between 0.6 and 1.0 V in oxygen-saturated 0.1 M HClO4, Au28/Pt100 was the most durable sample against the electrochemical potential cycles. The results clearly showed that the Au atoms located at coordinatively-unsaturated sites, e.g. at the corners or edges of the Pt nanoparticles, can improve the ORR durability by suppressing unsaturated-site-induced degradation of the Pt nanoparticles.

Broadband optical properties of graphene and HOPG investigated by spectroscopic Mueller matrix ellipsometry

NASA Astrophysics Data System (ADS)

Song, Baokun; Gu, Honggang; Zhu, Simin; Jiang, Hao; Chen, Xiuguo; Zhang, Chuanwei; Liu, Shiyuan

2018-05-01

Optical properties of mono-graphene fabricated by chemical vapor deposition (CVD) and highly oriented pyrolytic graphite (HOPG) are comparatively studied by Mueller matrix ellipsometry (MME) over an ultra-wide energy range of 0.73-6.42 eV. A multilayer stacking model is constructed to describe the CVD mono-graphene, in which the roughness of the glass substrate and the water adsorption on the graphene are considered. We introduce a uniaxial anisotropic dielectric model to parameterize the optical constants of both the graphene and the HOPG. With the established models, broadband optical constants of the graphene and the HOPG are determined from the Mueller matrix spectra based on a point-by-point method and a non-linear regression method, respectively. Two significant absorption peaks at 4.75 eV and 6.31 eV are observed in the extinction coefficient spectra of the mono-graphene, which can be attributed to the von-Hove singularity (i.e., the π-to-π∗ exciton transition) near the M point and the σ-to-σ∗ exciton transition near the Γ point of the Brillouin zone, respectively. Comparatively, only a major absorption peak at 4.96 eV appears in the ordinary extinction coefficient spectra of the HOPG, which is mainly formed by the π-to-π∗ interband transition.

A collection system for dry solid residues from exhaled breath for analysis via atomic force microscopy.

PubMed

Morozov, Victor N; Mikheev, Andrey Y

2017-01-09

Exhaled air contains sub-micron droplets of lung liquid, which potentially bear biomarkers of lung diseases. After dehydration they form dry residue particles (DRPs). As a first step in developing techniques to characterize individual DRPs, a new electrostatic collector was designed in which DRPs are charged within a unipolar corona charger, concentrated in a cone funnel, and deposited onto a limited area of a highly oriented pyrolytic graphite surface. The collector captures 80%-90% of DRPs at an optimal flow rate of 0.15 l min -1 . Atomic force microscopy (AFM) revealed flattened round particles 20-50 nm high, with notable protrusions at their surface suggestive of an inhomogeneous internal structure. Exposure to humid air resulted in the DRPs spreading over the surface, with a 50%-200% decrease in their heights and an increase in their lateral dimensions so that their volume decreased by only 10% ± 3%. Exposure to saturated chloroform vapor resulted in drainage of 10%-15% of the DRP volume (presumably lipids), forming collar-shaped rings around each particle but leaving the core size and structure unchanged. AFM measurements combined with laser counter measurements of the DRP concentrations were used to estimate that one liter of air exhaled by volunteers contained less than 100 pg of dry residue material.

Integration of the ferromagnetic insulator EuO onto graphene.

PubMed

Swartz, Adrian G; Odenthal, Patrick M; Hao, Yufeng; Ruoff, Rodney S; Kawakami, Roland K

2012-11-27

We have demonstrated the deposition of EuO films on graphene by reactive molecular beam epitaxy in a special adsorption-controlled and oxygen-limited regime, which is a critical advance toward the realization of the exchange proximity interaction (EPI). It has been predicted that when the ferromagnetic insulator (FMI) EuO is brought into contact with graphene, an overlap of electronic wave functions at the FMI/graphene interface can induce a large spin splitting inside the graphene. Experimental realization of this effect could lead to new routes for spin manipulation, which is a necessary requirement for a functional spin transistor. Furthermore, EPI could lead to novel spintronic behavior such as controllable magnetoresistance, gate tunable exchange bias, and quantized anomalous Hall effect. However, experimentally, EuO has not yet been integrated onto graphene. Here we report the successful growth of high-quality crystalline EuO on highly oriented pyrolytic graphite and single-layer graphene. The epitaxial EuO layers have (001) orientation and do not induce an observable D peak (defect) in the Raman spectra. Magneto-optic measurements indicate ferromagnetism with a Curie temperature of 69 K, which is the value for bulk EuO. Transport measurements on exfoliated graphene before and after EuO deposition indicate only a slight decrease in mobility.

