Development of highly porous crystalline titania photocatalysts

NASA Astrophysics Data System (ADS)

Marszewski, Michal

The objectives of this dissertation are the design, synthesis, and characterization of titania materials with surface area, porosity, crystallinity and doping tailored toward photocatalytic applications. Ultimately, the research should result in a strategy allowing the synthesis of titania with all these important features. The synthetic methods investigated in this research will include: i) soft-templating, ii) hard-templating, and iii) modified precursor strategy. Soft-templating strategy uses organic templates--either block copolymers or surfactants--that under specific conditions assemble into micelles, and later, these micelles are used to template the desired material around them. The resulting organic-inorganic composite is then calcined in air to remove the organic template and recover the final material with high surface area and large pore volume. This work explores 1) synthesis of titania materials in the presence of polymer templates, and the effects of different synthetic conditions on the structure of the resulting materials. Hard-templating, in contrast to soft-templating, uses inorganic templates. The hard template is introduced during the synthesis to cast its shape onto the fabricated material and removed afterwards, when the material has formed. The final material is an inverse replica of the hard template used, typically with a well-developed mesostructure. This work explores 1) hard templating synthesis of titania materials using silica and alumina, and 2) the effects of the template amount and type. The modified precursor strategy is a novel synthetic method, developed in this research, and designed specifically to achieve titania material with high surface area, large pore volume, high crystallinity, and possibly doping. The modified precursors are prepared by reacting generic titania precursors, such as titanium isopropoxide (TIPO), with organic acids, which results in substitution of some or all alkoxide groups in TIPO structure. The goal is to introduce new, easily carbonizable groups in TIPO structure so that the modified precursor can serve as titania and carbon precursor simultaneously. Subsequently, during carbonization in inert atmosphere, a carbon framework is formed that works as a scaffold, protecting titania during its crystallization. Afterwards, the carbon scaffold is removed by calcination in air. This work explores the modified precursor strategy by 1) preparing titania materials from TIPO modified with different carboxylic acids and 2) investigating the effect of the modifying acid on the properties of the carbon-titania composites and the final titania materials.

Method for making thin carbon foam electrodes

DOEpatents

Pekala, R.W.; Mayer, S.T.; Kaschmitter, J.L.; Morrison, R.L.

1999-08-03

A method for fabricating thin, flat carbon electrodes by infiltrating highly porous carbon papers, membranes, felts, metal fibers/powders, or fabrics with an appropriate carbon foam precursor material is disclosed. The infiltrated carbon paper, for example, is then cured to form a gel-saturated carbon paper, which is subsequently dried and pyrolyzed to form a thin sheet of porous carbon. The material readily stays flat and flexible during curing and pyrolyzing to form thin sheets. Precursor materials include polyacrylonitrile (PAN), polymethylacrylonitrile (PMAN), resorcinol/formaldehyde, catechol/formaldehyde, phenol/formaldehyde, etc., or mixtures thereof. These thin films are ideal for use as high power and energy electrodes in batteries, capacitors, and fuel cells, and are potentially useful for capacitive deionization, filtration and catalysis.

Microwave-assisted synthesis of porous carbon-titania and highly crystalline titania nanostructures.

PubMed

Parker, Alison; Marszewski, Michal; Jaroniec, Mietek

2013-03-01

Porous carbon-titania and highly crystalline titania nanostructured materials were obtained through a microwave-assisted one-pot synthesis. Resorcinol and formaldehyde were used as carbon precursors, triblock copolymer Pluronic F127 as a stabilizing agent, and titanium isopropoxide as a titania precursor. This microwave-assisted one-pot synthesis involved formation of carbon spheres according to the recently modified Stöber method followed by hydrolysis and condensation of titania precursor. This method afforded carbon-titania composite materials containing anatase phase with specific surface areas as high as 390 m(2) g(-1). The pure nanostructured titania, obtained after removal of carbon through calcination of the composite material in air, was shown to be the anatase phase with considerably higher degree of crystallinity and the specific surface area as high as 130 m(2) g(-1). The resulting titania, because of its high surface area, well-developed porosity, and high crystallinity, is of great interest for catalysis, water treatment, lithium batteries, and other energy-related applications.

A Reliable Homemade Electrode Based on Glassy Polymeric Carbon

ERIC Educational Resources Information Center

Santos, Andre L.; Takeuchi, Regina M.; Oliviero, Herilton P.; Rodriguez, Marcello G.; Zimmerman, Robert L.

2004-01-01

The production of a GPC-based material by submitting a cross-linked resin precursor to control thermal conditions is discussed. The precursor material is prepolymerized at 60-degree Celsius in a mold and is carbonized in inert atmosphere by slowly raising the temperature, the rise is performed to avoid change in the shape of the carbonization…

Aerogel and xerogel composites for use as carbon anodes

DOEpatents

Cooper, John F.; Tillotson, Thomas M.; Hrubesh, Lawrence W.

2010-10-12

A method for forming a reinforced rigid anode monolith and fuel and product of such method. The method includes providing a solution of organic aerogel or xerogel precursors including at least one of a phenolic resin, phenol (hydroxybenzene), resorcinol(1,3-dihydroxybenzene), or catechol(1,2-dihydroxybenzene); at least one aldehyde compound selected from the group consisting of formaldehyde, acetaldehyde, and furfuraldehyde; and an alkali carbonate or phosphoric acid catalyst; adding internal reinforcement materials comprising carbon to said precursor solution to form a precursor mixture; gelling said precursor mixture to form a composite gel; drying said composite gel; and pyrolyzing said composite gel to form a wettable aerogel/carbon composite or a wettable xerogel/carbon composite, wherein said composites comprise chars and said internal reinforcement materials, and wherein said composite is suitable for use as an anode with the chars being fuel capable of being combusted in a molten salt electrochemical fuel cell in the range from 500 C to 800 C to produce electrical energy. Additional methods and systems/compositions are also provided.

Bimetallic Metal-Organic Frameworks for Controlled Catalytic Graphitization of Nanoporous Carbons

PubMed Central

Tang, Jing; Salunkhe, Rahul R.; Zhang, Huabin; Malgras, Victor; Ahamad, Tansir; Alshehri, Saad M.; Kobayashi, Naoya; Tominaka, Satoshi; Ide, Yusuke; Kim, Jung Ho; Yamauchi, Yusuke

2016-01-01

Single metal-organic frameworks (MOFs), constructed from the coordination between one-fold metal ions and organic linkers, show limited functionalities when used as precursors for nanoporous carbon materials. Herein, we propose to merge the advantages of zinc and cobalt metals ions into one single MOF crystal (i.e., bimetallic MOFs). The organic linkers that coordinate with cobalt ions tend to yield graphitic carbons after carbonization, unlike those bridging with zinc ions, due to the controlled catalytic graphitization by the cobalt nanoparticles. In this work, we demonstrate a feasible method to achieve nanoporous carbon materials with tailored properties, including specific surface area, pore size distribution, degree of graphitization, and content of heteroatoms. The bimetallic-MOF-derived nanoporous carbon are systematically characterized, highlighting the importance of precisely controlling the properties of the carbon materials. This can be done by finely tuning the components in the bimetallic MOF precursors, and thus designing optimal carbon materials for specific applications. PMID:27471193

Novel materials for electrochemical power sources—introduction of PUREBLACK ® Carbons

NASA Astrophysics Data System (ADS)

Barsukov, Igor V.; Gallego, Maritza A.; Doninger, Joseph E.

Graphitization heat treatment of a precursor carbon black was seen to effectively produce a wide variety of forms of partially graphitized nano-sized carbonaceous materials with a set of unique properties, some of which are reported in this paper in comparison with those properties of the precursor carbon material. These novel materials were given the name of PUREBLACK ® Carbons. Among some of the unique properties are: higher conductivity than that of acetylene type carbon blacks due to PUREBLACK ® Carbon's particles having more graphitic structure; very low to zero volatile content (external oxygen, sulfur, etc., groups, which are often believed to be the cause of initiation of self-discharge reactions in batteries); very low equilibrium moisture pickup (20 ppm level), which makes it particularly attractive in lithium metal or lithium-ion based electrochemical systems; high purity. Electrochemical testing of the newly proposed PUREBLACK ® Carbons in several battery systems offers significant promise that it presents a viable solution to the needs of industry.

Preparation of Pt Nanocatalyst on Carbon Materials via a Reduction Reaction of a Pt Precursor in a Drying Process.

PubMed

Lee, Jae-Young; Lee, Woo-Kum; Rim, Hyung-Ryul; Joung, Gyu-Bum; Weidner, John W; Lee, Hong-Ki

2016-06-01

Platinum (Pt) nanocatalyst for a proton-exchange membrane fuel cell (PEMFC) was prepared on a carbon black particle or a graphite particle coated with a nafion polymer via a reduction of platinum(II) bis(acetylacetonate) denoted as Pt(acac)2 as a Pt precursor in a drying process. Sublimed Pt(acac)2 adsorbed on the nafion-coated carbon materials was reduced to Pt nanoparticles in a glass reactor at 180 degrees C of N2 atmosphere. The morphology of Pt nanoparticles on carbon materials was observed by scanning electron microscopy (SEM) and the distribution of Pt nanoparticles was done by transmission electron microscopy (TEM). The particle size was estimated by analyzing the TEM image using an image analyzer. It was found that nano-sized Pt particles were deposited on the surface of carbon materials, and the number density and the average particle size increased with increasing reduction time.

Modeling Initial Stage of Ablation Material Pyrolysis: Graphitic Precursor Formation and Interfacial Effects

NASA Technical Reports Server (NTRS)

Desai, Tapan G.; Lawson, John W.; Keblinski, Pawel

2010-01-01

Reactive molecular dynamics simulations are used to study initial stage of pyrolysis of ablation materials and their composites with carbon nanotubes and carbon fibers. The products formed during pyrolysis are characterized and water is found as the primary product in all cases. The water formation mechanisms are analyzed and the value of the activation energy for water formation is estimated. A detailed study on graphitic precursor formation reveals the presence of two temperature zones. In the lower temperature zone (less than 2000 K) polymerization occurs resulting in formation of large, stable graphitic precursors, and in the high temperature zone (greater than 2000 K) polymer scission results in formation of short polymer chains/molecules. Simulations performed in the high temperature zone on the phenolic resin composites (with carbon nanotubes and carbon fibers) shows that the presence of interfaces had no substantial effect on the chain scission rate or the activation energy value for water formation.

Room-temperature Electrochemical Synthesis of Carbide-derived Carbons and Related Materials

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

Gogotsi, Yury

2015-02-28

This project addresses room-temperature electrochemical etching as an energy-efficient route to synthesis of 3D nanoporous carbon networks and layered 2D carbons and related structures, as well as provides fundamental understanding of structure and properties of materials produced by this method. Carbide-derived-carbons (CDCs) are a growing class of nanostructured carbon materials with properties that are desirable for many applications, such as electrical energy and gas storage. The structure of these functional materials is tunable by the choice of the starting carbide precursor, synthesis method, and process parameters. Moving from high-temperature synthesis of CDCs through vacuum decomposition above 1400°C and chlorination abovemore » 400°C, our studies under the previous DOE BES support led to identification of precursor materials and processing conditions for CDC synthesis at temperatures as low as 200°C, resulting in amorphous and highly reactive porous carbons. We also investigated synthesis of monolithic CDC films from carbide films at 250-1200°C. The results of our early studies provided new insights into CDC formation, led to development of materials for capacitive energy storage, and enabled fundamental understanding of the electrolyte ions confinement in nanoporous carbons.« less

Surface-functionalized mesoporous carbon materials

DOEpatents

Dai, Sheng; Gorka, Joanna; Mayes, Richard T.

2016-02-02

A functionalized mesoporous carbon composition comprising a mesoporous carbon scaffold having mesopores in which polyvinyl polymer grafts are covalently attached, wherein said mesopores have a size of at least 2 nm and up to 50 nm. Also described is a method for producing the functionalized mesoporous composition, wherein a reaction medium comprising a precursor mesoporous carbon, vinyl monomer, initiator, and solvent is subjected to sonication of sufficient power to result in grafting and polymerization of the vinyl monomer into mesopores of the precursor mesoporous carbon. Also described are methods for using the functionalized mesoporous carbon, particularly in extracting metal ions from metal-containing solutions.

Progress Report on PICA Activities in Support of New Frontiers Missions

NASA Technical Reports Server (NTRS)

Stackpoole, Margaret; Venkatapathy, Ethiraj; Violette, Steve

2017-01-01

Phenolic Impregnated Carbon Ablator (PICA) is a TPS material that has been used in a number of previous flight missions (Stardust, MSL) and is planned for a number of future missions (OSIRIS-Rex and Mars 2020) so it has substantial flight heritage, is applicable to a wide range of missions, and is often baselined as the TPS in future NASA proposal activities. As is common with a number of TPS materials, PICA faces a supply chain issue with the rayon precursor from which the carbon fibers used in the PICA preform are derived. PICA uses a non-woven form of the rayon, which once carbonized, is used in the low-density carbon FiberForm (carbon tile) preform utilized in PICA. Current PICA uses a NASA-qualified non-domestic rayon supplier (Sniace), however the qualified supplier is no longer manufacturing the rayon materials. This activity will address PICA sustainability, by initially carbonizing the remaining stockpile of Sniace rayon precursor. A additional FiberForm manufacturing task from alternate rayon sources is also in progress.

Nitrogen-doped carbon spheres: A new high-energy-density and long-life pseudo-capacitive electrode material for electrochemical flow capacitor.

PubMed

Hou, Shujin; Wang, Miao; Xu, Xingtao; Li, Yandong; Li, Yanjiang; Lu, Ting; Pan, Likun

2017-04-01

One of the most challenging issues in developing electrochemical flow capacitor (EFC) technology is the design and synthesis of active electrode materials with high energy density and long cycle life. However, in practical cases, the energy density and cycle ability obtained currently cannot meet the practical need. In this work, we propose a new active material, nitrogen-doped carbon spheres (NCSs), as flowable electrodes for EFC application. The NCSs were prepared via one-pot hydrothermal synthesis in the presence of resorcinol/formaldehyde as carbon precursors and melamine as nitrogen precursor, followed by carbonization in nitrogen flow at various temperatures. The results of EFC experiments demonstrate that NCSs obtained at 800°C exhibit a high energy density of 13.5Whkg -1 and an excellent cycle ability, indicating the superiority of NCSs for EFC application. Copyright © 2016 Elsevier Inc. All rights reserved.

Directed Synthesis of Nanoporous Carbons from Task-Specific Ionic Liquid Precursors for the Adsorption of CO 2

DOE PAGES

Mahurin, Shannon M.; Fulvio, Pasquale F.; Hillesheim, Patrick C.; ...

2014-07-31

Postcombustion CO 2 capture has become a key component of greenhouse-gas reduction as anthropogenic emissions continue to impact the environment. In this paper, we report a one-step synthesis of porous carbon materials using a series of task-specific ionic liquids for the adsorption of CO 2. By varying the structure of the ionic liquid precursor, we were able to control pore architecture and surface functional groups of the carbon materials in this one-step synthesis process leading to adsorbents with high CO 2 sorption capacities (up to 4.067 mmol g -1) at 0 °C and 1 bar. Finally, added nitrogen functional groupsmore » led to high CO 2/N 2 adsorption-selectivity values ranging from 20 to 37 whereas simultaneously the interaction energy was enhanced relative to carbon materials with no added nitrogen.« less

Carbide-derived carbons - From porous networks to nanotubes and graphene

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

Presser, V.; Heon, M.; Gogotsi, Y.

2011-02-09

Carbide-derived carbons (CDCs) are a large family of carbon materials derived from carbide precursors that are transformed into pure carbon via physical (e.g., thermal decomposition) or chemical (e.g., halogenation) processes. Structurally, CDC ranges from amorphous carbon to graphite, carbon nanotubes or graphene. For halogenated carbides, a high level of control over the resulting amorphous porous carbon structure is possible by changing the synthesis conditions and carbide precursor. The large number of resulting carbon structures and their tunability enables a wide range of applications, from tribological coatings for ceramics, or selective sorbents, to gas and electrical energy storage. In particular, themore » application of CDC in supercapacitors has recently attracted much attention. This review paper summarizes key aspects of CDC synthesis, properties, and applications. It is shown that the CDC structure and properties are sensitive to changes of the synthesis parameters. Understanding of processing–structure–properties relationships facilitates tuning of the carbon material to the requirements of a certain application.« less

An electrochemical sensor based on nitrogen doped carbon material prepared from nitrogen-containing precursors

NASA Astrophysics Data System (ADS)

Cui, G. Y.; Wang, C. Y.; Xiang, G. Q.; Zhou, B.

2018-01-01

In this work, a nitrogen doped carbon material (NDC) was prepared by using a copper adenine complex as precursor and applied to electrochemical sensing of Vitamin B2 (VB2). The experimental results show that the nitrogen doped carbon material is obtained after calcination at 650 °C under argon atmosphere, afterwards, which were characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), fourier transform infrared (FT-IR), and electrochemical method. According to the XRD data, the product was a carbon material, and infrared data demonstrates that there are two kinds of carbonyl nitrogen combination, respectively, C-N and C = N combination of ways. Importantly, we used NDC to construct electrochemical biosensor to detect VB2 by differential pulse voltammetry (DPV). The linear range was 6 × 10-6 - 3.5 × 10-4 M (R=0.9962), the minimum detection limit was 5.4 × 10-6 M, and the sensitivity is better. Consequently, it has better sensing performance.

ACBC to Balcite: Bioinspired Synthesis of a Highly Substituted High-Temperature Phase from an Amorphous Precursor

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

Whittaker, Michael L.; Joester, Derk

2017-04-28

Energy-efficient synthesis of materials locked in compositional and structural states far from equilibrium remains a challenging goal, yet biomineralizing organisms routinely assemble such materials with sophisticated designs and advanced functional properties, often using amorphous precursors. However, incorporation of organics limits the useful temperature range of these materials. Herein, the bioinspired synthesis of a highly supersaturated calcite (Ca0.5Ba0.5CO3) called balcite is reported, at mild conditions and using an amorphous calcium–barium carbonate (ACBC) (Ca1- x Ba x CO3·1.2H2O) precursor. Balcite not only contains 50 times more barium than the solubility limit in calcite but also displays the rotational disorder on carbonate sitesmore » that is typical for high-temperature calcite. It is significantly harder (30%) and less stiff than calcite, and retains these properties after heating to elevated temperatures. Analysis of balcite local order suggests that it may require the formation of the ACBC precursor and could therefore be an example of nonclassical nucleation. These findings demonstrate that amorphous precursor pathways are powerfully enabling and provide unprecedented access to materials far from equilibrium, including high-temperature modifications by room-temperature synthesis.« less

Preparation and characterization of graphene/turbostratic carbon derived from chitosan film for supercapacitor electrodes

NASA Astrophysics Data System (ADS)

Hanappi, M. F. Y. M.; Deraman, M.; Suleman, M.; Othman, M. A. R.; Basri, N. H.; Nor, N. S. M.; Hamdan, E.; Sazali, N. E. S.; Tajuddin, N. S. M.

2018-04-01

Electrochemical capacitors or supercapacitors are the potential energy storage devices which are known for having higher specific capacitance and specific energy than electrolytic capacitors. Electric double-layer capacitors (EDLCs) also referred as ultracapacitors is a class of supercapacitors that employ different forms of carbon like activated carbon, CNT, graphene etc., as electrodes. The performance of the supercapacitors is determined by its components namely electrolyte, electrode, etc. Carbon electrodes with high surface area and desired pore size distribution are always preferred and which can be tailored by varying the precursor and method of preparation. In recent years, owing to their low cost, ease of synthesis, high stability and conductivity, the activated carbons derived from biomass precursors have been investigated as potential electrode material for the EDLCs. In this report, we present the preparation and characterization of graphene/turbostratic carbon monolith (CM) electrodes from the carbon grains (CGs) obtained by carbonization (under the flow of nitrogen, N2 gas and over a temperature range from 600 °C to 1000 °C) of biomass precursor chitosan film. The procedure to prepare the chitosan film is described elsewhere. The carbon grains are characterized using Raman spectroscopy (RS) and X-ray diffraction (XRD). We expect that the CGs would have the similar characteristics as graphene and would be a potential electrode material for EDLCs application.

Aerogel and xerogel composites for use as carbon anodes

DOEpatents

Cooper, John F [Oakland, CA; Tillotson, Thomas M [Tracy, CA; Hrubesh, Lawrence W [Pleasanton, CA

2008-08-12

Disclosed herein are aerogel and xerogel composite materials suitable for use as anodes in fuel cells and batteries. Precursors to the aerogel and xerogel compounds are infused with inorganic polymeric materials or carbon particles and then gelled. The gels are then pyrolyzed to form composites with internal structural support.

Adsorption of p-cresol on novel diatomite/carbon composites.

PubMed

Hadjar, H; Hamdi, B; Ania, C O

2011-04-15

Hybrid inorganic/organic adsorbents were synthesized using mixtures of diatomite and carbon charcoal as precursors, and explored for the removal of p-cresol from aqueous solution. The carbon/diatomite composites displayed a bimodal and interconnected porous structure which was partially inherited from both precursors. They display moderate surface areas (between 100 and 400 m(2)g(-1)) due to their large inorganic content (between 70 and 90 wt.%), since the diatomite is a non-porous material. Compared to activated carbons with a more developed porosity, p-cresol adsorption on the prepared carbon/diatomite composites was much faster, showing adsorption capacities similar to those of conventional adsorbents over a wide pH range. These results show a good affinity of p-cresol molecules towards the hybrid inorganic/organic composites, and demonstrate the suitability of these novel materials for the removal of aromatic (polar) molecules, despite their dominant inorganic character. Copyright © 2011 Elsevier B.V. All rights reserved.

Processes for making dense, spherical active materials for lithium-ion cells

DOEpatents

Kang, Sun-Ho [Naperville, IL; Amine, Khalil [Downers Grove, IL

2011-11-22

Processes are provided for making dense, spherical mixed-metal carbonate or phosphate precursors that are particularly well suited for the production of active materials for electrochemical devices such as lithium ion secondary batteries. Exemplified methods include precipitating dense, spherical particles of metal carbonates or metal phosphates from a combined aqueous solution using a precipitating agent such as ammonium hydrogen carbonate, sodium hydrogen carbonate, or a mixture that includes sodium hydrogen carbonate. Other exemplified methods include precipitating dense, spherical particles of metal phosphates using a precipitating agent such as ammonium hydrogen phosphate, ammonium dihydrogen phosphate, sodium phosphate, sodium hydrogen phosphate, sodium dihydrogen phosphate, or a mixture of any two or more thereof. Further provided are compositions of and methods of making dense, spherical metal oxides and metal phosphates using the dense, spherical metal precursors. Still further provided are electrodes and batteries using the same.

Copper modified carbon molecular sieves for selective oxygen removal

NASA Technical Reports Server (NTRS)

Sharma, Pramod K. (Inventor); Seshan, Panchalam K. (Inventor)

1992-01-01

Carbon molecular sieves modified by the incorporation of finely divided elemental copper useful for the selective sorption of oxygen at elevated temperatures. The carbon molecular sieves can be regenerated by reduction with hydrogen. The copper modified carbon molecular sieves are prepared by pyrolysis of a mixture of a copper-containing material and polyfunctional alcohol to form a sorbent precursor. The sorbent precursors are then heated and reduced to produce copper modified carbon molecular sieves. The copper modified carbon molecular sieves are useful for sorption of all concentrations of oxygen at temperatures up to about 200.degree. C. They are also useful for removal of trace amount of oxygen from gases at temperatures up to about 600.degree. C.

Fabricating Large-Area Sheets of Single-Layer Graphene by CVD

NASA Technical Reports Server (NTRS)

Bronikowski, Michael; Manohara, Harish

2008-01-01

This innovation consists of a set of methodologies for preparing large area (greater than 1 cm(exp 2)) domains of single-atomic-layer graphite, also called graphene, in single (two-dimensional) crystal form. To fabricate a single graphene layer using chemical vapor deposition (CVD), the process begins with an atomically flat surface of an appropriate substrate and an appropriate precursor molecule containing carbon atoms attached to substituent atoms or groups. These molecules will be brought into contact with the substrate surface by being flowed over, or sprayed onto, the substrate, under CVD conditions of low pressure and elevated temperature. Upon contact with the surface, the precursor molecules will decompose. The substituent groups detach from the carbon atoms and form gas-phase species, leaving the unfunctionalized carbon atoms attached to the substrate surface. These carbon atoms will diffuse upon this surface and encounter and bond to other carbon atoms. If conditions are chosen carefully, the surface carbon atoms will arrange to form the lowest energy single-layer structure available, which is the graphene lattice that is sought. Another method for creating the graphene lattice includes metal-catalyzed CVD, in which the decomposition of the precursor molecules is initiated by the catalytic action of a catalytic metal upon the substrate surface. Another type of metal-catalyzed CVD has the entire substrate composed of catalytic metal, or other material, either as a bulk crystal or as a think layer of catalyst deposited upon another surface. In this case, the precursor molecules decompose directly upon contact with the substrate, releasing their atoms and forming the graphene sheet. Atomic layer deposition (ALD) can also be used. In this method, a substrate surface at low temperature is covered with exactly one monolayer of precursor molecules (which may be of more than one type). This is heated up so that the precursor molecules decompose and form one monolayer of the target material.

Carbon fiber manufacturing via plasma technology

DOEpatents

Paulauskas, Felix L.; Yarborough, Kenneth D.; Meek, Thomas T.

2002-01-01

The disclosed invention introduces a novel method of manufacturing carbon and/or graphite fibers that avoids the high costs associated with conventional carbonization processes. The method of the present invention avoids these costs by utilizing plasma technology in connection with electromagnetic radiation to produce carbon and/or graphite fibers from fully or partially stabilized carbon fiber precursors. In general, the stabilized or partially stabilized carbon fiber precursors are placed under slight tension, in an oxygen-free atmosphere, and carbonized using a plasma and electromagnetic radiation having a power input which is increased as the fibers become more carbonized and progress towards a final carbon or graphite product. In an additional step, the final carbon or graphite product may be surface treated with an oxygen-plasma treatment to enhance adhesion to matrix materials.

Intercalation of Lithium in Pitch-Based Graphitized Carbon Fibers Chemically Modified by Fluorine: Soft Carbon With or Without an Oxide Surface

NASA Technical Reports Server (NTRS)

Hung, Ching-Chen; Prisko, Aniko

1999-01-01

The effects of carbon structure and surface oxygen on the carbon's performance as the anode in lithium-ion battery were studied. Two carbon materials were used for the electrochemical tests: soft carbon made from defluorination of graphite fluoride, and the carbon precursor from which the graphite fluoride was made. In this research the precursor was graphitized carbon fiber P-100. It was first fluorinated to form CF(0.68), then defluorinated slowly at 350 to 450 C in bromoform, and finally heated in 1000 C nitrogen before exposed to room temperature air, producing disordered soft carbon having basic surface oxides. This process caused very little carbon loss. The electrochemical test involved cycles of lithium intercalation and deintercalation using C/saturated LiI-50/50 (vol %) EC and DMC/Li half cell. The cycling test had four major results. (1) The presence of a basic oxide surface may prevent solvent from entering the carbon structure and therefore prolong the carbon's cycle life for lithium intercalation-deintercalation. (2) The disordered soft carbon can store lithium through two different mechanisms. One of them is lithium intercalation. which gives the disordered carbon an electrochemical behavior similar to its more ordered graphitic precursor. The other is unknown in its chemistry, but is responsible for the high-N,oltage portion (less than 0.3V) of the charge-discharge curve. (3) Under certain conditions, the disordered carbon can store more lithium than its precursor. (4) These sample and its precursor can intercalate at 200 mA/g. and deintercalate at a rate of 2000 mA/g without significant capacity loss.

Effect of Silica Nanoparticles on the Photoluminescence Properties of BCNO Phosphor

NASA Astrophysics Data System (ADS)

Nuryadin, Bebeh W.; Faryuni, Irfana Diah; Iskandar, Ferry; Abdullah, Mikrajuddin; Khairurrijal, Khairurrijal

2011-12-01

Effect of additional silica nanoparticles on the photoluminescence (PL) performance of boron carbon oxy-nitride (BCNO) phosphor was investigated. As a precursor, boric acid and urea were used as boron and nitrogen sources, respectively. The carbon sources was polyethylene glycol (PEG) with average molecule weight 20000 g/mol.. Precursor solutions were prepared by mixing these raw materials in pure water, followed by stirring to achieve homogeneous solutions. In this precursor, silica nanoparticles were added at various mass ratio from 0 to 7 %wt in the solution. The precursors were then heated at 750 °C for 60 min in a ceramic crucible under atmospheric pressure. The photoluminescence (PL) spectrum that characterized by spectrophotometer showed a single, distinct, and broad emission band varied from blue to near red color, depend on the PEG, boric acid and urea ratio in the precursor. The addition of silica nanoparticles caused the increasing of PL intensity as well as the shifting of peak wavelength of PL spectrum. The peak shifting of PL was affected by the concentration of silica nanoparticles that added into the precursor. We believe that the BCNO-silica composite phosphor becomes a promising material for the phosphor conversion-based white light-emitting diodes.

Boron/Carbon/Silicon/Nitrogen Ceramics And Precursors

NASA Technical Reports Server (NTRS)

Riccitiello, Salvatore; Hsu, Ming TA; Chen, Timothy S.

1996-01-01

Ceramics containing various amounts of boron, carbon, silicon, and nitrogen made from variety of polymeric precursors. Synthesized in high yield from readily available and relatively inexpensive starting materials. Stable at room temperature; when polymerized, converted to ceramics in high yield. Ceramics resist oxidation and other forms of degradation at high temperatures; used in bulk to form objects or to infiltrate other ceramics to obtain composites having greater resistance to oxidation and high temperatures.

Marine and Freshwater Feedstocks as a Precursor for Nitrogen-Containing Carbons: A Review

PubMed Central

Ilnicka, Anna; Lukaszewicz, Jerzy P.

2018-01-01

Marine-derived as well as freshwater feedstock offers important benefits, such as abundance, morphological and structural variety, and the presence of multiple elements, including nitrogen and carbon. Therefore, these renewal resources may be useful for obtaining N- and C-containing materials that can be manufactured by various methods, such as pyrolysis and hydrothermal processes supported by means of chemical and physical activators. However, every synthesis concept relies on an efficient transfer of nitrogen and carbon from marine/freshwater feedstock to the final product. This paper reviews the advantages of marine feedstock over synthetic and natural but non-marine resources as precursors for the manufacturing of N-doped activated carbons. The manufacturing procedure influences some crucial properties of nitrogen-doped carbon materials, such as pore structure and the chemical composition of the surface. An extensive review is given on the relationship between carbon materials manufacturing from marine feedstock and the elemental content of nitrogen, together with a description of the chemical bonding of nitrogen atoms at the surface. N-doped carbons may serve as effective adsorbents for the removal of pollutants from the gas or liquid phase. Non-recognized areas of adsorption-based applications for nitrogen-doped carbons are presented, too. The paper proves that nitrogen-doped carbon materials belong to most of the prospective electrode materials for electrochemical energy conversion and storage technologies such as fuel cells, air–metal batteries, and supercapacitors, as well as for bioimaging. The reviewed material belongs to the widely understood field of marine biotechnology in relation to marine natural products. PMID:29701697

Carbon Fiber Composite Materials for Automotive Applications

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

Norris, Jr., Robert E.; Mainka, Hendrik

Volkswagen (VW) is internationally recognized for quantity and quality of world-wide vehicle production and the Oak Ridge National Laboratory (ORNL) is internationally recognized in materials research and development. With automotive production ramping up in the recently constructed VW Group of America facility in Chattanooga, Tennessee, ORNL and VW initiated discussions in 2012 concerning opportunities for collaboration around ORNL’s carbon fiber and composites programs. ORNL is conducting an internationally recognized program to develop and implement lower cost carbon fibers and composites for automotive and other “energy missions” for the US Department of Energy. Significant effort is ongoing in selecting, developing, andmore » evaluating alternative precursors, developing and demonstrating advanced conversion techniques, and developing and tailoring surface treatment, sizings, and formatting fiber for specific composite matrices and end-use applications. ORNL already had North America’s most comprehensive suite of tools for carbon fiber research and development and established a semiproduction demonstration line referred to as the Carbon Fiber Technology Facility (CFTF) to facilitate implementation of low cost carbon fiber (LCCF) approaches in early 2013. ORNL and VW agreed to collaborate in a formal Cooperative Research and Development Agreement (NFE-12-03992) specifically focused on evaluating applicability of low cost carbon fiber products for potential vehicle components. The goal of the work outlined in this report was to develop and qualify uses for carbon fiber-reinforced structures in connection with civilian ground transportation. Significant progress was achieved in evaluating and understanding lignin-based precursor materials; however, availability of carbon fiber converted from lignin precursor combined with logistical issues associated with the Visa limitations for the VW participant resulted in significantly shortening of the collaboration period and development of the targeted application(s). Alternatively, objectives of this work have been refined and are now largely being pursued through the involvement of ORNL and VW participation in the more recently established Innovation for Advanced Composites Manufacturing Innovation (IACMI) where composite materials applications are being demonstrated in a much larger scope.« less

Carbon Cryogel and Carbon Paper-Based Silicon Composite Anode Materials for Lithium-Ion Batteries

NASA Technical Reports Server (NTRS)

Woodworth, James; Baldwin, Richard; Bennett, William

2010-01-01

A variety of materials are under investigation for use as anode materials in lithium-ion batteries, of which, the most promising are those containing silicon. 6 One such material is a composite formed via the dispersion of silicon in a resorcinol-formaldehyde (RF) gel followed by pyrolysis. Two silicon-carbon composite materials, carbon microspheres and nanofoams produced from nano-phase silicon impregnated RF gel precursors have been synthesized and investigated. Carbon microspheres are produced by forming the silicon-containing RF gel into microspheres whereas carbon nano-foams are produced by impregnating carbon fiber paper with the silicon containing RF gel to create a free standing electrode. 1-5 Both materials have demonstrated their ability to function as anodes and utilize the silicon present in the material. Stable reversible capacities above 400 mAh/g for the bulk material and above 1000 mAh/g of Si have been observed.

Silicon Composite Anode Materials for Lithium Ion Batteries Based on Carbon Cryogels and Carbon Paper

NASA Technical Reports Server (NTRS)

Woodworth, James; Baldwin, Richard; Bennett, William

2010-01-01

A variety of materials are under investigation for use as anode materials in lithium-ion batteries, of which, the most promising are those containing silicon. One such material is a composite formed via the dispersion of silicon in a resorcinol-formaldehyde (RF) gel followed by pyrolysis. Two silicon-carbon composite materials, carbon microspheres and nanofoams produced from nano-phase silicon impregnated RF gel precursors have been synthesized and investigated. Carbon microspheres are produced by forming the silicon-containing RF gel into microspheres whereas carbon nanofoams are produced by impregnating carbon fiber paper with the silicon containing RF gel to create a free standing electrode. Both materials have demonstrated their ability to function as anodes and utilize the silicon present in the material. Stable reversible capacities above 400 mAh/g for the bulk material and above 1000 mAh/g of Si have been observed.

Sustaining PICA for Future NASA Robotic Science Missions Including NF-4 and Discovery

NASA Technical Reports Server (NTRS)

Stackpoole, Mairead; Venkatapathy, Ethiraj; Violette, Steve

2018-01-01

Phenolic Impregnated Carbon Ablator (PICA), invented in the mid 1990's, is a low-density ablative thermal protection material proven capable of meeting sample return mission needs from the moon, asteroids, comets and other unrestricted class V destinations as well as for Mars. Its low density and efficient performance characteristics have proven effective for use from Discovery to Flag-ship class missions. It is important that NASA maintain this thermal protection material capability and ensure its availability for future NASA use. The rayon based carbon precursor raw material used in PICA preform manufacturing has experienced multiple supply chain issues and required replacement and requalification at least twice in the past 25 years and a third substitution is now needed. The carbon precursor replacement challenge is twofold - the first involves finding a long-term replacement for the current rayon and the second is to assess its future availability periodically to ensure it is sustainable and be alerted if additional replacement efforts need to be initiated. This paper reviews current PICA sustainability activities to identify a rayon replacement and to establish that the capability of the new PICA derived from an alternative precursor is in family with previous versions.

Sustaining Phenolic Impregnated Carbon Ablator (PICA) TPS for Future NASA Robotic Science Missions Including NF-4 and Discovery

NASA Technical Reports Server (NTRS)

Venkatapathy, E.; Stackpoole, M.; Violette, S.

2018-01-01

Phenolic Impregnated Carbon Ablator (PICA), invented in the mid 1990s, is a low-density ablative thermal protection material proven capable of meeting sample return mission needs from the moon, asteroids, comets and other unrestricted class V destinations as well as for Mars. Its low density and efficient performance characteristics have proven effective for use from Discovery to Flagship class missions. It is important that NASA maintain this TPS material capability and ensure its availability for future NASA use. The rayon based carbon precursor raw material used in PICA preform manufacturing required replacement and requalification at least twice in the past 25 years and a third substitution is now needed. The carbon precursor replacement challenge is twofold the first involves finding a long-term replacement for the current rayon and the second is to assess its future availability periodically to ensure it is sustainable and be alerted if additional replacement efforts need to be initiated. Rayon is no longer a viable process in the US and Europe due to environmental concerns. In the early 80s rayon producers began investigating a new method of producing a cellulosic fiber through a more environmentally responsible process. This cellulosic fiber, lyocell, is a viable replacement precursor for PICA fiberform. This presentation reviews current SMD-PSD funded PICA sustainability activities in ensuring a rayon replacement for the long term is identified and in establishing that the capability of the new PICA derived from an alternative precursor is in family with previous versions of the so called heritage PICA.

Preparation of novel carbon microfiber/carbon nanofiber-dispersed polyvinyl alcohol-based nanocomposite material for lithium-ion electrolyte battery separator.

PubMed

Sharma, Ajit K; Khare, Prateek; Singh, Jayant K; Verma, Nishith

2013-04-01

A novel nanocomposite polyvinyl alcohol precursor-based material dispersed with the web of carbon microfibers and carbon nanofibers is developed as lithium (Li)-ion electrolyte battery separator. The primary synthesis steps of the separator material consist of esterification of polyvinyl acetate to produce polyvinyl alcohol gel, ball-milling of the surfactant dispersed carbon micro-nanofibers, mixing of the milled micron size (~500 nm) fibers to the reactant mixture at the incipience of the polyvinyl alcohol gel formation, and the mixing of hydrophobic reagents along with polyethylene glycol as a plasticizer, to produce a thin film of ~25 μm. The produced film, uniformly dispersed with carbon micro-nanofibers, has dramatically improved performance as a battery separator, with the ion conductivity of the electrolytes (LiPF6) saturated film measured as 0.119 S-cm(-1), approximately two orders of magnitude higher than that of polyvinyl alcohol. The other primary characteristics of the produced film, such as tensile strength, contact angle, and thermal stability, are also found to be superior to the materials made of other precursors, including polypropylene and polyethylene, discussed in the literature. The method of producing the films in this study is novel, simple, environmentally benign, and economically viable. Copyright © 2012 Elsevier B.V. All rights reserved.