Formation, dissolution and properties of surface nanobubbles

NASA Astrophysics Data System (ADS)

Che, Zhizhao; Theodorakis, Panagiotis E.

2017-02-01

Surface nanobubbles are stable gaseous phases in liquids that form on solid substrates. While their existence has been confirmed, there are many open questions related to their formation and dissolution processes along with their structures and properties, which are difficult to investigate experimentally. To address these issues, we carried out molecular dynamics simulations based on atomistic force fields for systems comprised of water, air (N2 and O2), and a Highly Oriented Pyrolytic Graphite (HOPG) substrate. Our results provide insights into the formation/dissolution mechanisms of nanobubbles and estimates for their density, contact angle, and surface tension. We found that the formation of nanobubbles is driven by an initial nucleation process of air molecules and the subsequent coalescence of the formed air clusters. The clusters form favorably on the substrate, which provides an enhanced stability to the clusters. In contrast, nanobubbles formed in the bulk either move randomly to the substrate and spread or move to the water--air surface and pop immediately. Moreover, nanobubbles consist of a condensed gaseous phase with a surface tension smaller than that of an equivalent system under atmospheric conditions, and contact angles larger than those in the equivalent nanodroplet case. We anticipate that this study will provide useful insights into the physics of nanobubbles and will stimulate further research in the field by using all-atom simulations.

Nucleation processes of nanobubbles at a solid/water interface

NASA Astrophysics Data System (ADS)

Fang, Chung-Kai; Ko, Hsien-Chen; Yang, Chih-Wen; Lu, Yi-Hsien; Hwang, Ing-Shouh

2016-04-01

Experimental investigations of hydrophobic/water interfaces often return controversial results, possibly due to the unknown role of gas accumulation at the interfaces. Here, during advanced atomic force microscopy of the initial evolution of gas-containing structures at a highly ordered pyrolytic graphite/water interface, a fluid phase first appeared as a circular wetting layer ~0.3 nm in thickness and was later transformed into a cap-shaped nanostructure (an interfacial nanobubble). Two-dimensional ordered domains were nucleated and grew over time outside or at the perimeter of the fluid regions, eventually confining growth of the fluid regions to the vertical direction. We determined that interfacial nanobubbles and fluid layers have very similar mechanical properties, suggesting low interfacial tension with water and a liquid-like nature, explaining their high stability and their roles in boundary slip and bubble nucleation. These ordered domains may be the interfacial hydrophilic gas hydrates and/or the long-sought chemical surface heterogeneities responsible for contact line pinning and contact angle hysteresis. The gradual nucleation and growth of hydrophilic ordered domains renders the original homogeneous hydrophobic/water interface more heterogeneous over time, which would have great consequence for interfacial properties that affect diverse phenomena, including interactions in water, chemical reactions, and the self-assembly and function of biological molecules.

Interfacial gas nanobubbles or oil nanodroplets?

PubMed

Wang, Xingya; Zhao, Binyu; Hu, Jun; Wang, Shuo; Tai, Renzhong; Gao, Xingyu; Zhang, Lijuan

2017-01-04

The existence of nanobubbles at a solid-liquid interface with high stability has been confirmed by myriad experimental studies, and their gaseous nature has also been extensively verified. However, nanodroplets of polydimethylsiloxane (PDMS) recently observed in the atomic force microscopy (AFM) measurement of nanobubbles plague the nanobubble community. It may easily lead to wrong interpretations of the AFM results and thus hinders further application of the already widely used AFM in nanobubble studies. Therefore, finding a direct experimental solution to distinguish nanobubbles from nanodroplets in AFM measurements is a matter of great urgency. Herein, we first developed an effective and reproducible method to produce PDMS nanodroplets at the highly ordered pyrolytic graphite (HOPG)/water interface. From their size, contact angle, and stiffness, the formed PDMS nanodroplets are not distinguishable from nanobubbles. However, the force curves on these two objects are strikingly different from each other, i.e., a peculiar plateau in both the approach and retraction curves was found on nanobubbles whereas they changed linearly between the jump-in and jump-off point on PDMS nanodroplets. Thus, the present study not only provided a simple and effective procedure to generate PDMS nanodroplets but also paved a simple practical and in situ way to discriminate nanobubbles from the PDMS nanodroplets by direct AFM force measurements.