Copper crystallite in carbon molecular sieves for selective oxygen removal

NASA Technical Reports Server (NTRS)

Sharma, Pramod K. (Inventor); Seshan, Panchalam K. (Inventor)

1993-01-01

Carbon molecular sieves modified by the incorporation of finely divided elemental copper useful for the selective sorption of oxygen at elevated temperatures. The carbon molecular sieves can be regenerated by reduction with hydrogen. The copper modified carbon molecular sieves are prepared by pyrolysis of a mixture of a copper-containing material and polyfurfuryl alcohol to form a sorbent precursor. The sorbent precursors are then heated and reduced to produce copper modified carbon molecular sieves. The copper modified carbon molecular sieves are useful for sorption of all concentrations of oxygen at temperatures up to about 200.degree. C. They are also useful for removal of trace amount of oxygen from gases at temperatures up to about 600.degree. C.

Hierarchical porous carbon microspheres derived from porous starch for use in high-rate electrochemical double-layer capacitors.

PubMed

Du, Si-Hong; Wang, Li-Qun; Fu, Xiao-Ting; Chen, Ming-Ming; Wang, Cheng-Yang

2013-07-01

Porous starch was used as a precursor for hierarchical porous carbon microspheres. The preparation consisted of stabilisation, carbonisation and KOH activation, and the resultant hierarchical porous carbon microspheres had a large BET surface area of 3251 m(2)g(-1). Due to the large surface area and the hierarchical pore structure, electrodes made of the hierarchical porous carbon microsphere materials had high specific capacitances of 304 Fg(-1) at a current density of 0.05 Ag(-1) and 197 Fg(-1) at a current density of 180 Ag(-1) when used in a symmetric capacitor with 6M KOH as the electrolyte. After 10,000 cycles, the capacitor still exhibited a stable performance with a capacitance retention of 98%. These results indicate that porous starch is an excellent precursor to prepare high performance electrode materials for EDLCs. Copyright © 2013 Elsevier Ltd. All rights reserved.

Nanoarchitectures for Metal-Organic Framework-Derived Nanoporous Carbons toward Supercapacitor Applications.

PubMed

Salunkhe, Rahul R; Kaneti, Yusuf Valentino; Kim, Jeonghun; Kim, Jung Ho; Yamauchi, Yusuke

2016-12-20

The future advances of supercapacitors depend on the development of novel carbon materials with optimized porous structures, high surface area, high conductivity, and high electrochemical stability. Traditionally, nanoporous carbons (NPCs) have been prepared by a variety of methods, such as templated synthesis, carbonization of polymer precursors, physical and chemical activation, etc. Inorganic solid materials such as mesoporous silica and zeolites have been successfully utilized as templates to prepare NPCs. However, the hard-templating methods typically involve several synthetic steps, such as preparation of the original templates, formation of carbon frameworks, and removal of the original templates. Therefore, these methods are not favorable for large-scale production. Metal-organic frameworks (MOFs) with high surface areas and large pore volumes have been studied over the years, and recently, enormous efforts have been made to utilize MOFs for electrochemical applications. However, their low conductivity and poor stability still present major challenges toward their practical applications in supercapacitors. MOFs can be used as precursors for the preparation of NPCs with high porosity. Their parent MOFs can be prepared with endless combinations of organic and inorganic constituents by simple coordination chemistry, and it is possible to control their porous architectures, pore volumes, surface areas, etc. These unique properties of MOF-derived NPCs make them highly attractive for many technological applications. Compared with carbonaceous materials prepared using conventional precursors, MOF-derived carbons have significant advantages in terms of a simple synthesis with inherent diversity affording precise control over porous architectures, pore volumes, and surface areas. In this Account, we will summarize our recent research developments on the preparation of three-dimensional (3-D) MOF-derived carbons for supercapacitor applications. This Account will be divided into three main sections: (1) useful background on carbon materials for supercapacitor applications, (2) the importance of MOF-derived carbons, and (3) potential future developments of MOF-derived carbons for supercapacitors. This Account focuses mostly on carbons derived from two types of MOFs, namely, zeolite imidazolate framework-8 (ZIF-8) and ZIF-67. By using examples from our previous works, we will show the uniqueness of these carbons for achieving high performance by control of the chemical reactions/conditions as well proper utilization in asymmetric/symmetric supercapacitor configurations. This Account will promote further developments of MOF-derived multifunctional carbon materials with controlled porous architectures for optimization of their electrochemical performance toward supercapacitor applications.

Microwave plasma CVD of NANO structured tin/carbon composites

DOEpatents

Marcinek, Marek [Warszawa, PL; Kostecki, Robert [Lafayette, CA

2012-07-17

A method for forming a graphitic tin-carbon composite at low temperatures is described. The method involves using microwave radiation to produce a neutral gas plasma in a reactor cell. At least one organo tin precursor material in the reactor cell forms a tin-carbon film on a supporting substrate disposed in the cell under influence of the plasma. The three dimensional carbon matrix material with embedded tin nanoparticles can be used as an electrode in lithium-ion batteries.

One-pot synthesis of transition metal ion-chelating ordered mesoporous carbon/carbon nanotube composites for active and durable fuel cell catalysts

NASA Astrophysics Data System (ADS)

Dombrovskis, Johanna K.; Palmqvist, Anders E. C.

2017-07-01

Development of non-precious metal catalysts for the oxygen reduction reaction (ORR) in proton exchange membrane (PEM) fuel cells with high activity and durability and with optimal water management properties is of outmost technological importance and highly challenging. Here we study the possibilities offered through judicious selection of small molecular precursors used for the formation of ordered mesoporous carbon-based non-precious metal ORR catalysts. By combining two complementary precursors, we present a one-pot synthesis that leads to a composite material consisting of transition metal ion-chelating ordered mesoporous carbon and multi-walled carbon nanotubes (TM-OMC/CNT). The resulting composite materials show high specific surface areas and a carbon structure that exhibits graphitic signatures. The synthesis procedure allows for tuning of the carbon structure, the surface area, the pore volume and the ratio of the two components of the composite. The TM-OMC/CNT composites were processed into membrane electrode assemblies and evaluated in single cell fuel cell measurements where they showed a combination of good ORR activity and very high durability.

Carbon Cryogel Silicon Composite Anode Materials for Lithium Ion Batteries

NASA Technical Reports Server (NTRS)

Woodworth James; Baldwin, Richard; Bennett, William

2010-01-01

A variety of materials are under investigation for use as anode materials in lithium-ion batteries, of which, the most promising are those containing silicon. 10 One such material is a composite formed via the dispersion of silicon in a resorcinol-formaldehyde (RF) gel followed by pyrolysis. Two silicon-carbon composite materials, carbon microspheres and nanofoams produced from nano-phase silicon impregnated RF gel precursors have been synthesized and investigated. Carbon microspheres are produced by forming the silicon-containing RF gel into microspheres whereas carbon nano-foams are produced by impregnating carbon fiber paper with the silicon containing RF gel to create a free standing electrode. 1-4,9 Both materials have demonstrated their ability to function as anodes and utilize the silicon present in the material. Stable reversible capacities above 400 mAh/g for the bulk material and above 1000 mAh/g of Si have been observed.

High-performance oxygen reduction catalysts in both alkaline and acidic fuel cells based on pre-treating carbon material and iron precursor

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

Song, Ping; Barkholtz, Heather M.; Wang, Ying

We demonstrate a new and simple method for pre-treating the carbon material and iron precursor to prepare oxygen reduction reaction (ORR) catalysts, which can produce super-high performance and stability in alkaline solution, with high performance in acid solution. This strategy using cheap materials is simply controllable. Moreover, it has achieved smaller uniform nanoparticles to exhibit high stability, and the synergetic effect of Fe and N offered much higher performance in ORR than commercial Pt/C, with high maximum power density in alkaline and acid fuel cell test. So it can make this kind of catalysts be the most promising alternatives ofmore » Pt-based catalysts with best performance/price.« less

Role of precursor crystal structure on electrochemical performance of carbide-derived carbon electrodes

NASA Astrophysics Data System (ADS)

Palazzo, Benjamin; Norris, Zach; Taylor, Greg; Yu, Lei; Lofland, Samuel; Hettinger, Jeffrey

2015-03-01

Binary carbides with hexagonal and cubic crystal structures have been synthesized by reactive magnetron sputtering of vanadium and other transition metals in acetylene or methane gas mixed with argon. The binary carbides are converted to carbide-derived carbon (CDC) films using chlorine gas in a post-deposition process in an external vacuum reaction furnace. Residual chlorine has been removed using an annealing step in a hydrogen atmosphere. The CDC materials have been characterized by x-ray diffraction, x-ray fluorescence, and scanning electron microscopy. The performance of the CDC materials in electrochemical device applications has been measured with the hexagonal phase precursor demonstrating a significantly higher specific capacitance in comparison to that of the cubic phase. We report these results and pore-size distributions of these and similar materials.

Biomorphous SiC ceramics prepared from cork oak as precursor

NASA Astrophysics Data System (ADS)

Yukhymchuk, V. O.; Kiselov, V. S.; Valakh, M. Ya.; Tryus, M. P.; Skoryk, M. A.; Rozhin, A. G.; Kulinich, S. A.; Belyaev, A. E.

2016-04-01

Porous ceramic materials of SiC were synthesized from carbon matrices obtained via pyrolysis of natural cork as precursor. We propose a method for the fabrication of complex-shaped porous ceramic hardware consisting of separate parts prepared from natural cork. It is demonstrated that the thickness of the carbon-matrix walls can be increased through their impregnation with Bakelite phenolic glue solution followed by pyrolysis. This decreases the material's porosity and can be used as a way to modify its mechanical and thermal characteristics. Both the carbon matrices (resulted from the pyrolysis step) and the resultant SiC ceramics are shown to be pseudomorphous to the structure of initial cork. Depending on the synthesis temperature, 3C-SiC, 6H-SiC, or a mixture of these polytypes, could be obtained. By varying the mass ratio of initial carbon and silicon components, stoichiometric SiC or SiC:C:Si, SiC:C, and SiC:Si ceramics could be produced. The structure, as well as chemical and phase composition of the prepared materials were studied by means of Raman spectroscopy and scanning electron microscopy.

Carbon reactivation kinetics in GaAs: Its dependence on dopant precursor, doping level, and layer thickness

NASA Astrophysics Data System (ADS)

Mimila-Arroyo, J.; Bland, S.; Barbé, M.

2002-05-01

The reactivation kinetics of the acceptor behavior of carbon, its dependence on dopant precursors, doping level, layer thickness, and annealing temperature, as well as the behavior of carbon-hydrogen complexes in GaAs grown by metalorganic chemical vapor deposition are studied. Independent of the carbon source, in the "as grown" material, systematically carbon hydrogen complexes are present and the hole concentration is lower than the corresponding carbon concentration. The carbon reactivation kinetics was achieved by ex situ rapid thermal annealing through a series of multistage annealing experiments and assessed at each annealing stage by infrared absorption, hydrogen secondary ion mass spectroscopy profiling, and hole concentration measurements. Carbon reactivation occurs solely by the debonding of hydrogen from the isolated carbon acceptor and its out-diffusion from the sample. The carbon reactivation kinetics can be treated as a first order one with an activation energy, Ea=1.42±0.01 eV, independent of doping precursors, doping level, and layer thickness. The reactivation constant results to decrease as doping level and layer thickness increase. An empirical formula has been obtained that allows one to calculate the reactivation constant as a function of the carbon doping, layer thickness, and annealing temperature, allowing one to determine the optimal carbon reactivation conditions for any C:GaAs layer.

Preparation of porous carbons from polymeric precursors modified with acrylated kraft lignin

NASA Astrophysics Data System (ADS)

Sobiesiak, M.

2016-04-01

The presented studies concern the preparation of porous carbons from a BPA.DA-St polymer containing acrylated kraft lignin as a monomer. The porous polymeric precursor in the form of microspheres was synthesized in suspension polymerization process. Next samples of the polymer were impregnated with acetic acid or aqueous solution of acetates (potassium or ammonia), dried and carbonised in nitrogen atmosphere at 450°C. After carbonization microspherical shape of the materials was remained, that is desired feature for potential application in chromatography or SPE technique. Chemical and textural properties of the porous carbon adsorbents were characterized using infrared spectroscopy (ATR-FTIR), thermogravimetry analyses with mass spectrometry of released gases (TG-MS) and nitrogen sorption experiments. The presented studies revealed the impregnation is useful method for development of porous structure of carbonaceous materials. The highest values of porous structure parameters were obtained when acetic acid and ammonium acetate were used as impregnating substances. On the surface of the materials oxygen functional groups are present that is important for specific interactions during sorption processes. The highest contents of functionalities were observed for carbon BPA.DA-St-LA-C-AcNH4.

Controllable Synthesis of Functional Hollow Carbon Nanostructures with Dopamine As Precursor for Supercapacitors.

PubMed

Liu, Chao; Wang, Jing; Li, Jiansheng; Luo, Rui; Shen, Jinyou; Sun, Xiuyun; Han, Weiqing; Wang, Lianjun

2015-08-26

N-doped hollow carbon spheres (N-HCSs) are promising candidates as electrode material for supercapacitor application. In this work, we report a facile one-step synthesis of discrete and highly dispersible N-HCSs with dopamine (DA) as a carbon precursor and TEOS as a structure-assistant agent in a mixture containing water, ethanol, and ammonia. The architectures of resultant N-HCSs, including yolk-shell hollow carbon spheres (YS-HCSs), single-shell hollow carbon spheres (SS-HCSs), and double-shells hollow carbon spheres (DS-HCSs), can be efficiently controlled through the adjustment of the amount of ammonia. To explain the relation and formation mechanism of these hollow carbon structures, the samples during the different synthetic steps, including polymer/silica spheres, carbon/silica spheres and silica spheres by combustion in air, were characterized by TEM. Electrochemical measurements performed on YS-HCSs, SS-HCSs, and DS-HCSs showed high capacitance with 215, 280, and 381 F g(-1), respectively. Moreover, all the nitrogen-doped hollow carbon nanospheres showed a good cycling stability 97.0% capacitive retention after 3000 cycles. Notably, the highest capacitance of DS-HCSs up to 381 F g(-1) is higher than the capacitance reported so far for many carbon-based materials, which may be attributed to the high surface area, hollow structure, nitrogen functionalization, and double-shell architecture. These kinds of N-doped hollow-structured carbon spheres may show promising prospects as advanced energy storage materials and catalyst supports.

Dry Process for Manufacturing Hybridized Boron Fiber/Carbon Fiber Thermoplastic Composite Materials from a Solution Coated Precursor

NASA Technical Reports Server (NTRS)

Belvin, Harry L. (Inventor); Cano, Roberto J. (Inventor)

2003-01-01

An apparatus for producing a hybrid boron reinforced polymer matrix composite from precursor tape and a linear array of boron fibers. The boron fibers are applied onto the precursor tapes and the precursor tape processed within a processing component having an impregnation bar assembly. After passing through variable-dimension forming nip-rollers, the precursor tape with the boron fibers becomes a hybrid boron reinforced polymer matrix composite. A driving mechanism is used to pulled the precursor tape through the method and a take-up spool is used to collect the formed hybrid boron reinforced polymer matrix composite.

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

Coker, Eric Nicholas; Miller, James E.

A thermal oxidation-reduction cycle is disclosed that uses iron titanium oxide as the reactive material. The cycle may be used for the thermal splitting of water and/or carbon dioxide to form hydrogen and/or carbon monoxide. The formed compounds may be used as syngas precursors to form fuels.

Encapsulating Reactive Nanoparticles in Carbon Nanotubes Using Flame-Based Synthesis

DTIC Science & Technology

2008-12-22

Results from the Aerosol Catalyst Method using Ferrocene as Precursor Running the experiment using a rich premixed flame seeded with ferrocene allows...flames with ferrocene seeding. There is significant catalyst nanoparticle production, encased within carbon material, namely CNTs. Resonant Raman

High performance carbon fibers from very high molecular weight polyacrylonitrile precursors

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

Morris, E. Ashley; Weisenberger, Matthew C.; Abdallah, Mohamed G.

In this study, carbon fibers are unique reinforcing agents for lightweight composite materials due to their outstanding mechanical properties and low density. Current technologies are capable of producing carbon fibers with 90-95% of the modulus of perfect graphite (~1025 GPa). However, these same carbon fibers possess less than 10% of the theoretical carbon fiber strength, estimated to be about 100 GPa.[1] Indeed, attempts to increase carbon fiber rigidity results in lower breaking strength. To develop advanced carbon fibers with both very high strength and modulus demands a new manufacturing methodology. Here, we report a method of manufacturing high strength, verymore » high modulus carbon fibers from a very high molecular weight (VHMW) polyacrylonitrile (PAN) precursor without the use of nanomaterial additives such as nucleating or structure-templating agents, as have been used by others.[2,3]« less

High performance carbon fibers from very high molecular weight polyacrylonitrile precursors

DOE PAGES

Morris, E. Ashley; Weisenberger, Matthew C.; Abdallah, Mohamed G.; ...

2016-02-02

In this study, carbon fibers are unique reinforcing agents for lightweight composite materials due to their outstanding mechanical properties and low density. Current technologies are capable of producing carbon fibers with 90-95% of the modulus of perfect graphite (~1025 GPa). However, these same carbon fibers possess less than 10% of the theoretical carbon fiber strength, estimated to be about 100 GPa.[1] Indeed, attempts to increase carbon fiber rigidity results in lower breaking strength. To develop advanced carbon fibers with both very high strength and modulus demands a new manufacturing methodology. Here, we report a method of manufacturing high strength, verymore » high modulus carbon fibers from a very high molecular weight (VHMW) polyacrylonitrile (PAN) precursor without the use of nanomaterial additives such as nucleating or structure-templating agents, as have been used by others.[2,3]« less

Evaluating biomass-derived hierarchically porous carbon as the positive electrode material for hybrid Na-ion capacitors

NASA Astrophysics Data System (ADS)

Chen, Jizhang; Zhou, Xiaoyan; Mei, Changtong; Xu, Junling; Zhou, Shuang; Wong, Ching-Ping

2017-02-01

As a promising renewable resource, biomass has several advantages such as wide availability, low cost, and versatility. In this study, we use peanut shell, wheat straw, rice straw, corn stalk, cotton stalk, and soybean stalk as the precursors to synthesize hierarchically porous carbon as the positive electrode material for hybrid Na-ion capacitors, aiming to establish a criterion of choosing suitable biomass precursors. The carbon derived from wood-like cotton stalk has abundant interconnected macropores, high surface area of 1994 m2 g-1, and large pore volume of 1.107 cm3 g-1, thanks to which it exhibits high reversible capacitance of 160.5 F g-1 at 0.2 A g-1 and great rate capability, along with excellent cyclability. The carbonaceous positive electrode material is combined with a Na2Ti2.97Nb0.03O7 negative electrode material to assemble a hybrid Na-ion capacitor, which delivers a high specific energy of 169.4 Wh kg-1 at 120.5 W kg-1, ranking among the best-performed hybrid ion capacitors.

25th anniversary article: "Cooking carbon with salt": carbon materials and carbonaceous frameworks from ionic liquids and poly(ionic liquid)s.