Analysis of the substrate influence on the ordering of epitaxial molecular layers: The special case of point-on-line coincidence

NASA Astrophysics Data System (ADS)

Mannsfeld, S. C.; Fritz, T.

2004-02-01

The physical structure of organic-inorganic heteroepitaxial thin films is usually governed by a fine balance between weak molecule-molecule interactions and a weakly laterally varying molecule-substrate interaction potential. Therefore, in order to investigate the energetics of such a layer system one has to consider large molecular domains. So far, layer potential calculations for large domains of organic thin films on crystalline substrates were difficult to perform concerning the computational effort which stems from the vast number of atoms which have to be included. Here, we present a technique which enables the calculation of the molecule-substrate interaction potential for large molecular domains by utilizing potential energy grid files. This technique allows the investigation of the substrate influence in systems prepared by organic molecular beam epitaxy (OMBE), like 3,4,9,10-perylenetetracarboxylicdianhydride on highly oriented pyrolytic graphite. For this system the so-called point-on-line coincidence was proposed, a growth mode which has been controversially discussed in literature. Furthermore, we are able to provide evidence for a general energetic advantage of such point-on-line coincident domain orientations over arbitrarily oriented domains which substantiates that energetically favorable lattice structures in OMBE systems are not restricted to commensurate unit cells or coincident super cells.

Transmission measurement based on STM observation to detect the penetration depth of low-energy heavy ions in botanic samples.

PubMed

Liu, Feng; Wang, Yugang; Xue, Jianming; Wang, Sixue; Du, Guanhua; Zhao, Weijiang

2003-02-01

The penetration depth of low-energy heavy ions in botanic samples was detected with a new transmission measurement. In the measurement, highly oriented pyrolytic graphite (HOPG) pieces were placed behind the botanic samples with certain thickness. During the irradiation of heavy ions with energy of tens of keV, the energetic particles transmitted from those samples were received by the HOPG pieces. After irradiation, scanning tunneling microscope (STM) was applied to observe protrusion-like damage induced by these transmitted ions on the surface of the HOPG. The statistical average number density of protrusions and the minimum transmission rate of the low-energy heavy ions can be obtained. The detection efficiency of the new method for low-energy heavy ions was about 0.1-1 and the background in the measurement can be reduced to as low as 1.0 x 10(8) protrusions/cm2. With this method, the penetration depth of the energetic particles was detected to be no less than 60 micrometers in kidney bean slices when the slices were irradiated by 100 keVAr+ ion at the fluence of 5 x 10(16) ions/cm2. c2002 Elsevier Science Ltd. All rights reserved.

Peeling the astronomical onion.

PubMed

Rosu-Finsen, Alexander; Marchione, Demian; Salter, Tara L; Stubbing, James W; Brown, Wendy A; McCoustra, Martin R S

2016-11-23

Water ice is the most abundant solid in the Universe. Understanding the formation, structure and multiplicity of physicochemical roles for water ice in the cold, dense interstellar environments in which it is predominantly observed is a crucial quest for astrochemistry as these are regions active in star and planet formation. Intuitively, we would expect the mobility of water molecules deposited or synthesised on dust grain surfaces at temperatures below 50 K to be very limited. This work delves into the thermally-activated mobility of H 2 O molecules on model interstellar grain surfaces. The energy required to initiate this process is studied by reflection-absorption infrared spectroscopy of small quantities of water on amorphous silica and highly oriented pyrolytic graphite surfaces as the surface is annealed. Strongly non-Arrhenius behaviour is observed with an activation energy of 2 kJ mol -1 on the silica surface below 25 K and 0 kJ mol -1 on both surfaces between 25 and 100 K. The astrophysical implication of these results is that on timescales shorter than that estimated for the formation of a complete monolayer of water ice on a grain, aggregation of water ice will result in a non-uniform coating of water, hence leaving bare grain surface exposed. Other molecules can thus be formed or adsorbed on this bare surface.