PubMed

Fellinger, Tim-Patrick; Thomas, Arne; Yuan, Jiayin; Antonietti, Markus

2013-11-06

This review surveys recent work on the use of ionic liquids (ILs) and polymerized ionic liquids (PILs) as precursors to synthesize functional carbon materials. As solvents or educts with negligible vapour pressure, these systems enable simple processing, composition, and structural control of the resulting carbons under rather simple and green synthesis conditions. Recent applications of the resulting nanocarbons across a multitude of fields, such as fuel cells, energy storage in batteries and supercapacitors, catalysis, separation, and sorption materials are highlighted. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The Synthesis of LiMnxFe1−xPO4/C Cathode Material through Solvothermal Jointed with Solid-State Reaction

PubMed Central

He, Xiangming; Wang, Jixian; Dai, Zhongjia; Wang, Li; Tian, Guangyu

2016-01-01

LiMnxFe1−xPO4/C material has been synthesized through a facile solid-state reaction under the condition of carbon coating, using solvothermal-prepared LiMnPO4 and LiFePO4 as precursors and sucrose as a carbon resource. XRD and element distribution analysis reveal completed solid-state reaction of precursors. LiMnxFe1−xPO4/C composites inherit the morphology of precursors after heat treatment without obvious agglomeration and size increase. LiMnxFe1−xPO4 solid solution forms at low temperature around 350 °C, and Mn2+/Fe2+ diffuse completely within 1 h at 650 °C. The LiMnxFe1−xPO4/C (x < 0.8) composite exhibits a high-discharge capacity of over 120 mAh·g−1 (500 Wh·kg−1) at low C-rates. This paves a way to synthesize the crystal-optimized LiMnxFe1−xPO4/C materials for high performance Li-ion batteries. PMID:28773887

Solid-state synthesis of YAG powders through microwave coupling of oxide/carbon particulate mixtures

DOE PAGES

Wildfire, Christina; Sabolsky, Edward M.; Spencer, Michael J.; ...

2017-06-14

The rapid synthesis of yttrium aluminum garnet (Y 3Al 15O 12, YAG) powder was investigated through the use of microwave irradiation of the oxide precursor system. For this investigation, an external hybrid heating source was not used. Instead, the rapid heating of the precursor materials (yttria and alumina powders, which are typically transparent to 2.45 GHz microwaves) was initiated by mixing an intrinsic absorbing material (carbon) into the original oxide precursors. The effect of the carbon characteristics, such as carbon source, concentration, particle size, and agglomerate microstructure were evaluated on the efficiency of coupling and resultant oxide reaction. The microwavemore » power was varied to optimize the YAG conversion and eliminate intermediate phase formation. Interactions between the conductive carbon particles and the dielectric oxides within the microwave exposure produced local arching and micro-plasma formation within the powder bed, resulting in the rapid formation of the refractory YAG composition. This optimal conduction led to temperatures of 1000°C that could be achieved in less than 5 min resulting in the formation of > 90 vol% YAG. The understanding of a conductor/dielectric particulate system here, provided insight into possible application of similar systems where microwave irradiation could be used for enhanced solid-state formation, local melting events, and gas phase reactions with a composite powder media.« less

Organosilicon Polymers as Precursors for Silicon Containing Ceramics: Recent Developments.

DTIC Science & Technology

1987-08-14

the polymer to a ceramic material, hopefully of the desired composition . In the latter alternative, shrinkage during pyrolysis should not be great...carbon-carbon composite materials. In order to have a useful preceramic polymer . considerations of structure and reactivitv are of paramount importance...process so that on pyrolysis non-volatile, three-dimensional networks (which lead to maximum weight retention) are formed. Thus. preceramic polymer

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

Wildfire, Christina; Sabolsky, Edward M.; Spencer, Michael J.

The rapid synthesis of yttrium aluminum garnet (Y 3Al 15O 12, YAG) powder was investigated through the use of microwave irradiation of the oxide precursor system. For this investigation, an external hybrid heating source was not used. Instead, the rapid heating of the precursor materials (yttria and alumina powders, which are typically transparent to 2.45 GHz microwaves) was initiated by mixing an intrinsic absorbing material (carbon) into the original oxide precursors. The effect of the carbon characteristics, such as carbon source, concentration, particle size, and agglomerate microstructure were evaluated on the efficiency of coupling and resultant oxide reaction. The microwavemore » power was varied to optimize the YAG conversion and eliminate intermediate phase formation. Interactions between the conductive carbon particles and the dielectric oxides within the microwave exposure produced local arching and micro-plasma formation within the powder bed, resulting in the rapid formation of the refractory YAG composition. This optimal conduction led to temperatures of 1000°C that could be achieved in less than 5 min resulting in the formation of > 90 vol% YAG. The understanding of a conductor/dielectric particulate system here, provided insight into possible application of similar systems where microwave irradiation could be used for enhanced solid-state formation, local melting events, and gas phase reactions with a composite powder media.« less

Hot wire production of single-wall and multi-wall carbon nanotubes

DOEpatents

Dillon, Anne C.; Mahan, Archie H.; Alleman, Jeffrey L.

2010-10-26

Apparatus (210) for producing a multi-wall carbon nanotube (213) may comprise a process chamber (216), a furnace (217) operatively associated with the process chamber (216), and at least one filament (218) positioned within the process chamber (216). At least one power supply (220) operatively associated with the at least one filament (218) heats the at least one filament (218) to a process temperature. A gaseous carbon precursor material (214) operatively associated with the process chamber (216) provides carbon for forming the multi-wall carbon nanotube (213). A metal catalyst material (224) operatively associated with the process (216) catalyzes the formation of the multi-wall carbon nanotube (213).

The hybrid nanostructure of MnCo2O4.5 nanoneedle/carbon aerogel for symmetric supercapacitors with high energy density

NASA Astrophysics Data System (ADS)

Hao, Pin; Zhao, Zhenhuan; Li, Liyi; Tuan, Chia-Chi; Li, Haidong; Sang, Yuanhua; Jiang, Huaidong; Wong, C. P.; Liu, Hong

2015-08-01

Current applications of carbon-based supercapacitors are limited by their low energy density. One promising strategy to enhance the energy density is to couple metal oxides with carbon materials. In this study, a porous MnCo2O4.5 nanoneedle/carbon aerogel hybrid nanostructure was synthesized by assembling MnCo2O4.5 nanoneedle arrays on the surface of channel walls of hierarchical porous carbon aerogels derived from chitosan for the supercapacitor application. The synthetic process of the hybrid nanostructure involves two steps, i.e. the growth of Mn-Co precursors on carbon aerogel by a hydrothermal process and the conversion of the precursor into MnCo2O4.5 nanoneedles by calcination. The carbon aerogel exhibits a high electrical conductivity, high specific surface area and porous structure, ensuring high electrochemical performance of the hybrid nanostructure when coupled with the porous MnCo2O4.5 nanoneedles. The symmetric supercapacitor using the MnCo2O4.5 nanoneedle/carbon aerogel hybrid nanostructure as the active electrode material exhibits a high energy density of about 84.3 Wh kg-1 at a power density of 600 W kg-1. The voltage window is as high as 1.5 V in neutral aqueous electrolytes. Due to the unique nanostructure of the electrodes, the capacitance retention reaches 86% over 5000 cycles.Current applications of carbon-based supercapacitors are limited by their low energy density. One promising strategy to enhance the energy density is to couple metal oxides with carbon materials. In this study, a porous MnCo2O4.5 nanoneedle/carbon aerogel hybrid nanostructure was synthesized by assembling MnCo2O4.5 nanoneedle arrays on the surface of channel walls of hierarchical porous carbon aerogels derived from chitosan for the supercapacitor application. The synthetic process of the hybrid nanostructure involves two steps, i.e. the growth of Mn-Co precursors on carbon aerogel by a hydrothermal process and the conversion of the precursor into MnCo2O4.5 nanoneedles by calcination. The carbon aerogel exhibits a high electrical conductivity, high specific surface area and porous structure, ensuring high electrochemical performance of the hybrid nanostructure when coupled with the porous MnCo2O4.5 nanoneedles. The symmetric supercapacitor using the MnCo2O4.5 nanoneedle/carbon aerogel hybrid nanostructure as the active electrode material exhibits a high energy density of about 84.3 Wh kg-1 at a power density of 600 W kg-1. The voltage window is as high as 1.5 V in neutral aqueous electrolytes. Due to the unique nanostructure of the electrodes, the capacitance retention reaches 86% over 5000 cycles. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr04421a

Converting a carbon preform object to a silicon carbide object

NASA Technical Reports Server (NTRS)

Levin, Harry (Inventor)

1990-01-01

A process for converting in depth a carbon or graphite preform object to a silicon carbide object, silicon carbide/silicon object, silicon carbide/carbon-core object, or a silicon carbide/silicon/carbon-core object, by contacting it with silicon liquid and vapor over various lengths of contact time in a reaction chamber. In the process, a stream comprised of a silicon-containing precursor material in gaseous phase below the decomposition temperature of said gas and a coreactant, carrier or diluent gas such as hydrogen is passed through a hole within a high emissivity, thin, insulating septum into the reaction chamber above the melting point of silicon. The thin septum has one face below the decomposition temperature of the gas and an opposite face exposed to the reaction chamber. Thus, the precursor gas is decomposed directly to silicon in the reaction chamber. Any stream of decomposition gas and any unreacted precursor gas from the reaction chamber is removed. A carbon or graphite preform object placed in the reaction chamber is contacted with the silicon. The carbon or graphite preform object is recovered from the reactor chamber after it has been converted to a desired silicon carbide, silicon and carbon composition.

Electric Pulse Discharge Activated Carbon Supercapacitors for Transportation Application

NASA Astrophysics Data System (ADS)

Nayak, Subhadarshi; Agrawal, Jyoti

2012-03-01

ScienceTomorrow is developing a high-speed, low-cost process for synthesizing high-porosity electrodes for electrochemical double-layer capacitors. Four types of coal (lignite, subbituminous, bituminous, and anthracite) were used as precursor materials for spark discharge activation with multiscale porous structure. The final porosity and pore distribution depended, among other factors, on precursor type. The high gas content in low-grade carbon resulted in mechanical disintegration, whereas high capacitance was attained in higher-grade coal. The properties, including capacitance, mechanical robustness, and internal conductivity, were excellent when the cost is taken into consideration.

Template-assisted mineral formation via an amorphous liquid phase precursor route

NASA Astrophysics Data System (ADS)

Amos, Fairland F.

The search for alternative routes to synthesize inorganic materials has led to the biomimetic route of producing ceramics. In this method, materials are manufactured at ambient temperatures and in aqueous solutions with soluble additives and insoluble matrix, similar to the biological strategy for the formation of minerals by living organisms. Using this approach, an anionic polypeptide additive was used to induce an amorphous liquid-phase precursor to either calcium carbonate or calcium phosphate. This precursor was then templated on either organic or inorganic substrates. Non-equilibrium morphologies, such as two-dimensional calcium carbonate films, one-dimensional calcium carbonate mesostructures and "molten" calcium phosphate spherulites were produced, which are not typical of the traditional (additive-free) solution grown crystals in the laboratory. In the study of calcium carbonate, the amorphous calcium carbonate mineral formed via the liquid-phase precursor, either underwent a dissolution-recrystallization event or a pseudo-solid-state transformation to produce different morphologies and polymorphs of the mineral. Discrete or aggregate calcite crystals were formed via the dissolution of the amorphous phase to allow the reprecipitation of the stable crystal. Non-equilibrium morphologies, e.g., films, mesotubules and mesowires were templated using organic and inorganic substrates and compartments. These structures were generated via an amorphous solid to crystalline solid transformation. Single crystalline tablets and mesowires of aragonite, which are reported to be found only in nature as skeletal structures of marine organisms, such as mollusk nacre and echinoderm teeth, were successfully synthesized. These biomimetic structures were grown via the polymer-induced liquid-phase precursor route in the presence of magnesium. Only low magnesium-bearing calcite was formed in the absence of the polymer. A similar approach of using a polymeric additive was implemented in calcium phosphate. Spherulitic crystals and films, seemingly formed from a molten state, were produced. These structures served as nucleating surfaces for the radial formation of calcium oxalate minerals. The composite calcium phosphate-calcium oxalate assemblies are similar to the core-shell structures found in certain kidney stones.

Nitrogen-doped ordered mesoporous carbon with a high surface area, synthesized through organic-inorganic coassembly, and its application in supercapacitors.

PubMed

Song, Yanfang; Li, Li; Wang, Yonggang; Wang, Congxiao; Guo, Zaipin; Xia, Yongyao

2014-07-21

A new nitrogen-doped ordered mesoporous carbon (N-doped OMC) is synthesized by using an organic-inorganic coassembly method, in which resol is used as the carbon precursor, dicyandiamide as the nitrogen precursor, silicate oligomers as the inorganic precursors, and F127 as the soft template. The N-doped OMC possesses a surface area as high as 1374 m(2)  g(-1) and a large pore size of 7.4 nm. As an electrode material for supercapacitors, the obtained carbon exhibits excellent cycling stability and delivers a reversible specific capacitance as high as 308 F g(-1) in 1 mol L(-1) H(2)SO(4) aqueous electrolyte, of which 58 % of the capacity is due to pseudo-capacitance. The large specific capacitance is attributed to proper pore size distributions, large surface area, and high nitrogen content. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A novel method to fabricate discrete porous carbon hemispheres and their electrochemical properties as supercapacitors.

PubMed

Chen, Jiafu; Lang, Zhanlin; Xu, Qun; Zhang, Jianan; Fu, Jianwei; Chen, Zhimin

2013-11-07

A simple and efficient method to produce discrete, hierarchical porous carbon hemispheres (CHs) with high uniformity has been successfully developed by constructing nanoreactors and using low crosslinked poly(styrene-co-divinylbenzene) (P(St-co-DVB)) capsules as precursors. The samples are characterized by scanning and transmission electron microscopy, Fourier transform infrared and Raman spectroscopy, X-ray diffraction, and N2 adsorption and desorption. Considering their application, the cyclic voltammetry and electrochemical impedance spectroscopy characterization are tested. The experimental results show that the achievement of discrete and perfect carbon hemispheres is dependent on the proper amount of DVB in the P(St-co-DVB) capsules, which can contribute to the ideal thickness or mechanical strength of the shells. When the amount of DVB is 35 wt% in the precursors, a high Brunauer-Emmett-Teller surface area of 676 m(2) g(-1) can be obtained for the carbon hemispheres, and the extremely large pore volume of 2.63 cm(3) g(-1) can also be achieved at the same time. The electrochemical test shows the carbon hemispheres have a higher specific capacitance of ca. 83 F g(-1) at 10 mV s(-1), compared to other carbon materials. So this method supplies a platform to extend the fabrication field of carbon materials and supplies more chances for the application of carbon materials including carbon hemispheres that are important components and substrates for supercapacitors.

Nitrogen-doped porous graphitic carbon as an excellent electrode material for advanced supercapacitors.

PubMed

Sun, Li; Tian, Chungui; Fu, Yu; Yang, Ying; Yin, Jie; Wang, Lei; Fu, Honggang

2014-01-07

An advanced supercapacitor material based on nitrogen-doped porous graphitic carbon (NPGC) with high a surface area was synthesized by means of a simple coordination-pyrolysis combination process, in which tetraethyl orthosilicate (TEOS), nickel nitrate, and glucose were adopted as porogent, graphitic catalyst precursor, and carbon source, respectively. In addition, melamine was selected as a nitrogen source owing to its nitrogen-enriched structure and the strong interaction between the amine groups and the glucose unit. A low-temperature treatment resulted in the formation of a NPGC precursor by combination of the catalytic precursor, hydrolyzed TEOS, and the melamine-glucose unit. Following pyrolysis and removal of the catalyst and porogent, the NPGC material showed excellent electrical conductivity owing to its high crystallinity, a large Brunauer-Emmett-Teller surface area (SBET =1027 m(2)  g(-1) ), and a high nitrogen level (7.72 wt %). The unusual microstructure of NPGC materials could provide electrochemical energy storage. The NPGC material, without the need for any conductive additives, showed excellent capacitive behavior (293 F g(-1) at 1 A g(-1) ), long-term cycling stability, and high coulombic efficiency (>99.9 % over 5000 cycles) in KOH when used as an electrode. Notably, in a two-electrode symmetric supercapacitor, NPGC energy densities as high as 8.1 and 47.5 Wh kg(-1) , at a high power density (10.5 kW kg(-1) ), were achieved in 6 M KOH and 1 M Et4 NBF4 -PC electrolytes, respectively. Thus, the synthesized NPGC material could be a highly promising electrode material for advanced supercapacitors and other conversion devices. Copyright © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Poultry litter-based activated carbon for removing heavy metal ions in water.

PubMed

Guo, Mingxin; Qiu, Guannan; Song, Weiping

2010-02-01

Utilization of poultry litter as a precursor material to manufacture activated carbon for treating heavy metal-contaminated water is a value-added strategy for recycling the organic waste. Batch adsorption experiments were conducted to investigate kinetics, isotherms, and capacity of poultry litter-based activated carbon for removing heavy metal ions in water. It was revealed that poultry litter-based activated carbon possessed significantly higher adsorption affinity and capacity for heavy metals than commercial activated carbons derived from bituminous coal and coconut shell. Adsorption of metal ions onto poultry litter-based carbon was rapid and followed Sigmoidal Chapman patterns as a function of contact time. Adsorption isotherms could be described by different models such as Langmuir and Freundlich equations, depending on the metal species and the coexistence of other metal ions. Potentially 404 mmol of Cu2+, 945 mmol of Pb2+, 236 mmol of Zn2+, and 250-300 mmol of Cd2+ would be adsorbed per kg of poultry litter-derived activated carbon. Releases of nutrients and metal ions from litter-derived carbon did not pose secondary water contamination risks. The study suggests that poultry litter can be utilized as a precursor material for economically manufacturing granular activated carbon that is to be used in wastewater treatment for removing heavy metals.

Sustaining PICA for Future NASA Robotic Science Missions Including NF-4 and Discovery

NASA Technical Reports Server (NTRS)

Stackpoole, Mairead; Venkatapathy, Ethiraj; Violette, Steven

2018-01-01

Phenolic Impregnated Carbon Ablator (PICA), invented in the mid 1990's, is a low-density ablative thermal protection material proven capable of meeting sample return mission needs from the moon, asteroids, comets and other "unrestricted class V destinations" as well as for Mars. Its low density and efficient performance characteristics have proven effective for use from Discovery to Flagship class missions. It is important that NASA maintain this TPS material capability and ensure its availability for future NASA use. The rayon based carbon precursor raw material used in PICA preform manufacturing required replacement and requalification at least twice in the past 25 years and a third substitution is now needed. The carbon precursor replacement challenge is twofold - the first involves finding a long-term replacement for the current rayon and the second is to assess its future availability periodically to ensure it is sustainable and be alerted if additional replacement efforts need to be initiated. Rayon is no longer a viable process in the US and Europe due to environmental concerns. In the early 80's rayon producers began investigating a new method of producing a cellulosic fiber through a more environmentally responsible process. This cellulosic fiber, lyocell, is a viable replacement precursor for PICA fiberform. This presentation reviews current SMD-PSD funded PICA sustainability activities in ensuring a rayon replacement for the long term is identified and in establishing that the capability of the new PICA derived from an alternative precursor is in family with previous versions of the so called "heritage" PICA.

Lignin-based active anode materials synthesized from low-cost renewable resources

DOEpatents

Rios, Orlando; Tenhaeff, Wyatt Evan; Daniel, Claus; Dudney, Nancy Johnston; Johs, Alexander; Nunnery, Grady Alexander; Baker, Frederick Stanley

2016-06-07

A method of making an anode includes the steps of providing fibers from a carbonaceous precursor, the carbon fibers having a glass transition temperature T.sub.g. In one aspect the carbonaceous precursor is lignin. The carbonaceous fibers are placed into a layered fiber mat. The fiber mat is fused by heating the fiber mat in the presence of oxygen to above the T.sub.g but no more than 20% above the T.sub.g to fuse fibers together at fiber to fiber contact points and without melting the bulk fiber mat to create a fused fiber mat through oxidative stabilization. The fused fiber mat is carbonized by heating the fused fiber mat to at least 650.degree. C. under an inert atmosphere to create a carbonized fused fiber mat. A battery anode formed from carbonaceous precursor fibers is also disclosed.

Hydrothermal development and characterization of the wear-resistant boron carbide from Pandanus: a natural carbon precursor

NASA Astrophysics Data System (ADS)

Saritha Devi, H. V.; Swapna, M. S.; Ambadas, G.; Sankararaman, S.

2018-04-01

Boron carbide (B4C) is a prominent semiconducting material that finds applications in the field of science and technology. The excellent physical, thermal and electronic properties make it suitable as ceramic armor, wear-resistant, lens polisher and neutron absorber in the nuclear industry. The existing methods of synthesis of boron carbide involve the use of toxic chemicals that adversely affect the environment. In the present work, we report for the first time the use of the hydrothermal method, for converting the cellulose from Pandanus leaves as the carbon precursor for the synthesis of B4C. The carbon precursor is changed into porous functionalized carbon by treating with sodium borohydride (NaBH4), followed by treating with boric acid to obtain B4C. The samples are characterized by scanning electron microscopy, X-ray diffraction, Fourier transform infrared, Raman, photoluminescent and Ultraviolet-Visible absorption spectroscopy. The formation of B4C from natural carbon source— Pandanus presents an eco-friendly, economic and non-toxic approach for the synthesis of refractory carbides.

Method for the preparation of high surface area high permeability carbons

DOEpatents

Lagasse, Robert R.; Schroeder, John L.

1999-05-11

A method for preparing carbon materials having high surface area and high macropore volume to provide high permeability. These carbon materials are prepared by dissolving a carbonizable polymer precursor, in a solvent. The solution is cooled to form a gel. The solvent is extracted from the gel by employing a non-solvent for the polymer. The non-solvent is removed by critical point drying in CO.sub.2 at an elevated pressure and temperature or evaporation in a vacuum oven. The dried product is heated in an inert atmosphere in a first heating step to a first temperature and maintained there for a time sufficient to substantially cross-link the polymer material. The cross-linked polymer material is then carbonized in an inert atmosphere.

Carbon material for hydrogen storage

DOEpatents

Bourlinos, Athanasios; Steriotis, Theodore; Stubos, Athanasios; Miller, Michael A

2016-09-13

The present invention relates to carbon based materials that are employed for hydrogen storage applications. The material may be described as the pyrolysis product of a molecular precursor such as a cyclic quinone compound. The pyrolysis product may then be combined with selected transition metal atoms which may be in nanoparticulate form, where the metals may be dispersed on the material surface. Such product may then provide for the reversible storage of hydrogen. The metallic nanoparticles may also be combined with a second metal as an alloy to further improve hydrogen storage performance.

MIL-100 derived nitrogen-embodied carbon shells embedded with iron nanoparticles

NASA Astrophysics Data System (ADS)

Mao, Chengyu; Kong, Aiguo; Wang, Yuan; Bu, Xianhui; Feng, Pingyun

2015-06-01

The use of metal-organic frameworks (MOFs) as templates and precursors to synthesize new carbon materials with controllable morphology and pre-selected heteroatom doping holds promise for applications as efficient non-precious metal catalysts. Here, we report a facile pyrolysis pathway to convert MIL-100 into nitrogen-doped carbon shells encapsulating Fe nanoparticles in a comparative study involving multiple selected nitrogen sources. The hierarchical porous architecture, embedded Fe nanoparticles, and nitrogen decoration endow this composite with a superior oxygen reduction activity. Furthermore, the excellent durability and high methanol tolerance even outperform the commercial Pt-C catalyst.The use of metal-organic frameworks (MOFs) as templates and precursors to synthesize new carbon materials with controllable morphology and pre-selected heteroatom doping holds promise for applications as efficient non-precious metal catalysts. Here, we report a facile pyrolysis pathway to convert MIL-100 into nitrogen-doped carbon shells encapsulating Fe nanoparticles in a comparative study involving multiple selected nitrogen sources. The hierarchical porous architecture, embedded Fe nanoparticles, and nitrogen decoration endow this composite with a superior oxygen reduction activity. Furthermore, the excellent durability and high methanol tolerance even outperform the commercial Pt-C catalyst. Electronic supplementary information (ESI) available: Material synthesis and elemental analysis, electrochemistry measurements, and additional figures. See DOI: 10.1039/c5nr02346g

Method for preparing metallated filament-wound structures

DOEpatents

Peterson, George R.

1979-01-01

Metallated graphite filament-wound structures are prepared by coating a continuous multi-filament carbon yarn with a metal carbide, impregnating the carbide coated yarn with a polymerizable carbon precursor, winding the resulting filament about a mandrel, partially curing the impregnation in air, subjecting the wound composite to heat and pressure to cure the carbon precursor, and thereafter heating the composite in a sizing die at a pressure loading of at least 1000 psi for graphitizing the carbonaceous material in the composite. The carbide in the composite coalesces into rod-like shapes which are disposed in an end-to-end relationship parallel with the filaments to provide resistance to erosion in abrasive laden atmospheres.

TOTAL ORGANIC CARBON ANALYZERS AS TOOLS FOR MEASURING CARBONACEOUS MATTER IN NATURAL WATERS

EPA Science Inventory

For some utilities, new US drinking water regulations may require removal of disinfection byproduct (DBP) precursor material as a means of mimnimizing DBP formation. The EPa's Stage 1 DBP Rule relies on total organic carbon (TOC) concentrations as a measure of the effectiveness o...

Preparation and CO 2 adsorption properties of soft-templated mesoporous carbons derived from chestnut tannin precursors

DOE PAGES

Nelson, Kimberly M.; Mahurin, Shannon Mark; Mayes, Richard T.; ...

2015-10-09

This paper presents a soft templating approach for mesoporous carbon using the polyphenolic heterogeneous biomass, chestnut tannin, as the carbon precursor. By varying synthesis parameters such as tannin:surfactant ratio, cross-linker, reaction time and acid catalyst, the pore structure could be controllably modulated from lamellar to a more ordered hexagonal array. Carbonization at 600 °C under nitrogen produced a bimodal micro-mesoporous carbonaceous material exhibiting enhanced hydrogen bonding with the soft template, similar to that shown by soft-templating of phenolic-formaldehyde resins, allowing for a tailorable pore size. By utilizing the acidic nature of chestnut tannin (i.e. gallic and ellagic acid), hexagonal-type mesostructuresmore » were formed without the use of an acid catalyst. The porous carbon materials were activated with ammonia to increase the available surface area and incorporate nitrogen-containing functionality which led to a maximum CO 2 adsorption capacity at 1 bar of 3.44 mmol/g and 2.27 mmol/g at 0 °C and 25 °C, respectively. The ammonia-activated carbon exhibited multiple peaks in the adsorption energy distribution which indicates heterogeneity of adsorption sites for CO 2 capture.« less

Activated carbon from biomass

NASA Astrophysics Data System (ADS)

Manocha, S.; Manocha, L. M.; Joshi, Parth; Patel, Bhavesh; Dangi, Gaurav; Verma, Narendra

2013-06-01

Activated carbon are unique and versatile adsorbents having extended surface area, micro porous structure, universal adsorption effect, high adsorption capacity and high degree of surface reactivity. Activated carbons are synthesized from variety of materials. Most commonly used on a commercial scale are cellulosic based precursors such as peat, coal, lignite wood and coconut shell. Variation occurs in precursors in terms of structure and carbon content. Coir having very low bulk density and porous structure is found to be one of the valuable raw materials for the production of highly porous activated carbon and other important factor is its high carbon content. Exploration of good low cost and non conventional adsorbent may contribute to the sustainability of the environment and offer promising benefits for the commercial purpose in future. Carbonization of biomass was carried out in a horizontal muffle furnace. Both carbonization and activation were performed in inert nitrogen atmosphere in one step to enhance the surface area and to develop interconnecting porosity. The types of biomass as well as the activation conditions determine the properties and the yield of activated carbon. Activated carbon produced from biomass is cost effective as it is easily available as a waste biomass. Activated carbon produced by combination of chemical and physical activation has higher surface area of 2442 m2/gm compared to that produced by physical activation (1365 m2/gm).

Amorphous calcium carbonate: A precursor phase for aragonite in shell disease of the pearl oyster.

PubMed

Huang, Jingliang; Liu, Chuang; Xie, Liping; Zhang, Rongqing

2018-02-26

Amorphous calcium carbonate (ACC) has long been shown to act as an important constituent or precursor phase for crystalline material in mollusks. However, the presence and the role of ACC in bivalve shell formation are not fully studied. In this study, we found that brown deposits containing heterogeneous calcium carbonates were precipitated when a shell disease occurred in the pearl oyster Pinctada fucata. Calcein-staining of the brown deposits indicated that numerous amorphous calcium deposits were present, which was further confirmed by Fourier-transform infrared spectroscopy (FTIR), Raman spectrum and X-ray difraction (XRD) analyses. So we speculate that ACC plays an important role in rapid calcium carbonate precipitation during shell repair process in diseased oysters. Copyright © 2018 Elsevier Inc. All rights reserved.

3-D dumbbell-like LiNi1/3Mn1/3Co1/3O2 cathode materials assembled with nano-building blocks for lithium-ion batteries

NASA Astrophysics Data System (ADS)

Ryu, Won-Hee; Lim, Sung-Jin; Kim, Won-Keun; Kwon, HyukSang

2014-07-01

Dumbbell-like microsphere carbonate precursors including multi-transition metal components (Ni1/3Mn1/3Co1/3CO3) assembled with nano-building blocks were synthesized by urea-assisted solvo/hydrothermal method, and layered cathode materials (LiNi1/3Mn1/3Co1/3O2) were subsequently prepared using the similarly shaped carbonate precursors for Li-ion batteries. For the synthesis of hierarchical microsphere structures, the partial addition of viscous organic solvent (e.g. ethylene glycol) in aqueous solution played a crucial role, not only in suppressing the sudden particle growth but also in regulating the directional crystallization of carbonate particles on the surface. The dumbbell-like LiNi1/3Mn1/3Co1/3O2 assembled with nanocubes prepared via the urea-assisted solvo/hydrothermal method exhibited better electrochemical characteristics, such as initial discharge capacity, cyclic performance, and rate-capability as a cathode material of Li-ion batteries, compared with the LiNi1/3Mn1/3Co1/3O2 materials prepared via the conventional co-precipitation method.

Nitro Lignin-Derived Nitrogen-Doped Carbon as an Efficient and Sustainable Electrocatalyst for Oxygen Reduction.

PubMed

Graglia, Micaela; Pampel, Jonas; Hantke, Tina; Fellinger, Tim-Patrick; Esposito, Davide

2016-04-26

The use of lignin as a precursor for the synthesis of materials is nowadays considered very interesting from a sustainability standpoint. Here we illustrate the synthesis of a micro-, meso-, and macroporous nitrogen-doped carbon (NDC) using lignin extracted from beech wood via alkaline hydrothermal treatment and successively functionalized via aromatic nitration. The so obtained material is thus carbonized in the eutectic salt melt KCl/ZnCl2. The final NDC shows an excellent activity as electrocatalyst for the oxygen reduction reaction.

A Unique 3D Nitrogen-Doped Carbon Composite as High-Performance Oxygen Reduction Catalyst

PubMed Central

Karunagaran, Ramesh; Tung, Tran Thanh; Tran, Diana; Coghlan, Campbell; Doonan, Christian

2017-01-01

The synthesis and properties of an oxygen reduction catalyst based on a unique 3-dimensional (3D) nitrogen doped (N-doped) carbon composite are described. The composite material is synthesised via a two-step hydrothermal and pyrolysis method using bio-source low-cost materials of galactose and melamine. Firstly, the use of iron salts and galactose to hydrothermally produceiron oxide (Fe2O3) magnetic nanoparticle clusters embedded carbon spheres. Secondly, magnetic nanoparticles diffused out of the carbon sphere when pyrolysed in the presence of melamine as nitrogen precursor. Interestingly, many of these nanoparticles, as catalyst-grown carbon nanotubes (CNTs), resulted in the formation of N-doped CNTs and N-doped carbon spheres under the decomposition of carbon and a nitrogen environment. The composite material consists of integrated N-doped carbon microspheres and CNTs show high ORR activity through a predominantly four-electron pathway. PMID:28792432

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

Methyl 3-[3',4'-(methylenedioxy)phenyl]-2-methyl glycidate: an ecstasy precursor seized in Sydney, Australia.

PubMed

Collins, Michael; Heagney, Aaron; Cordaro, Frank; Odgers, David; Tarrant, Gregory; Stewart, Samantha

2007-07-01

Five 44 gallon drums labeled as glycidyl methacrylate were seized by the Australian Customs Service and the Australian Federal Police at Port Botany, Sydney, Australia, in December 2004. Each drum contained a white, semisolid substance that was initially suspected to be 3,4-methylenedioxymethylamphetamine (MDMA). Gas chromatography-mass spectroscopy (GC/MS) analysis demonstrated that the material was neither glycidyl methacrylate nor MDMA. Because intelligence sources employed by federal agents indicated that this material was in some way connected to MDMA production, suspicion fell on the various MDMA precursor chemicals. Using a number of techniques including proton nuclear magnetic resonance spectroscopy ((1)H NMR), carbon nuclear magnetic resonance spectroscopy ((13)C NMR), GC/MS, infrared spectroscopy, and total synthesis, the unknown substance was eventually identified as methyl 3-[3',4'(methylenedioxy)phenyl]-2-methyl glycidate. The substance was also subjected to a published hydrolysis and decarboxylation procedure and gave a high yield of the MDMA precursor chemical, 3,4-methylenedioxyphenyl-2-propanone, thereby establishing this material as a "precursor to a precursor."

Method for the preparation of high surface area high permeability carbons

DOEpatents

Lagasse, R.R.; Schroeder, J.L.

1999-05-11

A method for preparing carbon materials having high surface area and high macropore volume to provide high permeability. These carbon materials are prepared by dissolving a carbonizable polymer precursor, in a solvent. The solution is cooled to form a gel. The solvent is extracted from the gel by employing a non-solvent for the polymer. The non-solvent is removed by critical point drying in CO{sub 2} at an elevated pressure and temperature or evaporation in a vacuum oven. The dried product is heated in an inert atmosphere in a first heating step to a first temperature and maintained there for a time sufficient to substantially cross-link the polymer material. The cross-linked polymer material is then carbonized in an inert atmosphere. 3 figs.

Fluidized bed deposition of diamond

DOEpatents

Laia, Jr., Joseph R.; Carroll, David W.; Trkula, Mitchell; Anderson, Wallace E.; Valone, Steven M.

1998-01-01

A process for coating a substrate with diamond or diamond-like material including maintaining a substrate within a bed of particles capable of being fluidized, the particles having substantially uniform dimensions and the substrate characterized as having different dimensions than the bed particles, fluidizing the bed of particles, and depositing a coating of diamond or diamond-like material upon the substrate by chemical vapor deposition of a carbon-containing precursor gas mixture, the precursor gas mixture introduced into the fluidized bed under conditions resulting in excitation mechanisms sufficient to form the diamond coating.

Precursors of Halobenzoquinones and Their Removal During Drinking Water Treatment Processes.

PubMed

Wang, Wei; Qian, Yichao; Jmaiff, Lindsay K; Krasner, Stuart W; Hrudey, Steve E; Li, Xing-Fang

2015-08-18

Halobenzoquinones (HBQs) widely occur in drinking water treatment plant (DWTP) effluents; however, HBQ precursors and their removal by treatments remain unclear. Thus, we have investigated HBQ precursors in plant influents and their removal by each treatment before chlorination in nine DWTPs. The levels of HBQ precursors were determined using formation potential (FP) tests for 2,6-dichloro-1,4-benzoquinone (DCBQ), 2,3,6-trichloro-1,4-benzoquinone (TCBQ), 2,6-dichloro-3-methyl-1,4-benzoquinone (DCMBQ), and 2,6-dibromo-1,4-benzoquinone (DBBQ). HBQ precursors were present in all plant influents. DCBQ precursors were the most abundant (DCBQ FP up to 205 ng/L). Coagulation removed dissolved organic carbon (DOC) (up to 56%) and HBQ precursors (up to 39% for DCBQ). The level of removal of DOC was significantly greater than the level of removal of HBQ FP, suggesting that organic matter removed by coagulation had a high proportion of non-HBQ-precursor material. Granular activated carbon (GAC) decreased the level of HBQ FPs by 10-20%, where DOC removal was only 0.2-4.7%, suggesting that the GAC was not in the adsorption mode and biodegradation of HBQ precursors may have been occurring. Ozonation destroyed/transformed HBQ FPs by 10-30%, whereas anthracite/sand filtration and UV irradiation appeared to have no impact. The results demonstrated that the combined treatments did not substantially reduce HBQ precursor levels in water.

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

Eilert, André; Roberts, F. Sloan; Friebel, Daniel

Nanostructured copper cathodes are among the most efficient and selective catalysts to date for making multicarbon products from the electrochemical carbon dioxide reduction reaction (CO 2RR). We report an in situ X-ray absorption spectroscopy investigation of the formation of a copper nanocube CO 2RR catalyst with high activity that highly favors ethylene over methane production. The results show that the precursor for the copper nanocube formation is copper(I)-oxide, not copper(I)-chloride as previously assumed. A second route to an electrochemically similar material via a copper(II)–carbonate/hydroxide is also reported. In conclusion, this study highlights the importance of using oxidized copper precursors formore » constructing selective CO 2 reduction catalysts and shows the precursor oxidation state does not affect the electrocatalyst selectivity toward ethylene formation.« less

Level 3 material characterization of NARC HRPF, HRHU, HRHF, and HRPU

NASA Technical Reports Server (NTRS)

Tobias, Mark E.

1993-01-01

The North American Rayon Corporation (NARC) precursor was developed, qualified, and characterized for Space Shuttle nozzle carbon-cloth phenolic ablative materials in three distinct phases. The characterization phase includes thermal and structural material property analysis and comparisons. This report documents the thermal and structural material property characterization performed by Southern Research Institute (SRI) on the two NARC baseline and two crossover materials.

Natural cotton as precursor for the refractory boron carbide—a hydrothermal synthesis and characterization

NASA Astrophysics Data System (ADS)

Saritha Devi, H. V.; Swapna, M. S.; Raj, Vimal; Ambadas, G.; Sankararaman, S.

2018-01-01

Boron carbide (B4C) is an excellent covalent carbide that finds applications in industries and nuclear power plants. The present synthesis methods of boron carbide are expensive and involve the use of toxic chemicals that adversely affect environment. In the present work, we report for the first time the use of the hydrothermal method for converting the cellulose from cotton as the carbon precursor for B4C. The carbon precursor is converted into functionalized porous carbonaceous material by hydrothermal treatment followed by sodium borohydride. It is further treated with boric acid to make it a B4C precursor. The precursor is characterized by UV-visible diffuse reflectance, Raman, Fourier transform infrared, photoluminescent and energy dispersive spectroscopy. The morphology and structure analysis is carried out using field emission scanning electron microscopy and x-ray diffraction techniques. The results of structural and optical characterization of the sample synthesized are compared with the commercial B4C. The thermal stability of the sample is studied by thermogravimetric analysis. The sample annealed at 700 °C is found to be B4C devoid of amorphous carbon with a yield of 44.7%. The analysis reveals the formation of boron carbide from the sample.

Characterization and electrochemical application of carbon materials based on poly(phenylene oxide)

NASA Astrophysics Data System (ADS)

Gray, Hunter

Carbon materials possess excellent electrical and surface properties for the next generation of energy storage devices. Polymers provide a carbon rich and tailorable precursor for the production of carbon materials. Therefore, activated carbons were prepared from poly(2,6-dimethyl-1,4-phenylene oxide) (PPO) via a three step process: thermal oxidation, carbonization, and activation with KOH. The activated carbons are predominately microporous with BET specific surface areas up to 2638 m2/g. Impedance spectroscopy revealed these carbons possess electrical conductivities comparable to commercial carbon blacks and consequently were employed in thin-film composite electrodes in electrochemical double-layer capacitors. Cyclic voltammetry confirmed maximum specific capacitances of 13.23 F/g and 2.848 F/g for aqueous and organic electrolyte systems, respectively. Additionally, carbon nanotubes were synthesized from PPO and other polymers with a nickel catalyst via chemical vapor deposition as revealed by transmission electron microscopy. This is the first report of carbon nanotubes produced from PPO.