Transmission measurement based on STM observation to detect the penetration depth of low-energy heavy ions in botanic samples

NASA Technical Reports Server (NTRS)

Liu, Feng; Wang, Yugang; Xue, Jianming; Wang, Sixue; Du, Guanhua; Zhao, Weijiang

2003-01-01

The penetration depth of low-energy heavy ions in botanic samples was detected with a new transmission measurement. In the measurement, highly oriented pyrolytic graphite (HOPG) pieces were placed behind the botanic samples with certain thickness. During the irradiation of heavy ions with energy of tens of keV, the energetic particles transmitted from those samples were received by the HOPG pieces. After irradiation, scanning tunneling microscope (STM) was applied to observe protrusion-like damage induced by these transmitted ions on the surface of the HOPG. The statistical average number density of protrusions and the minimum transmission rate of the low-energy heavy ions can be obtained. The detection efficiency of the new method for low-energy heavy ions was about 0.1-1 and the background in the measurement can be reduced to as low as 1.0 x 10(8) protrusions/cm2. With this method, the penetration depth of the energetic particles was detected to be no less than 60 micrometers in kidney bean slices when the slices were irradiated by 100 keVAr+ ion at the fluence of 5 x 10(16) ions/cm2. c2002 Elsevier Science Ltd. All rights reserved.

Switch on the high thermal conductivity of graphene paper.

PubMed

Xie, Yangsu; Yuan, Pengyu; Wang, Tianyu; Hashemi, Nastaran; Wang, Xinwei

2016-10-14

This work reports on the discovery of a high thermal conductivity (κ) switch-on phenomenon in high purity graphene paper (GP) when its temperature is reduced from room temperature down to 10 K. The κ after switch-on (1732 to 3013 W m -1 K -1 ) is 4-8 times that before switch-on. The triggering temperature is 245-260 K. The switch-on behavior is attributed to the thermal expansion mismatch between pure graphene flakes and impurity-embedded flakes. This is confirmed by the switch behavior of the temperature coefficient of resistance. Before switch-on, the interactions between pure graphene flakes and surrounding impurity-embedded flakes efficiently suppress phonon transport in GP. After switch-on, the structure separation frees the pure graphene flakes from the impurity-embedded neighbors, leading to a several-fold κ increase. The measured κ before and after switch-on is consistent with the literature reported κ values of supported and suspended graphene. By conducting comparison studies with pyrolytic graphite, graphene oxide paper and partly reduced graphene paper, the whole physical picture is illustrated clearly. The thermal expansion induced switch-on is feasible only for high purity GP materials. This finding points out a novel way to switch on/off the thermal conductivity of graphene paper based on substrate-phonon scattering.

The effect of thermal reduction on the photoluminescence and electronic structures of graphene oxides.

PubMed

Chuang, C-H; Wang, Y-F; Shao, Y-C; Yeh, Y-C; Wang, D-Y; Chen, C-W; Chiou, J W; Ray, Sekhar C; Pong, W F; Zhang, L; Zhu, J F; Guo, J H

2014-04-10

Electronic structures of graphene oxide (GO) and hydro-thermally reduced graphene oxides (rGOs) processed at low temperatures (120-180°C) were studied using X-ray absorption near-edge structure (XANES), X-ray emission spectroscopy (XES) and resonant inelastic X-ray scattering (RIXS). C K-edge XANES spectra of rGOs reveal that thermal reduction restores C = C sp(2) bonds and removes some of the oxygen and hydroxyl groups of GO, which initiates the evolution of carbonaceous species. The combination of C K-edge XANES and Kα XES spectra shows that the overlapping π and π* orbitals in rGOs and GO are similar to that of highly ordered pyrolytic graphite (HOPG), which has no band-gap. C Kα RIXS spectra provide evidence that thermal reduction changes the density of states (DOSs) that is generated in the π-region and/or in the gap between the π and π* levels of the GO and rGOs. Two-dimensional C Kα RIXS mapping of the heavy reduction of rGOs further confirms that the residual oxygen and/or oxygen-containing functional groups modify the π and σ features, which are dispersed by the photon excitation energy. The dispersion behavior near the K point is approximately linear and differs from the parabolic-like dispersion observed in HOPG.

Local atomic order of a metallic glass made visible by scanning tunneling microscopy

NASA Astrophysics Data System (ADS)

Luo, Yuansu; Samwer, Konrad

2018-06-01

Exploring the atomic level structure in amorphous materials by STM becomes extremely difficult due to the localized electronic states. Here we carried out STM studies on a quasi-low-dimensional film of metallic glass Zr65Cu27.5Al7.5 which is ‘ultrathin’ compared with the localization length and/or the length scale of short range order. The local electronic structure must appear more inherent, having states at E f available for tip-sample tunneling current. To enhance imaging contrasts between long-range and short-range orders, the highly oriented pyrolytic graphite was chosen as substrate, so that the structural heterogeneity arising from competition between the glass former ability and the epitaxy can be ascertained. A chemical order predicted for this system was observed in atomic ordered regimes (1–2 monolayers), accompanied with a superstructure with the period Zr–Cu(Al)–Zr along three hexagonal axes. The result implies a chemical short range order in disordered regimes, where polyhedral clusters are dominant with the solute atom Cu(Al) in the center. An attempt for the structural modelling was made based on high resolution STM images, giving icosahedral order on the surface and different Voronoi clusters in 3D space.

GINA--a polarized neutron reflectometer at the Budapest Neutron Centre.

PubMed

Bottyán, L; Merkel, D G; Nagy, B; Füzi, J; Sajti, Sz; Deák, L; Endrőczi, G; Petrenko, A V; Major, J

2013-01-01

The setup, capabilities, and operation parameters of the neutron reflectometer GINA, the recently installed "Grazing Incidence Neutron Apparatus" at the Budapest Neutron Centre, are introduced. GINA, a dance-floor-type, constant-energy, angle-dispersive reflectometer is equipped with a 2D position-sensitive detector to study specular and off-specular scattering. Wavelength options between 3.2 and 5.7 Å are available for unpolarized and polarized neutrons. Spin polarization and analysis are achieved by magnetized transmission supermirrors and radio-frequency adiabatic spin flippers. As a result of vertical focusing by a five-element pyrolytic graphite monochromator, the reflected intensity from a 20 × 20 mm(2) sample has been doubled. GINA is dedicated to studies of magnetic films and heterostructures, but unpolarized options for non-magnetic films, membranes, and other surfaces are also provided. Shortly after its startup, reflectivity values as low as 3 × 10(-5) have been measured by the instrument. The instrument capabilities are demonstrated by a non-polarized and a polarized reflectivity experiment on a Si wafer and on a magnetic film of [(62)Ni/(nat)Ni](5) isotope-periodic layer composition. The facility is now open for the international user community. Its further development is underway establishing new sample environment options and spin analysis of off-specularly scattered radiation as well as further decreasing the background.

Coherent anti-Stokes Raman scattering enhancement of thymine adsorbed on graphene oxide

PubMed Central

2014-01-01

Coherent anti-Stokes Raman scattering (CARS) of carbon nanostructures, namely, highly oriented pyrolytic graphite, graphene nanoplatelets, graphene oxide, and multiwall carbon nanotubes as well CARS spectra of thymine (Thy) molecules adsorbed on graphene oxide were studied. The spectra of the samples were compared with spontaneous Raman scattering (RS) spectra. The CARS spectra of Thy adsorbed on graphene oxide are characterized by shifts of the main bands in comparison with RS. The CARS spectra of the initial nanocarbons are definitely different: for all investigated materials, there is a redistribution of D- and G-mode intensities, significant shift of their frequencies (more than 20 cm-1), and appearance of new modes about 1,400 and 1,500 cm-1. The D band in CARS spectra is less changed than the G band; there is an absence of 2D-mode at 2,600 cm-1 for graphene and appearance of intensive modes of the second order between 2,400 and 3,000 cm-1. Multiphonon processes in graphene under many photon excitations seem to be responsible for the features of the CARS spectra. We found an enhancement of the CARS signal from thymine adsorbed on graphene oxide with maximum enhancement factor about 105. The probable mechanism of CARS enhancement is discussed. PMID:24948887

High repetition pump-and-probe photoemission spectroscopy based on a compact fiber laser system.

PubMed

Ishida, Y; Otsu, T; Ozawa, A; Yaji, K; Tani, S; Shin, S; Kobayashi, Y

2016-12-01

The paper describes a time-resolved photoemission (TRPES) apparatus equipped with a Yb-doped fiber laser system delivering 1.2-eV pump and 5.9-eV probe pulses at the repetition rate of 95 MHz. Time and energy resolutions are 11.3 meV and ∼310 fs, respectively, the latter is estimated by performing TRPES on a highly oriented pyrolytic graphite (HOPG). The high repetition rate is suited for achieving high signal-to-noise ratio in TRPES spectra, thereby facilitating investigations of ultrafast electronic dynamics in the low pump fluence (p) region. TRPES of polycrystalline bismuth (Bi) at p as low as 30 nJ/mm 2 is demonstrated. The laser source is compact and is docked to an existing TRPES apparatus based on a 250-kHz Ti:sapphire laser system. The 95-MHz system is less prone to space-charge broadening effects compared to the 250-kHz system, which we explicitly show in a systematic probe-power dependency of the Fermi cutoff of polycrystalline gold. We also describe that the TRPES response of an oriented Bi(111)/HOPG sample is useful for fine-tuning the spatial overlap of the pump and probe beams even when p is as low as 30 nJ/mm 2 .