Material State Awareness for Composites Part II: Precursor Damage Analysis and Quantification of Degraded Material Properties Using Quantitative Ultrasonic Image Correlation (QUIC)

PubMed Central

Patra, Subir; Banerjee, Sourav

2017-01-01

Material state awareness of composites using conventional Nondestructive Evaluation (NDE) method is limited by finding the size and the locations of the cracks and the delamination in a composite structure. To aid the progressive failure models using the slow growth criteria, the awareness of the precursor damage state and quantification of the degraded material properties is necessary, which is challenging using the current NDE methods. To quantify the material state, a new offline NDE method is reported herein. The new method named Quantitative Ultrasonic Image Correlation (QUIC) is devised, where the concept of microcontinuum mechanics is hybrid with the experimentally measured Ultrasonic wave parameters. This unique combination resulted in a parameter called Nonlocal Damage Entropy for the precursor awareness. High frequency (more than 25 MHz) scanning acoustic microscopy is employed for the proposed QUIC. Eight woven carbon-fiber-reinforced-plastic composite specimens were tested under fatigue up to 70% of their remaining useful life. During the first 30% of the life, the proposed nonlocal damage entropy is plotted to demonstrate the degradation of the material properties via awareness of the precursor damage state. Visual proofs for the precursor damage states are provided with the digital images obtained from the micro-optical microscopy, the scanning acoustic microscopy and the scanning electron microscopy. PMID:29258256

Cauliflower-derived porous carbon without activation for electrochemical capacitor and CO2 capture applications

NASA Astrophysics Data System (ADS)

Du, Juan; Yu, Yifeng; Lv, Haijun; Chen, Chunlin; Zhang, Jian; Chen, Aibing

2018-01-01

Carbon materials have attracted great attention in CO2 capture and energy storage due to their excellent characteristics such as tunable pore structure, modulated surface properties and superior bulk conductivities, etc. Biomass, provided by nature with non-toxic, widespread, abundant, and sustainable advantages, is considered to be a very promising precursor of carbons for the view of economic, environmental, and societal issues. However, the preparation of high-performance biomass-derived carbons is still a big challenge because of the multistep process for their synthesis and subsequent activation. Herein, hierarchically porous structured carbon materials have been prepared by directly carbonizing dried cauliflowers without any addition of agents and activation process, featuring with large specific surface area, hierarchically porous structure and improved pore volume, as well as suitable nitrogen content. Being used as a solid-state CO2 adsorbent, the obtained product exhibited a high CO2 adsorption capacity of 3.1 mmol g-1 under 1 bar and 25 °C and a remarkable reusability of 96.7% retention after 20 adsorption/regeneration cycles. Our study reveals that choosing a good biomass source was significant as the unique structure of precursor endows the carbonized product with abundant pores without the need of any post-treatment. Used as an electrode material in electrochemical capacitor, the non-activated porous carbon displayed a fairly high specific capacitance of 228.9 F g-1 at 0.5 A g-1 and an outstanding stability of 99.2% retention after 5000 cycles at 5 A g-1. [Figure not available: see fulltext.

Soft and wrinkled carbon membranes derived from petals for flexible supercapacitors

PubMed Central

Yu, Xiuxiu; Wang, Ying; Li, Li; Li, Hongbian; Shang, Yuanyuan

2017-01-01

Biomass materials are promising precursors for the production of carbonaceous materials due to their abundance, low cost and renewability. Here, a freestanding wrinkled carbon membrane (WCM) electrode material for flexible supercapacitors (SCs) was obtained from flower petal. The carbon membrane was fabricated by a simple thermal pyrolysis process and further activated by heating the sample in air. As a binder and current collector-free electrode, the activated wrinkled carbon membrane (AWCM) exhibited a high specific capacitance of 332.7 F/g and excellent cycling performance with 92.3% capacitance retention over 10000 cycles. Moreover, a flexible all-solid supercapacitor with AWCM electrode was fabricated and showed a maximum specific capacitance of 154 F/g and great bending stability. The development of this flower petal based carbon membrane provides a promising cost-effective and environmental benign electrode material for flexible energy storage. PMID:28361914

Nitrogen doped carbon derived from polyimide/multiwall carbon nanotube composites for high performance flexible all-solid-state supercapacitors

NASA Astrophysics Data System (ADS)

Kim, Dae Kyom; Kim, Nam Dong; Park, Seung-Keun; Seong, Kwang-dong; Hwang, Minsik; You, Nam-Ho; Piao, Yuanzhe

2018-03-01

Flexible all-solid-state supercapacitors are desirable as potential energy storage systems for wearable technologies. Herein, we synthesize aminophenyl multiwall carbon nanotube (AP-MWCNT) grafted polyimide precursor by in situ polymerization method as a nitrogen-doped carbon precursor. Flexible supercapacitor electrodes are fabricated via a coating of carbon precursor on carbon cloth surface and carbonization at high temperature directly. The as-obtained electrodes, which can be directly used without any binders or additives, can deliver a high specific capacitance of 333.4 F g-1 at 1 A g-1 (based on active material mass) and excellent cycle stability with 103% capacitance retention after 10,000 cycles in a three-electrode system. The flexible all-solid-state supercapacitor device exhibits a high volumetric capacitance of 3.88 F cm-3 at a current density of 0.02 mA cm-3. And also the device can deliver a maximum volumetric energy density of 0.50 mWh cm-3 and presents good cycling stability with 85.3% capacitance retention after 10,000 cycles. This device cell can not only show extraordinary mechanical flexibilities allowing folding, twisting, and rolling but also demonstrate remarkable stable electrochemical performances under their forms. This work provides a novel approach to obtain carbon textile-based flexible supercapacitors with high electrochemical performance and mechanical flexibility.

Porous nitrogen-doped carbon derived from silk fibroin protein encapsulating sulfur as a superior cathode material for high-performance lithium-sulfur batteries.

PubMed

Zhang, Jiawei; Cai, Yurong; Zhong, Qiwei; Lai, Dongzhi; Yao, Juming

2015-11-14

The features of a carbon substrate are crucial for the electrochemical performance of lithium-sulfur (Li-S) batteries. Nitrogen doping of carbon materials is assumed to play an important role in sulfur immobilisation. In this study, natural silk fibroin protein is used as a precursor of nitrogen-rich carbon to fabricate a novel, porous, nitrogen-doped carbon material through facile carbonisation and activation. Porous carbon, with a reversible capacity of 815 mA h g(-1) at 0.2 C after 60 cycles, serves as the cathode material in Li-S batteries. Porous carbon retains a reversible capacity of 567 mA h g(-1), which corresponds to a capacity retention of 98% at 1 C after 200 cycles. The promising electrochemical performance of porous carbon is attributed to its mesoporous structure, high specific surface area and nitrogen doping into the carbon skeleton. This study provides a general strategy to synthesise nitrogen-doped carbons with a high specific surface area, which is crucial to improve the energy density and electrochemical performance of Li-S batteries.

Weak-link capacitor

DOEpatents

Dirk, Shawn M [Albuquerque, NM; Johnson, Ross S [Albuquerque, NM; Wheeler, David R [Albuquerque, NM; Bogart, Gregory R [Corrales, NM

2011-06-07

A process for making a dielectric material where a precursor polymer selected from poly(phenylene vinylene) polyacetylene, poly(p-phenylene), poly(thienylene vinylene), poly(1,4-naphthylene vinylene), and poly(p-pyridine vinylene) is energized said by exposure by radiation or increase in temperature to a level sufficient to eliminate said leaving groups contained within the precursor polymer, thereby transforming the dielectric material into a conductive polymer. The leaving group in the precursor polymer can be a chloride, a bromide, an iodide, a fluoride, an ester, an xanthate, a nitrile, an amine, a nitro group, a carbonate, a dithiocarbamate, a sulfonium group, an oxonium group, an iodonium group, a pyridinium group, an ammonium group, a borate group, a borane group, a sulphinyl group, or a sulfonyl group.

Weak-link capacitor

DOEpatents

Dirk, Shawn M.; Johnson, Ross S.; Wheeler, David R.; Bogart, Gregory R.

2013-04-23

A process for making a dielectric material where a precursor polymer selected from poly(phenylene vinylene)polyacetylene, poly(p-phenylene), poly(thienylene vinylene), poly(1,4-naphthylene vinylene), and poly(p-pyridine vinylene) is energized said by exposure by radiation or increase in temperature to a level sufficient to eliminate said leaving groups contained within the precursor polymer, thereby transforming the dielectric material into a conductive polymer. The leaving group in the precursor polymer can be a chloride, a bromide, an iodide, a fluoride, an ester, an xanthate, a nitrile, an amine, a nitro group, a carbonate, a dithiocarbamate, a sulfonium group, an oxonium group, an iodonium group, a pyridinium group, an ammonium group, a borate group, a borane group, a sulphinyl group, or a sulfonyl group.

The hybrid nanostructure of MnCo2O4.5 nanoneedle/carbon aerogel for symmetric supercapacitors with high energy density.

PubMed

Hao, Pin; Zhao, Zhenhuan; Li, Liyi; Tuan, Chia-Chi; Li, Haidong; Sang, Yuanhua; Jiang, Huaidong; Wong, C P; Liu, Hong

2015-09-14

Current applications of carbon-based supercapacitors are limited by their low energy density. One promising strategy to enhance the energy density is to couple metal oxides with carbon materials. In this study, a porous MnCo2O4.5 nanoneedle/carbon aerogel hybrid nanostructure was synthesized by assembling MnCo2O4.5 nanoneedle arrays on the surface of channel walls of hierarchical porous carbon aerogels derived from chitosan for the supercapacitor application. The synthetic process of the hybrid nanostructure involves two steps, i.e. the growth of Mn-Co precursors on carbon aerogel by a hydrothermal process and the conversion of the precursor into MnCo2O4.5 nanoneedles by calcination. The carbon aerogel exhibits a high electrical conductivity, high specific surface area and porous structure, ensuring high electrochemical performance of the hybrid nanostructure when coupled with the porous MnCo2O4.5 nanoneedles. The symmetric supercapacitor using the MnCo2O4.5 nanoneedle/carbon aerogel hybrid nanostructure as the active electrode material exhibits a high energy density of about 84.3 Wh kg(-1) at a power density of 600 W kg(-1). The voltage window is as high as 1.5 V in neutral aqueous electrolytes. Due to the unique nanostructure of the electrodes, the capacitance retention reaches 86% over 5000 cycles.

Fabrication of carbonate apatite block based on internal dissolution-precipitation reaction of dicalcium phosphate and calcium carbonate.

PubMed

Daitou, Fumikazu; Maruta, Michito; Kawachi, Giichiro; Tsuru, Kanji; Matsuya, Shigeki; Terada, Yoshihiro; Ishikawa, Kunio

2010-05-01

In this study, we investigated a novel method for fabrication of carbonate apatite block without ionic movement between precursor and solution by using precursor that includes all constituent ions of carbonate apatite. A powder mixture prepared from dicalcium phosphate anhydrous and calcite at appropriate Ca/P ratios (1.5, 1.67, and 1.8) was used as starting material. For preparation of specimens, the slurry made from the powder mixture and distilled water was packed in a split stainless steel mold and heat - treated, ranging from 60 degrees C to 100 degrees C up to 48 hours at 100% humidity. It appeared that carbonate apatite could be obtained above 70 degrees C and monophasic carbonate apatite could be obtained from the powder mixture at Ca/P ratio of 1.67. Carbonate content of the specimen was about 5-7%. Diametral tensile strength of the carbonate apatite blocks slightly decreased with increasing treatment temperature. The decrease in diametral tensile strength is thought to be related to the crystal size of the carbonate apatite formed.

Intrinsic activation: the relationship between biomass inorganic content and porosity formation during pyrolysis.

PubMed

Stratford, James P; Hutchings, Tony R; de Leij, Frans A A M

2014-05-01

The utility of pyrolytic carbons is closely related to their porosity and surface area, there is a clear benefit to the development of biomass pyrolysis processes which produce highly porous carbons. The results presented in this work demonstrate that by using biomass precursors with high inorganic content along with specified process conditions, carbons can be consistently produced with specific surface areas between 900 and 1600 m(2)/g. Results from 12 different source materials show that the formation of increased porosity in pyrolytic carbons is strongly associated with the presence of inorganic elements in the precursors including: magnesium, potassium and sulfur. It was found that pyrolysis of macro-algae can produce especially high specific surface area carbons (mean: 1500 m(2)/g), without externally applied activating agents. Using cheap readily available agricultural residues such as oilseed rape straw, pyrolytic carbons can be produced with specific surface areas of around 950 m(2)/g. Copyright © 2014 Elsevier Ltd. All rights reserved.

Use of organic precursors and graphenes in the controlled synthesis of carbon-containing nanomaterials for energy storage and conversion.

PubMed

Yang, Shubin; Bachman, Robert E; Feng, Xinliang; Müllen, Klaus

2013-01-15

The development of high-performance electrochemical energy storage and conversion devices, including supercapacitors, lithium-ion batteries, and fuel cells, is an important step on the road to alternative energy technologies. Carbon-containing nanomaterials (CCNMs), defined here as pure carbon materials and carbon/metal (oxide, hydroxide) hybrids with structural features on the nanometer scale, show potential application in such devices. Because of their pronounced electrochemical activity, high chemical and thermal stability and low cost, researchers are interested in CCNMs to serve as electrodes in energy-related devices. Various all-carbon materials are candidates for electrochemical energy storage and conversion devices. Furthermore, carbon-based hybrid materials, which consist of a carbon component with metal oxide- or metal hydroxide-based nanostructures, offer the opportunity to combine the attractive properties of these two components and tune the behavior of the resulting materials. As such, the design and synthesis of CCNMs provide an attractive route for the construction of high-performance electrode materials. Studies in these areas have revealed that both the composition and the fabrication protocol employed in preparing CCNMs influence the morphology and microstructure of the resulting material and its electrochemical performance. Consequently, researchers have developed several synthesis strategies, including hard-templated, soft-templated, and template-free synthesis of CCNMs. In this Account, we focus on recent advances in the controlled synthesis of such CCNMs and the potential of the resulting materials for energy storage or conversion applications. The Account is divided into four major categories based on the carbon precursor employed in the synthesis: low molecular weight organic or organometallic molecules, hyperbranched or cross-linked polymers consisting of aromatic subunits, self-assembling discotic molecules, and graphenes. In each case, we highlight representative examples of CCNMs with both new nanostructures and electrochemical performance suitable for energy storage or conversion applications. In addition, this Account provides an overall perspective on the current state of efforts aimed at the controlled synthesis of CCNMs and identifies some of the remaining challenges.

Molten carbonate fuel cell cathode with mixed oxide coating

DOEpatents

Hilmi, Abdelkader; Yuh, Chao-Yi

2013-05-07

A molten carbonate fuel cell cathode having a cathode body and a coating of a mixed oxygen ion conductor materials. The mixed oxygen ion conductor materials are formed from ceria or doped ceria, such as gadolinium doped ceria or yttrium doped ceria. The coating is deposited on the cathode body using a sol-gel process, which utilizes as precursors organometallic compounds, organic and inorganic salts, hydroxides or alkoxides and which uses as the solvent water, organic solvent or a mixture of same.

Vanadium oxide-carbon nanotube composite electrodes for energy storage by supercritical fluid deposition: experiment design and device performance

NASA Astrophysics Data System (ADS)

Do, Quyet H.; Fielitz, Thomas R.; Zeng, Changchun; Arda Vanli, O.; Zhang, Chuck; Zheng, Jim P.

2013-08-01

Vanadium pentoxide (V2O5) deposited on porous multiwalled carbon nanotube (MWCNT) buckypaper using supercritical fluid CO2(scCO2) deposition shows excellent performance for electrochemical capacitors. However, the low weight loading of V2O5 is one of the main problems. In this paper, design of experiments and response surface methods were employed to explore strategies for improving the active material loading by increasing the organo-vanadium precursor adsorption. A second-order response surface model was fitted to the designed experiments to predict the loading of the vanadium precursors onto carbon nanotube buckypaper as a function of time, temperature and pressure of CO2, buckypaper functionalization, precursor type, initial precursor mass and stir speed. Operation conditions were identified by employing a model that led to a precursor loading of 19.33%, an increase of 72.28% over the initial screening design. CNTs-V2O5 composite electrodes fabricated from deposited samples using the optimized conditions demonstrated outstanding electrochemical performance (947.1 F g-1 of V2O5 at a high scan rate 100 mV s-1). The model also predicted operation conditions under which light precursor aggregation took place. The V2O5 from aggregated precursor still possessed considerable specific capacitance (311 F g-1 of V2O5 at a scan rate 100 mV s-1), and the significantly higher V2O5 loading (˜81%) contributed to an increase in overall electrode capacitance.

Composite catalysts supported on modified carbon substrates and methods of making the same

DOEpatents

Popov, Branko N [Columbia, SC; Subramanian, Nalini [Kennesaw, GA; Colon-Mercado, Hector R [Columbia, SC

2009-11-17

A method of producing a composite carbon catalyst is generally disclosed. The method includes oxidizing a carbon precursor (e.g., carbon black). Optionally, nitrogen functional groups can be added to the oxidized carbon precursor. Then, the oxidized carbon precursor is refluxed with a non-platinum transitional metal precursor in a solution. Finally, the solution is pyrolyzed at a temperature of at least about 500.degree. C.

Nitrogen-doped carbon-supported cobalt-iron oxygen reduction catalyst

DOEpatents

Zelenay, Piotr; Wu, Gang

2014-04-29

A Fe--Co hybrid catalyst for oxygen reaction reduction was prepared by a two part process. The first part involves reacting an ethyleneamine with a cobalt-containing precursor to form a cobalt-containing complex, combining the cobalt-containing complex with an electroconductive carbon supporting material, heating the cobalt-containing complex and carbon supporting material under conditions suitable to convert the cobalt-containing complex and carbon supporting material into a cobalt-containing catalyst support. The second part of the process involves polymerizing an aniline in the presence of said cobalt-containing catalyst support and an iron-containing compound under conditions suitable to form a supported, cobalt-containing, iron-bound polyaniline species, and subjecting said supported, cobalt-containing, iron bound polyaniline species to conditions suitable for producing a Fe--Co hybrid catalyst.

Pilot Scale Production of Activated Carbon Spheres Using Fluidized Bed Reactor and Its Evaluation for the Removal of Hexavalent Chromium from Aqueous Solutions

NASA Astrophysics Data System (ADS)

Tripathi, Nagesh Kumar; Sathe, Manisha

2017-12-01

Large scale production of activated carbon is need of ongoing research due to its excellent adsorption capacity for removal of heavy metals from contaminated solutions. In the present study, polymeric precursor polystyrene beads [Brunauer Emmett Teller (BET) surface area, 46 m2/g; carbon content, 40.64%; crushing strength, 0.32 kg/sphere] were used to produce a new variant of activated carbon, Activated Carbon Spheres (ACS) in a pilot scale fluidized bed reactor. ACS were prepared by carbonization of polymeric precursor at 850 °C followed by activation of resultant material with steam. Prepared ACS were characterized using scanning electron microscope, CHNS analyzer, thermogravimetric analyzer, surface area analyzer and crushing strength tester. The produced ACS have 1009 m2/g BET surface area, 0.89 cm3/g total pore volume, 92.32% carbon content and 1.1 kg/sphere crushing strength with less than 1% of moisture and ash content. The ACS were also evaluated for its potential to remove hexavalent chromium [Cr(VI)] from contaminated solutions. The chromium removal is observed to be 99.1% at initial concentration 50 mg/l, pH 2, ACS dose 1 g/l, contact time 2 h, agitation 120 rpm and temperature 30 °C. Thus ACS can be used as an adsorbent material for the removal of Cr(VI) from contaminated solutions.

Template-mediated, Hierarchical Engineering of Ordered Mesoporous Films and Powders

NASA Astrophysics Data System (ADS)

Tian, Zheng

Hierarchical control over pore size, pore topology, and meso/mictrostructure as well as material morphology (e.g., powders, monoliths, thin films) is crucial for meeting diverse materials needs among applications spanning next generation catalysts, sensors, batteries, sorbents, etc. The overarching goal of this thesis is to establish fundamental mechanistic insight enabling new strategies for realizing such hierarchical textural control for carbon materials that is not currently achievable with sacrificial pore formation by 'one-pot' surfactant-based 'soft'-templating or multi-step inorganic 'hard-templating. While 'hard'-templating is often tacitly discounted based upon its perceived complexity, it offers potential for overcoming key 'soft'-templating challenges, including bolstering pore stability, accommodating a more versatile palette of replica precursors, realizing ordered/spanning porosity in the case of porous thin films, simplifying formation of bi-continuous pore topologies, and inducing microstructure control within porous replica materials. In this thesis, we establish strategies for hard-templating of hierarchically porous and structured carbon powders and tunable thin films by both multi-step hard-templating and a new 'one-pot' template-replica precursor co-assembly process. We first develop a nominal hard-templating technique to successfully prepare three-dimensionally ordered mesoporous (3DOm) and 3DOm-supported microporous carbon thin films by exploiting our ability to synthesize and assemble size-tunable silica nanoparticles into scalable, colloidal crystalline thin film templates of tunable mono- to multi-layer thickness. This robust thin film template accommodates liquid and/or vapor-phase infiltration, polymerization, and pyrolysis of various carbon sources without pore contraction and/or collapse upon template sacrifice. The result is robust, flexible 3DOm or 3DOm-supported ultra-thin microporous films that can be transferred by stamp techniques to various substrates for low-cost counter-electrodes in dye-sensitized solar cells, as we demonstrate, or as potential high-flux membranes for molecular separations. Inspired by 'one-pot' 'soft'-templating approaches, wherein the pore forming agent and replica precursor are co-assembled, we establish how 'hard'-templating can be carried out in an analogous fashion. Namely, we show how pre-formed silica nanoparticles can be co-assembled from aqueous solutions with a carbon source (glucose), leading to elucidation of a pseudo-phase behavior in which we identify an operating window for synthesis of hierarchically bi-continuous carbon films. Systematic study of the association of carbon precursors with the silica particles in combination with transient coating experiments reveals mechanistic insight into how silica-adsorbed carbon precursor modulates particle assembly and ultimately controls template particle d-spacing. We uncover a critical d-spacing defining the boundary between ordered and disordered mesoporosity within the resulting films. We ultimately extend this thin-film mechanistic insight to realize 'one'-pot, bi-continuous 3DOm carbon powders. Through a combination of X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and high-resolution transmission electron microscopy (HR-TEM), we elucidate novel synthesis-structure relations for template-mediated microstructuring of the 3DOm replica carbons. Attractive properties of the resulting bi-continuous porous carbons for applications, for example, as novel electrodes, include high surface areas, large mesopore volumes, and tunable graphitic content (i.e. >50%) and character. We specifically demonstrate their performance, in thin film form, as counter-electrodes in dye-sensitized solar cells. We also demonstrate how they can be exploited in powder form as high-performance supercapacitor electrodes exhibiting attractive retention and absolute capacitance. We conclude the thesis by demonstrating the versatility of both the thin-film and powder templating processes developed herein, for realizing ordered binary colloidal crystal templates and their bi-modal porous carbon replica films, expanding compositional diversity of the 'one-pot' thin film process beyond carbons to include an example of 3DOm ZrO2 films, and employing the hard-templating process as a strategy for realizing 3DOm carbon-supported nanocarbides.

Tunable Graphitic Carbon Nano-Onions Development in Carbon Nanofibers for Multivalent Energy Storage

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

Schwarz, Haiqing L.

2016-01-01

We developed a novel porous graphitic carbon nanofiber material using a synthesis strategy combining electrospinning and catalytic graphitization. RF hydrogel was used as carbon precursors, transition metal ions were successfully introduced into the carbon matrix by binding to the carboxylate groups of a resorcinol derivative. Transition metal particles were homogeneously distributed throughout the carbon matrix, which are used as in-situ catalysts to produce graphitic fullerene-like nanostructures surrounding the metals. The success design of graphitic carbons with enlarged interlayer spacing will enable the multivalent ion intercalation for the development of multivalent rechargeable batteries.

MOF-derived nanohybrids for electrocatalysis and energy storage: current status and perspectives.

PubMed

Zhang, Hong; Liu, Ximeng; Wu, Yue; Guan, Cao; Cheetham, Anthony K; Wang, John

2018-03-27

More than 20 000 MOFs have been reported to date, with different combinations of metal ions/centers and organic linkers, and they can be grown into various 3D, 2D, 1D and 0D morphologies. The flexibility in control over varying length scales from atomic scale up to bulk structure allows access to an almost endless variety of MOF-based and MOF-derived materials. Indeed, MOFs themselves have been studied as a class of useful functional materials. More remarkably, extensive research conducted in recent years has shown that MOFs are exceptionally good precursors for a large variety of nanohybrids as active materials in both electrocatalysis and energy storage. As they already contain both carbon and well-dispersed metal atoms, MOFs can be converted to conductive carbons decorated with active metal species and doping elements through appropriate pyrolysis. Due to the great diversity accessible in the composition, structure, and morphology of MOFs, several types of MOF-derived nanohybrids are now among the best performing materials both for electrocatalysts and electrodes in various energy conversion and storage devices. In addition to mesoporous nano-carbons, both doped and undoped, carbon-metal nanohybrids, and carbon-compound nanohybrids, there are several types of core@shell, encapsulated nanostructures, embedded nanosystems and heterostructures that have been developed from MOFs recently. They can be made in either free-standing forms, nano- or micro-powders, grown on appropriate conducting substrates, or assembled together with other active materials. During the MOF to active material conversion, other active species or precursors can be inserted into the MOF-derived nanostructures or assembled on surfaces, leading to uniquely new porous nanostructures. These MOF-derived active materials for electrocatalysis and energy storage are nanohybrids consisting of more than functional components that are purposely integrated together at desired length scales for much-improved performance. This article reviews the current status of these nanohybrids and concludes with a brief perspective on the future of MOF-derived functional materials.

Poly(ethylene terephthalate)-based carbons as electrode material in supercapacitors

NASA Astrophysics Data System (ADS)

Domingo-García, M.; Fernández, J. A.; Almazán-Almazán, M. C.; López-Garzón, F. J.; Stoeckli, F.; Centeno, T. A.

A systematic study by complementary techniques shows that PET-waste from plastic vessels is a competitive precursor of carbon electrodes for supercapacitors. PET derived-activated carbons follow the general trends observed for highly porous carbons and display specific capacitances at low current density as high as 197 F g -1 in 2 M H 2SO 4 aqueous electrolyte and 98 F g -1 in the aprotic medium 1 M (C 2H 5) 4NBF 4/acetonitrile. Additionally, high performance has also been achieved at high current densities, which confirms the potential of this type of materials for electrical energy storage. A new method based on the basic solvolysis of PET-waste and the subsequent carbonization seems to be an interesting alternative to obtain porous carbons with enhanced properties for supercapacitors.

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

Carbon/ λ-MnO 2 composites for supercapacitor electrodes

NASA Astrophysics Data System (ADS)

Malak-Polaczyk, A.; Matei-Ghimbeu, C.; Vix-Guterl, C.; Frackowiak, E.

2010-04-01

In the present work a composite of carbon with λ-MnO 2 have been synthesized by a simple two-step route. In the first step, to obtain LiMn 2O 4/carbon material, mesoporous activated carbon was impregnated with the solution of precursor metal salts and heated subsequently. As-prepared materials were acid treated which resulted in the formation of λ-MnO 2/carbon. Physical properties, structure and specific surface area of electrode materials were studied by TEM, X-ray diffraction and nitrogen sorption measurements. Voltammetry cycling, galvanostatic charge/discharge and impedance spectroscopy measurements performed in two- and three-electrode cells have been applied in order to measure electrochemical parameters. TEM images confirmed well dispersed λ-MnO 2 particles on the surface of carbon material. The carbon in the composite plays an important role as the surface area enhancing component and a support of pseudocapacitive material. Furthermore, the through-connected porosity serves as a continuous pathway for electrolyte transport. A synergetic effect of the porous carbon framework and of the redox properties of the λ-MnO 2 is at the origin of improvement of specific capacitance values which has been observed for composites after delithiation.

Synthesis of nitrogen- and sulfur-codoped 3D cubic-ordered mesoporous carbon with superior performance in supercapacitors.

PubMed

Zhang, Deyi; Zheng, Liweng; Ma, Ying; Lei, Longyan; Li, Qinglin; Li, Yan; Luo, Heming; Feng, Huixia; Hao, Yuan

2014-02-26

In this contribution, nitrogen- and sulfur-codoped 3D cubic-ordered mesoporous carbon (KNOMC) materials with controlled dopant content (10.0-4.6 atom % for nitrogen and 0.94-0.75 atom % for sulfur) are presented, using KIT-6 as the template and pyrrole as the precursor, and its supercapacitive behavior is also investigated. The presented materials exhibit excellent supercapacitive performance by combining electrical double-layer capacitance and pseudocapacitance as well as the enhanced wettability and improved conductivity generated from the incorporation of nitrogen and sulfur into the framework of carbon materials. The specific capacitance of the presented materials reaches 320 F g(-1) at a current density of 1 A g(-1), which is significantly larger than that of the pristine-ordered mesoporous carbon reported in the literature and can even compete with some metal oxides and conducting polymers.

Process Parameters for Successful Synthesis of Carbon Nanotubes by Chemical Vapor Deposition: Implications for Chemical Mechanisms and Life-cycle Assessment

NASA Astrophysics Data System (ADS)

Xue, Ke

Manufacturing of carbon nanotubes (CNTs) via chemical vapor deposition (CVD) calls for thermal treatment associated with gas-phase rearrangement and catalyst deposition to achieve high cost efficiency and limited influence on environmental impact. Taking advantage of higher degree of structure control and economical efficiency, catalytic chemical vapor deposition (CCVD) has currently become the most prevailing synthesis approach for the synthesis of large-scale pure CNTs in past years. Because the synthesis process of CNTs dominates the potential ecotoxic impacts, materials consumption, energy consumption and greenhouse gas emissions should be further limited to efficiently reduce life cycle ecotoxicity of carbon naotubes. However, efforts to reduce energy and material requirements in synthesis of CNTs by CCVD are hindered by a lack of mechanistic understanding. In this thesis, the effect of operating parameters, especially the temperature, carbon source concentration, and residence time on the synthesis were studied to improve the production efficiency in a different angle. Thus, implications on the choice of operating parameters could be provided to help the synthesis of carbon nanotubes. Here, we investigated the typical operating parameters in conditions that have yielded successful CNT production in the published academic literature of over seventy articles. The data were filtered by quality of the resultant product and deemed either "successful" or "unsuccessful" according to the authors. Furthermore, growth rate data were tabulated and used as performance metric for the process whenever possible. The data provided us an opportunity to prompt possible and common methods for practioners in the synthesis of CNTs and motivate routes to achieve energy and material minimization. The statistical analysis revealed that methane and ethylene often rely on thermal conversion process to form direct carbon precursor; further, methane and ethylene could not be the direct CNT precursors by themselves. Acetylene does not show an additional energy demand or thermal conversion in the synthesis, and it could be the direct CNT precursors by itself; or at least, it would be most easily to get access to carbon nanotube growth while minimizing synthesis temperature. In detail, methane employs more energy demand (Tavg=883°C) than ethylene (Tavg=766°C), which in turn demands more energy than acetylene (Tavg=710°C) to successfully synthesize carbon nanotubes. The distinction in energy demand could be the result of kinetic energy requirements by the thermal conversion process of methane and ethylene to form direct CNT precursors, and methane employs the highest activation demand among three hydrocarbons. Thus, these results support the hypothesis that methane and ethylene could be thermally converted to form acetylene before CNT incorporation. In addition, methane and ethylene show the demand for hydrogen in thermal conversion process before CNT incorporation; whereas, hydrogen does not contribute to the synthesis via acetylene before CNT incorporation, except the reduction of catalyst. At relatively low hydrogen concentration, this work suggests that hydrogen prompts growth of carbon nanotubes via methane and ethylene, probably by reducing the catalysts or participating thermal reactions. In addition, "polymerization-like formation mechanism" could be supported by the higher growth rate of CNTs via ethylene than acetylene. There could be an optimum residence time to maintain a relatively higher growth rate. At too low residence time, carbon source could not be accumulated, causing a waste of material; while too high residence time may cause the limitation of carbon source supplement and accumulation of byproducts. At last, high concentration of carbon source and hydrogen could cause more energy consumption, while it helps to achieve a high growth rate, due to the more presence of direct carbon precursor.

Microwave hydrothermal transformation of amorphous calcium carbonate nanospheres and application in protein adsorption.

PubMed

Qi, Chao; Zhu, Ying-Jie; Chen, Feng

2014-03-26

Calcium carbonate and calcium phosphate are the main components of biominerals. Among all of the forms of biominerals, amorphous calcium carbonate (ACC) and amorphous calcium phosphate (ACP) are the most important forms because they play a pivotal role in the process of biomineralization and are the precursors to the crystalline polymorphs. In this work, we first synthesized ACC in vitro using adenosine 5'-triphosphate disodium salt (ATP) as the stabilizer and investigated the transformation of the ACC under microwave hydrothermal conditions, and ACC/ACP composite nanospheres and carbonated hydroxyapatite (CHA) nanospheres were successfully prepared. In this novel strategy, ATP has two main functions: it serves as the stabilizer for ACC and the phosphorus source for ACP and CHA. Most importantly, the morphology and the size of the ACC precursor can be well-preserved after microwave heating, so it provides a new method for the preparation of calcium phosphate nanostructured materials using phosphorus-containing biomolecule-stabilized ACC as the precursor. Furthermore, the as-prepared ACC/ACP composite nanospheres have excellent biocompatibility and high protein adsorption capacity, indicating that they are promising for applications in biomedical fields such as drug delivery and protein adsorption.

Chemically synthesized boron carbon oxynitride as a new cold cathode material

NASA Astrophysics Data System (ADS)

Banerjee, Diptonil; Maity, Supratim; Chattopadhyay, K. K.

2015-11-01

Synthesis of boron carbon oxynitride (BCNO) nanosheets at different temperature from amorphous to crystalline regime has been reported. The synthesis was done by a simple molten salt process using sodium borohydride and urea as precursors. Transmission electron microscopic study confirms the formation of sheet-like structure of the as-synthesized material. The performances of the as-synthesized BCNO nanosheets as cold cathode materials have been studied for the first time in the high vacuum electron field emission set up. It has been seen that the material gives considerable field emission current with turn on field as low as 2.95 V/μm with good stability and thus a new cold cathode material can be postulated.

Iron encapsulated in 3D N-doped carbon nanotube/porous carbon hybrid from waste biomass for enhanced oxidative activity.

PubMed

Yao, Yunjin; Zhang, Jie; Wu, Guodong; Wang, Shaobin; Hu, Yi; Su, Cong; Xu, Tongwen

2017-03-01

Novel iron encapsulated in nitrogen-doped carbon nanotubes (CNTs) supported on porous carbon (Fe@N-C) 3D structured materials for degrading organic pollutants were fabricated from a renewable, low-cost biomass, melamine, and iron salt as the precursors. SEM and TEM micrographs show that iron encapsulated bamboo shaped CNTs are vertically standing on carbon sheets, and thus, a 3D hybrid was formed. The catalytic activities of the prepared samples were thoroughly evaluated by activation of peroxymonosulfate for catalytic oxidation of Orange II solutions. The influences of some reaction conditions (pH, temperature, and concentrations of reactants, peroxymonosulfate, and dye) were extensively evaluated. It was revealed that the adsorption could enrich the pollutant which was then rapidly degraded by the catalytically generated radicals, accelerating the continuous adsorption of residual pollutant. Remarkable carbon structure, introduction of CNTs, and N/Fe doping result in promoted adsorption capability and catalytic performances. Due to the simple synthetic process and cheap carbon precursor, Fe@N-C 3D hybrid can be easily scaled up and promote the development of Fenton-like catalysts.

Biochar as potential sustainable precursors for activated carbon production: Multiple applications in environmental protection and energy storage.

PubMed

Tan, Xiao-Fei; Liu, Shao-Bo; Liu, Yun-Guo; Gu, Yan-Ling; Zeng, Guang-Ming; Hu, Xin-Jiang; Wang, Xin; Liu, Shao-Heng; Jiang, Lu-Hua

2017-03-01

There is a growing interest of the scientific community on production of activated carbon using biochar as potential sustainable precursors pyrolyzed from biomass wastes. Physical activation and chemical activation are the main methods applied in the activation process. These methods could have significantly beneficial effects on biochar chemical/physical properties, which make it suitable for multiple applications including water pollution treatment, CO 2 capture, and energy storage. The feedstock with different compositions, pyrolysis conditions and activation parameters of biochar have significant influences on the properties of resultant activated carbon. Compared with traditional activated carbon, activated biochar appears to be a new potential cost-effective and environmentally-friendly carbon materials with great application prospect in many fields. This review not only summarizes information from the current analysis of activated biochar and their multiple applications for further optimization and understanding, but also offers new directions for development of activated biochar. Copyright © 2016 Elsevier Ltd. All rights reserved.

Lignin Based Carbon Materials for Energy Storage Applications

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

Chatterjee, Sabornie; Saito, Tomonori; Rios, Orlando

The implementation of Li-ion battery technology into electric and hybrid electric vehicles and portable electronic devices such as smart phones, laptops and tablets, creates a demand for efficient, economic and sustainable materials for energy storage. However, the high cost and long processing time associated with manufacturing battery-grade anode and cathode materials are two big constraints for lowering the total cost of batteries and environmentally friendly electric vehicles. Lignin, a byproduct of the pulp and paper industry and biorefinery, is one of the most abundant and inexpensive natural biopolymers. It can be efficiently converted to low cost carbon fibers with optimalmore » properties for use as anode materials. Recent developments in the preparation of lignin precursors and conversion to carbon fiber-based anode materials have created a new class of anode materials with excellent electrochemical characteristics suitable for immediate use in existing Li- or Na-ion battery technologies.« less

Formation of Copper Catalysts for CO 2 Reduction with High Ethylene/Methane Product Ratio Investigated with In Situ X-ray Absorption Spectroscopy

DOE PAGES

Eilert, André; Roberts, F. Sloan; Friebel, Daniel; ...

2016-04-04

Nanostructured copper cathodes are among the most efficient and selective catalysts to date for making multicarbon products from the electrochemical carbon dioxide reduction reaction (CO 2RR). We report an in situ X-ray absorption spectroscopy investigation of the formation of a copper nanocube CO 2RR catalyst with high activity that highly favors ethylene over methane production. The results show that the precursor for the copper nanocube formation is copper(I)-oxide, not copper(I)-chloride as previously assumed. A second route to an electrochemically similar material via a copper(II)–carbonate/hydroxide is also reported. In conclusion, this study highlights the importance of using oxidized copper precursors formore » constructing selective CO 2 reduction catalysts and shows the precursor oxidation state does not affect the electrocatalyst selectivity toward ethylene formation.« less

Ultrasound-assisted synthesis and processing of carbon materials

NASA Astrophysics Data System (ADS)

Fortunato, Maria E.