Fiber Optic Sensors for Health Monitoring of Morphing Aircraft

NASA Technical Reports Server (NTRS)

Brown, Timothy; Wood, Karen; Childers, Brooks; Cano, Roberto; Jensen, Brian; Rogowski, Robert

2001-01-01

Fiber optic sensors are being developed for health monitoring of future aircraft. Aircraft health monitoring involves the use of strain, temperature, vibration and chemical sensors. These sensors will measure load and vibration signatures that will be used to infer structural integrity. Sine the aircraft morphing program assumes that future aircraft will be aerodynamically reconfigurable there is also a requirement for pressure, flow and shape sensors. In some cases a single fiber may be used for measuring several different parameters. The objective of the current program is to develop techniques for using optical fibers to monitor composite cure in real time during manufacture and to monitor in-service structural integrity of the composite structure. Graphite-epoxy panels were fabricated with integrated optical fibers of various types. The panels were mechanically and thermally tested to evaluate composite strength and sensor durability. Finally the performance of the fiber optic sensors was determined. Experimental results are presented evaluating the performance of embedded and surface mounted optical fibers for measuring strain, temperature and chemical composition. The performance of the fiber optic sensors was determined by direct comparison with results from more conventional instrumentation. The facilities for fabricating optical fiber and associated sensors and methods of demodulating Bragg gratings for strain measurement will be described.

Production of clean pyrolytic sugars for fermentation.

PubMed

Rover, Marjorie R; Johnston, Patrick A; Jin, Tao; Smith, Ryan G; Brown, Robert C; Jarboe, Laura

2014-06-01

This study explores the separate recovery of sugars and phenolic oligomers produced during fast pyrolysis with the effective removal of contaminants from the separated pyrolytic sugars to produce a substrate suitable for fermentation without hydrolysis. The first two stages from a unique recovery system capture "heavy ends", mostly water-soluble sugars and water-insoluble phenolic oligomers. The differences in water solubility can be exploited to recover a sugar-rich aqueous phase and a phenolic-rich raffinate. Over 93 wt % of the sugars is removed in two water washes. These sugars contain contaminants such as low-molecular-weight acids, furans, and phenols that could inhibit successful fermentation. Detoxification methods were used to remove these contaminants from pyrolytic sugars. The optimal candidate is NaOH overliming, which results in maximum growth measurements with the use of ethanol-producing Escherichia coli. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Low temperature conversion of plastic waste into light hydrocarbons.

PubMed

Shah, Sajid Hussain; Khan, Zahid Mahmood; Raja, Iftikhar Ahmad; Mahmood, Qaisar; Bhatti, Zulfiqar Ahmad; Khan, Jamil; Farooq, Ather; Rashid, Naim; Wu, Donglei

2010-07-15

Advance recycling through pyrolytic technology has the potential of being applied to the management of plastic waste (PW). For this purpose 1 l volume, energy efficient batch reactor was manufactured locally and tested for pyrolysis of waste plastic. The feedstock for reactor was 50 g waste polyethylene. The average yield of the pyrolytic oil, wax, pyrogas and char from pyrolysis of PW were 48.6, 40.7, 10.1 and 0.6%, respectively, at 275 degrees C with non-catalytic process. Using catalyst the average yields of pyrolytic oil, pyrogas, wax and residue (char) of 50 g of PW was 47.98, 35.43, 16.09 and 0.50%, respectively, at operating temperature of 250 degrees C. The designed reactor could work at low temperature in the absence of a catalyst to obtain similar products as for a catalytic process. 2010 Elsevier B.V. All rights reserved.

A comparison of nitrogen-doped sonoelectrochemical and chemical graphene nanosheets as hydrogen peroxide sensors.

PubMed

Wu, Yi-Shan; Liu, Zhe-Ting; Wang, Tzu-Pei; Hsu, Su-Yang; Lee, Chien-Liang

2018-04-01

Nitrogen-doped graphene nanosheet (N-SEGN) with pyrrolic nitrogen and 5-9 vacancy defects has been successfully prepared from a hydrothermal reaction of tetra-2-pyridinylpyrazine and sonoelectrochemistry-exfoliated graphene nanosheet, with point defects. Additionally, based on the same reaction using chemically reduced graphene oxide, nitrogen-doped chemically reduced graphene oxide (N-rGO) with graphitic nitrogen was prepared. The N-SEGN and N-rGO were used as a non-enzymatic H 2 O 2 sensors. The sensitivity of the N-SEGN was 231.3 μA·mM -1 ·cm -2 , much greater than 57.3 μA·mM -1 ·cm -2 of N-rGO. The N-SEGN showed their potential for being a H 2 O 2 sensor. Copyright © 2017 Elsevier B.V. All rights reserved.

Pyrolytic Synthesis of Carbon Nanotubes from Sucrose on a Mesoporous Silicate

NASA Technical Reports Server (NTRS)

Abdel-Fattah, Tarek; Siochi, Mia; Crooks, Roy

2005-01-01

Multiwall carbon nanotubes were synthesized from sucrose by a pyrolytic technique using mesoporous MCM-41 silicate templates without transition metal catalysts. The Nanotubes were examined in the carbon/silicate composite and after dissolution of the silicate. High resolution transmission electron microscopy study of the multiwall nanotubes showed them to be 15 nm in diameter, 200 nm in length and close-ended. There was variation in crystallinity with some nanotubes showing disordered wall structures.

Catalytic fast pyrolysis of biomass impregnated with potassium phosphate in a hydrogen atmosphere for the production of phenol and activated carbon

NASA Astrophysics Data System (ADS)

Lu, Qiang; Zhang, Zhen-xi; Wang, Xin; Guo, Hao-qiang; Cui, Min-shu; Yang, Yong-ping

2018-02-01

A new technique was proposed to co-produce phenol and activated carbon (AC) from catalytic fast pyrolysis of biomass impregnated with K3PO4 in a hydrogen atmosphere, followed by activation of the pyrolytic solid residues. Lab-scale catalytic fast pyrolysis experiments were performed to quantitatively determine the pyrolytic product distribution, as well as to investigate the effects of several factors on the phenol production, including pyrolysis atmosphere, catalyst type, biomass type, catalytic pyrolysis temperature, and catalyst impregnation content. In addition, the pyrolytic solid residues were activated to prepare ACs with high specific surface areas. The results indicated that phenol could be obtained due to the synergistic effects of K3PO4 and hydrogen atmosphere, with the yield and selectivity reaching 5.3 wt% and 17.8% from catalytic fast pyrolysis of poplar wood with 8 wt% K3PO4 at 550 oC in a hydrogen atmosphere. This technique was adaptable to different woody materials for phenol production. Moreover, gas product generated from the pyrolysis process was feasible to be recycled to provide the hydrogen atmosphere, instead of extra hydrogen supply. In addition, the pyrolytic solid residue was suitable for AC preparation, using CO2 activation method, the specific surface area was as high as 1605 m2/g.

The Pyrolytic Profile of Lyophilized and Deep-Frozen Compact Part of the Human Bone

PubMed Central

Lodowska, Jolanta; Wolny, Daniel; Kurkiewicz, Sławomir; Węglarz, Ludmiła

2012-01-01

Background. Bone grafts are used in the treatment of nonunion of fractures, bone tumors and in arthroplasty. Tissues preserved by lyophilization or deep freezing are used as implants nowadays. Lyophilized grafts are utilized in the therapy of birth defects and bone benign tumors, while deep-frozen ones are applied in orthopedics. The aim of the study was to compare the pyrolytic pattern, as an indirect means of the analysis of organic composition of deep-frozen and lyophilized compact part of the human bone. Methods. Samples of preserved bone tissue were subjected to thermolysis and tetrahydroammonium-hydroxide- (TMAH-) associated thermochemolysis coupled with gas chromatography and mass spectrometry (Py-GC/MS). Results. Derivatives of benzene, pyridine, pyrrole, phenol, sulfur compounds, nitriles, saturated and unsaturated aliphatic hydrocarbons, and fatty acids (C12–C20) were identified in the pyrolytic pattern. The pyrolyzates were the most abundant in derivatives of pyrrole and nitriles originated from proteins. The predominant product in pyrolytic pattern of the investigated bone was pyrrolo[1,2-α]piperazine-3,6-dione derived from collagen. The content of this compound significantly differentiated the lyophilized graft from the deep-frozen one. Oleic and palmitic acid were predominant among fatty acids of the investigated samples. The deep-frozen implants were characterized by higher percentage of long-chain fatty acids than lyophilized grafts. PMID:22619606

H/C atomic ratio as a smart linkage between pyrolytic temperatures, aromatic clusters and sorption properties of biochars derived from diverse precursory materials

PubMed Central

Xiao, Xin; Chen, Zaiming; Chen, Baoliang

2016-01-01

Biochar is increasingly gaining attention due to multifunctional roles in soil amelioration, pollution mitigation and carbon sequestration. It is a significant challenge to compare the reported results from world-wide labs regarding the structure and sorption of biochars derived from various precursors under different pyrolytic conditions due to a lack of a simple linkage. By combining the published works on various biochars, we established a quantitative relationship between H/C atomic ratio and pyrolytic temperature (T), aromatic structure, and sorption properties for naphthalene and phenanthrene. A reverse sigmoid shape between T and the H/C ratio was observed, which was independent of the precursors of biochars, including the ash contents. Linear correlations of Freundlich parameters (N, log Kf) and sorption amount (log Qe, log QA) with H/C ratios were found. A rectangle-like model was proposed to predict the aromatic cluster sizes of biochars from their H/C ratios, and then a good structure-sorption relationship was derived. These quantitative relationships indicate that the H/C atomic ratio is a universal linkage to predict pyrolytic temperatures, aromatic cluster sizes, and sorption characteristics. This study would guide the global study of biochars toward being comparable, and then the development of the structure-sorption relationships will benefit the structural design and environmental application of biochars. PMID:26940984

Catalytic Fast Pyrolysis of Biomass Impregnated with Potassium Phosphate in a Hydrogen Atmosphere for the Production of Phenol and Activated Carbon

PubMed Central

Lu, Qiang; Zhang, Zhen-xi; Wang, Xin; Guo, Hao-qiang; Cui, Min-shu; Yang, Yong-ping

2018-01-01

A new technique was proposed to co-produce phenol and activated carbon (AC) from catalytic fast pyrolysis of biomass impregnated with K3PO4 in a hydrogen atmosphere, followed by activation of the pyrolytic solid residues. Lab-scale catalytic fast pyrolysis experiments were performed to quantitatively determine the pyrolytic product distribution, as well as to investigate the effects of several factors on the phenol production, including pyrolysis atmosphere, catalyst type, biomass type, catalytic pyrolysis temperature, and catalyst impregnation content. In addition, the pyrolytic solid residues were activated to prepare ACs with high specific surface areas. The results indicated that phenol could be obtained due to the synergistic effects of K3PO4 and hydrogen atmosphere, with the yield and selectivity reaching 5.3 wt% and 17.8% from catalytic fast pyrolysis of poplar wood with 8 wt% K3PO4 at 550°C in a hydrogen atmosphere. This technique was adaptable to different woody materials for phenol production. Moreover, gas product generated from the pyrolysis process was feasible to be recycled to provide the hydrogen atmosphere, instead of extra hydrogen supply. In addition, the pyrolytic solid residue was suitable for AC preparation, using CO2 activation method, the specific surface area was as high as 1,605 m2/g. PMID:29515994

Cascade Production of Lactic Acid from Universal Types of Sugars Catalyzed by Lanthanum Triflate.

PubMed

Liu, Dajiang; Kim, Kwang Ho; Sun, Jian; Simmons, Blake A; Singh, Seema

2018-02-09

Lignocellulosic biomass conversion into value-added platform chemicals in the non-toxic, water-tolerant Lewis acid, and water solutions bears the hallmark of green chemistry. Lactic acid derived from biomass is an important chemical building block for biodegradable polymers such as polylactide. Herein, a universal method of converting lignocellulosic sugars into lactic acid using catalytic amount of water-stable Lewis acid La(OTf) 3 is demonstrated. The lignocellulosic sugars studied in this work include 1) pyrolytic sugars from pyrolysis oil, and 2) sugars derived from ionic liquid (IL)-pretreated biomass. Under moderate conditions (250 °C, 1 h), levoglucosan (major pyrolytic sugar), glucose, and xylose were converted into lactic acid with carbon-based molar yields of 75, 74, and 61 %, respectively. Furthermore, roughly 49 mol % (based on levoglucosan) and 74 wt % (relative to pretreated biomass) of lactic acid were obtained from the conversion of pyrolytic sugars and sugar-rich fraction after lignin removal from switchgrass, respectively. To our knowledge, this is the first reported conversion of pyrolytic sugar into lactic acid by chemocatalysis and also lignocellulosic sugars are converted into lactic acid without hydrolysis. This approach could potentially be extended to other lignocellulosic sugars after simple removal of lignin from biomass pretreatment, rendering moderate to high yields of lactic acid. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.