2011-12-01

Part I: Porous carbons are of interest in many applications because of their high surface areas and other physicochemical properties, and much effort has been directed towards developing new methods for controlling the porosity of carbons. Ultrasonic spray pyrolysis (USP) is an aerosol method suitable for large-scale, continuous synthesis of materials. Ultrasound is used to create aerosol droplets of a precursor solution which serve as micron-sized spherical reactors for materials synthesis. This work presents a precursor system for the template-free USP synthesis of porous carbons using low-cost precursors that do not evolve or require hazardous chemicals: sucrose was used as the carbon source, and sodium carbonate, sodium bicarbonate, or sodium nitrate was added as a decomposition catalyst and porogen. The USP carbons had macroporous interiors and microporous shells with surface areas as high as 800 m2/g and a narrow pore size distribution. It was determined that the interior porosity was a result of the gas evolution from salt decomposition and not from the presence of a salt template. Porous carbon is frequently used as a catalyst support because it provides high surface area and it is chemically and physically stable under many anoxic reaction conditions. Typically, the preparation of supported catalysts requires multiple steps for carbonization and metal impregnation. In this work, iron-impregnated porous carbon microspheres (Fe-C) were prepared by a one-step USP process by incorporating both the carbon and metal sources into the precursor solution. Carbonization, pore formation, metal impregnation, and metal activation occurred simultaneously to produce Fe-C materials with surface areas as high as 800 m2/g and up to 10 wt% Fe incorporated as nanoparticles < 20 nm in diameter. Fe-C was used as a catalyst to reduce aqueous hexavalent chromium, which demonstrated the accessibility of the iron nanoparticles despite the fact that they are likely encapsulated in the porous carbon support. Part II: The effects of high intensity ultrasound arise from acoustic cavitation: the formation, growth, and collapse of bubbles in a liquid. Bubble collapse produces intense localized heating (˜5000 K), high pressures (˜300 atm), and enormous heating and cooling rates (>109 K/sec). In solid-liquid slurries, surface erosion and particle fracture occur due to the shockwaves and microjets formed from asymmetric bubble collapse at extended surfaces. The chemical and physical effects of ultrasound have been studied as an adjunct to the traditional chemical pretreatment of lignocellulosic biomass for ethanol production. Lignocellulosic biomass consists of cellulose, hemicellulose, and lignin. The surface effects of ultrasound were used in this work to increase the accessibility of the cellulose, which can be converted to glucose and then fermented into ethanol. The lignocellulosic biomass used in this work was Miscanthus x giganteus (Mxg) which was grown at the University of Illinois at Urbana-Champaign. The chemical effects of NaOH pretreatment on Mxg were enhanced by ultrasound: greater delignification and a significant increase in the amount of pores >5 nm were observed. ˜ 70% of the theoretical glucose yield was obtained by enzymatic saccharification of the ultrasound-assisted NaOH-pretreated Mxg; this is comparable to the yields that can be obtained by traditional alkaline pretreatments, but it was achieved in a shorter time and at a lower temperature. Because the apparatus used for laboratory studies is not a likely device for scale-up, the economics of ultrasound with regards to energy balance are not yet resolved.

Controlling porosity in lignin-derived nanoporous carbon for supercapacitor applications

DOE PAGES

Jeon, Ju-Won; Zhang, Libing; Lutkenhaus, Jodie L.; ...

2015-02-01

Low-cost renewable lignin has been used as a precursor to produce porous carbons. However, to date, it has not been easy to obtain high surface area porous carbon without activation processes or templating agents. Here, we demonstrate that low molecular weight lignin yields highly porous carbon (1092 m² g⁻¹) with more graphitization through direct carbonization without additional activation processes or templating agents. We found that molecular weight and oxygen consumption during carbonization are critical factors to obtain high surface area, graphitized porous carbons. This highly porous carbon from low-cost renewable lignin sources is a good candidate for supercapacitor electrode materials.

Controlling porosity in lignin-derived nanoporous carbon for supercapacitor applications

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

Jeon, Ju-Won; Zhang, Libing; Lutkenhaus, Jodie L.

Low-cost renewable lignin has been used as a precursor to produce porous carbons. However, to date, it has not been easy to obtain high surface area porous carbon without activation processes or templating agents. Here, we demonstrate that low molecular weight lignin yields highly porous carbon (1092 m² g⁻¹) with more graphitization through direct carbonization without additional activation processes or templating agents. We found that molecular weight and oxygen consumption during carbonization are critical factors to obtain high surface area, graphitized porous carbons. This highly porous carbon from low-cost renewable lignin sources is a good candidate for supercapacitor electrode materials.

Enhanced cyclic stability of SnS microplates with conformal carbon coating derived from ethanol vapor deposition for sodium-ion batteries

NASA Astrophysics Data System (ADS)

Li, Xiang; Liu, Jiangwen; Ouyang, Liuzhang; Yuan, Bin; Yang, Lichun; Zhu, Min

2018-04-01

Carbon coated SnS microplates (SnS@C MPs) were prepared via a facile chemical vapor deposition method using SnS2 nanoflakes as precursor and ethanol vapor as carbon source. The carbon coating restrains the growth of SnS during the heat treatment. Furthermore, it improves the electronic conductivity as well as accommodates volume variations of SnS during the sodiation and desodiation processes. Therefore, the rate capability and cycle performance of the SnS@C MPs as anode materials for sodium-ion batteries are remarkably enhanced compared with the bare SnS and the SnS2 precursor. At current densities of 0.1, 0.2, 0.5, 1 and 2 A g-1, the optimized SnS@C MPs exhibit stable capacities of 602.9, 532.1, 512.2, 465.9 and 427.2 mAh g-1, respectively. At 1 A g-1, they show a reversible capacity of 528.8 mAh g-1 in the first cycle, and maintain 444.7 mAh g-1 after 50 cycles, with capacity retention of 84.1%. The carbon coating through chemical vapor deposition using ethanol vapor as carbon sources is green, simple and cost-effective, which shows great promise to improve the reversible Na+ storage of electrode materials.

Cobalt- and iron-based nanoparticles hosted in SBA-15 mesoporous silica and activated carbon from biomass: Effect of modification procedure

NASA Astrophysics Data System (ADS)

Tsoncheva, Tanya; Genova, Izabela; Paneva, Daniela; Dimitrov, Momtchil; Tsyntsarski, Boyko; Velinov, Nicolay; Ivanova, Radostina; Issa, Gloria; Kovacheva, Daniela; Budinova, Temenujka; Mitov, Ivan; Petrov, Narzislav

2015-10-01

Ordered mesoporous silica of SBA-15 type and activated carbon, prepared from waste biomass (peach stones), are used as host matrix of nanosized iron and cobalt particles. The effect of preparation procedure on the state of loaded nanoparticles is in the focus of investigation. The obtained materials are characterized by Boehm method, low temperature physisorption of nitrogen, XRD, UV-Vis, FTIR, Mossbauer spectroscopy and temperature programmed reduction with hydrogen. The catalytic behaviour of the samples is tested in methanol decomposition. The dispersion, oxidative state and catalytic behaviour of loaded cobalt and iron nanoparticles are successfully tuned both by the nature of porous support and the metal precursor used during the samples preparation. Facile effect of active phase deposition from aqueous solution of nitrate precursors is assumed for activated carbon support. For the silica based materials the catalytic activity could be significantly improved when cobalt acetylacetonate is used during the modification. The complex effect of pore topology and surface functionality of different supports on the active phase formation is discussed.

Electrochemical Ultracapacitors Using Graphitic Nanostacks

NASA Technical Reports Server (NTRS)

Marotta, Christopher

2012-01-01

Electrochemical ultracapacitors (ECs) have been developed using graphitic nanostacks as the electrode material. The advantages of this technology will be the reduction of device size due to superior power densities and relative powers compared to traditional activated carbon electrodes. External testing showed that these materials display reduced discharge response times compared to state-of-the-art materials. Such applications are advantageous for pulsed power applications such as burst communications (satellites, cell phones), electromechanical actuators, and battery load leveling in electric vehicles. These carbon nanostructures are highly conductive and offer an ordered mesopore network. These attributes will provide more complete electrolyte wetting, and faster release of stored charge compared to activated carbon. Electrochemical capacitor (EC) electrode materials were developed using commercially available nanomaterials and modifying them to exploit their energy storage properties. These materials would be an improvement over current ECs that employ activated carbon as the electrode material. Commercially available graphite nanofibers (GNFs) are used as precursor materials for the synthesis of graphitic nanostacks (GNSs). These materials offer much greater surface area than graphite flakes. Additionally, these materials offer a superior electrical conductivity and a greater average pore size compared to activated carbon electrodes. The state of the art in EC development uses activated carbon (AC) as the electrode material. AC has a high surface area, but its small average pore size inhibits electrolyte ingress/egress. Additionally, AC has a higher resistivity, which generates parasitic heating in high-power applications. This work focuses on fabricating EC from carbon that has a very different structure by increasing the surface area of the GNF by intercalation or exfoliation of the graphitic basal planes. Additionally, various functionalities to the GNS surface will be added that can exhibit pseudocapacitance. This pseudocapacitance exhibits faradaic (charge transfer) properties that can further increase the overall relative and volumetric capacitance of the material. A process is also proposed to use GNF as a precursor material to fabricate GNS that will be used as EC electrodes. This results in much better electrical conductivity than activated carbon. This is advantageous for high-pulsed-power applications to reduce parasitic heating. Larger average pore size allows more complete electrolyte wetting (faster charge transfer kinetics). These properties contribute to a lowered equivalent series resistance (ESR), increased specific power, shorter charging times, and decreased parasitic heating. The high density of basal plane edges provides nucleation sites for activation (addition of hydrophilic functional groups) that facilitate electrolyte wetting, and will contribute to pseudocapacitance.

Combination of carbon nitride and carbon nanotubes: synergistic catalysts for energy conversion.

PubMed

Gong, Yutong; Wang, Jing; Wei, Zhongzhe; Zhang, Pengfei; Li, Haoran; Wang, Yong

2014-08-01

Due to their versatile features and environmental friendliness, functionalized carbon materials show great potential in practical applications, especially in energy conversion. Developing carbon composites with properties that can be modulated by simply changing the ratio of the original materials is an intriguing synthetic strategy. Here, we took cyanamide and multiwalled carbon nanotubes as precursors and introduced a facile method to fabricate a series of graphitic carbon nitride/carbon nanotubes (g-C3 N4 /CNTs) composites. These composites demonstrated different practical applications with different weight ratios of the components, that is, they showed synergistic effects in optoelectronic conversion when g-C3 N4 was the main ingredient and in oxygen reduction reaction (ORR) when CNTs dominated the composites. Our experiments indicated that the high electrical conductivity of carbon nanotubes promoted the transmission of the charges in both cases. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Fracture in Phenolic Impregnated Carbon Ablator

NASA Technical Reports Server (NTRS)

Agrawal, Parul; Chavez-Garcia, Jose; Pham, John

2013-01-01

This paper describes the development of a novel technique to understand the failure mechanisms inside thermal protection materials. The focus of this research is on the class of materials known as phenolic impregnated carbon ablators. It has successfully flown on the Stardust spacecraft and is the thermal protection system material chosen for the Mars Science Laboratory and SpaceX Dragon spacecraft. Although it has good thermal properties, structurally, it is a weak material. To understand failure mechanisms in carbon ablators, fracture tests were performed on FiberForm(Registered TradeMark) (precursor), virgin, and charred ablator materials. Several samples of these materials were tested to investigate failure mechanisms at a microstructural scale. Stress-strain data were obtained simultaneously to estimate the tensile strength and toughness. It was observed that cracks initiated and grew in the FiberForm when a critical stress limit was reached such that the carbon fibers separated from the binder. However, both for virgin and charred carbon ablators, crack initiation and growth occurred in the matrix (phenolic) phase. Both virgin and charred carbon ablators showed greater strength values compared with FiberForm samples, confirming that the presence of the porous matrix helps in absorbing the fracture energy.

Morphology-dependent Electrochemical Enhancements of Porous Carbon as Sensitive Determination Platform for Ascorbic Acid, Dopamine and Uric Acid

NASA Astrophysics Data System (ADS)

Cheng, Qin; Ji, Liudi; Wu, Kangbing; Zhang, Weikang

2016-02-01

Using starch as the carbon precursor and different-sized ZnO naoparticles as the hard template, a series of porous carbon materials for electrochemical sensing were prepared. Experiments of scanning electron microscopy, transmission electron microscopy and Nitrogen adsorption-desorption isotherms reveal that the particle size of ZnO has big impacts on the porous morphology and surface area of the resulting carbon materials. Through ultrasonic dispersion of porous carbon and subsequent solvent evaporation, different sensing interfaces were constructed on the surface of glassy carbon electrode (GCE). The electrochemical behaviors of ascorbic acid (AA), dopamine (DA) and uric acid (UA) were studied. On the surface of porous carbon materials, the accumulation efficiency and electron transfer ability of AA, DA and UA are improved, and consequently their oxidation signals enhance greatly. Moreover, the interface enhancement effects of porous carbon are also controlled by the particle size of hard template. The constructed porous carbon interface displays strong signal amplification ability and holds great promise in constructing a sensitive platform for the simultaneous determination of AA, DA and UA.

Using ALD To Bond CNTs to Substrates and Matrices

NASA Technical Reports Server (NTRS)

Wong, Eric W.; Bronikowski, Michael J.; Kowalczyk, Robert S.

2008-01-01

Atomic-layer deposition (ALD) has been shown to be effective as a means of coating carbon nanotubes (CNTs) with layers of Al2O3 that form strong bonds between the CNTs and the substrates on which the CNTs are grown. ALD is a previously developed vaporphase thin-film-growth technique. ALD differs from conventional chemical vapor deposition, in which material is deposited continually by thermal decomposition of a precursor gas. In ALD, material is deposited one layer of atoms at a time because the deposition process is self-limiting and driven by chemical reactions between the precursor gas and the surface of the substrate or the previously deposited layer.

Calcination and solid state reaction of ceramic-forming components to provide single-phase superconducting materials having fine particle size

DOEpatents

Balachandran, Uthamalingam; Poeppel, Roger B.; Emerson, James E.; Johnson, Stanley A.

1992-01-01

An improved method for the preparation of single phase, fine grained ceramic materials from precursor powder mixtures where at least one of the components of the mixture is an alkali earth carbonate. The process consists of heating the precursor powders in a partial vacuum under flowing oxygen and under conditions where the partial pressure of CO.sub.2 evolved during the calcination is kept to a very low level relative to the oxygen. The process has been found particularly suitable for the preparation of high temperature copper oxide superconducting materials such as YBa.sub.2 Cu.sub.3 O.sub.x "123" and YBa.sub.2 Cu.sub.4 O.sub.8 "124".

Porous carbon material containing CaO for acidic gas capture: preparation and properties.

PubMed

Przepiórski, Jacek; Czyżewski, Adam; Pietrzak, Robert; Toyoda, Masahiro; Morawski, Antoni W

2013-12-15

A one-step process for the preparation of CaO-containing porous carbons is described. Mixtures of poly(ethylene terephthalate) with natural limestone were pyrolyzed and thus hybrid sorbents could be easily obtained. The polymeric material and the mineral served as a carbon precursor and CaO delivering agent, respectively. We discuss effects of the preparation conditions and the relative amounts of the raw materials used for the preparations on the porosity of the hybrid products. The micropore areas and volumes of the obtained products tended to decrease with increasing CaO contents. Increase in the preparation temperature entailed a decrease in the micropore volume, whereas the mesopore volume increased. The pore creation mechanism is proposed on the basis of thermogravimetric and temperature-programmed desorption measurements. The prepared CaO-containing porous carbons efficiently captured SO2 and CO2 from air. Washing out of CaO from the hybrid materials was confirmed as a suitable method to obtain highly porous carbon materials. Copyright © 2013 Elsevier B.V. All rights reserved.

Carbon-rich supramolecular metallacycles and metallacages

PubMed Central

Northrop, Brian H.; Chercka, Dennis; Stang, Peter J.

2008-01-01

Coordination-driven self-assembly via the directional-bonding approach utilizes rigid transition metal acceptors and electron-rich donors to allow for complex, nanoscale 2D polygons and 3D polyhedra to be prepared under mild conditions and in high yields. To ensure proper rigidity and directionality, many acceptor and donor precursors contain largely carbon-rich aromatic and/or acetylenic moieties. This article introduces self-assembly as an alternative means of synthesizing carbon-rich materials and discusses the development, design, synthesis, and applications of carbon-rich supramolecular metallacycles and metallacages as well as the self-assembly of new diastereomeric carbon-rich supramolecular triangles. PMID:20011029

Carbon quantum dots and a method of making the same

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

Zidan, Ragaiy; Teprovich, Joseph A.; Washington, Aaron L.

The present invention is directed to a method of preparing a carbon quantum dot. The carbon quantum dot can be prepared from a carbon precursor, such as a fullerene, and a complex metal hydride. The present invention also discloses a carbon quantum dot made by reacting a carbon precursor with a complex metal hydride and a polymer containing a carbon quantum dot made by reacting a carbon precursor with a complex metal hydride.

Structure and Electromagnetic Properties of Cellular Glassy Carbon Monoliths with Controlled Cell Size

PubMed Central

Szczurek, Andrzej; Plyushch, Artyom; Macutkevic, Jan

2018-01-01

Electromagnetic shielding is a topic of high importance for which lightweight materials are highly sought. Porous carbon materials can meet this goal, but their structure needs to be controlled as much as possible. In this work, cellular carbon monoliths of well-defined porosity and cell size were prepared by a template method, using sacrificial paraffin spheres as the porogen and resorcinol-formaldehyde (RF) resin as the carbon precursor. Physicochemical studies were carried out for investigating the conversion of RF resin into carbon, and the final cellular monoliths were investigated in terms of elemental composition, total porosity, surface area, micropore volumes, and micro/macropore size distributions. Electrical and electromagnetic (EM) properties were investigated in the static regime and in the Ka-band, respectively. Due to the phenolic nature of the resin, the resultant carbon was glasslike, and the special preparation protocol that was used led to cellular materials whose cell size increased with density. The materials were shown to be relevant for EM shielding, and the relationships between those properties and the density/cell size of those cellular monoliths were elucidated. PMID:29723961

Towards deriving Ni-rich cathode and oxide-based anode materials from hydroxides by sharing a facile co-precipitation method.

PubMed

Qiu, Haifa; Du, Tengfei; Wu, Junfeng; Wang, Yonglong; Liu, Jian; Ye, Shihai; Liu, Sheng

2018-05-22

Although intensive studies have been conducted on layered transition metal oxide(TMO)-based cathode materials and metal oxide-based anode materials for Li-ion batteries, their precursors generally follow different or even complex synthesis routes. To share one route for preparing precursors of the cathode and anode materials, herein, we demonstrate a facile co-precipitation method to fabricate Ni-rich hydroxide precursors of Ni0.8Co0.1Mn0.1(OH)2. Ni-rich layered oxide of LiNi0.8Co0.1Mn0.1O2 is obtained by lithiation of the precursor in air. An NiO-based anode material is prepared by calcining the precursor or multi-walled carbon nanotubes (MWCNTs) incorporated precursors. The pre-addition of ammonia solution can simplify the co-precipitation procedures and the use of an air atmosphere can also make the heat treatment facile. LiNi0.8Co0.1Mn0.1O2 as the cathode material delivers a reversible capacity of 194 mA h g-1 at 40 mA g-1 and a notable cycling retention of 88.8% after 100 cycles at 200 mA g-1. This noticeable performance of the cathode arises from a decent particle morphology and high crystallinity of the layered oxides. As the anode material, the MWCNTs-incorporated oxides deliver a much higher reversible capacity of 811.1 mA h g-1 after 200 cycles compared to the pristine oxides without MWCNTs. The improvement on electrochemical performance can be attributed to synergistic effects from MWCNTs incorporation, including reinforced electronic conductivity, rich meso-pores and an alleviated volume effect. This facile and sharing method may offer an integrated and economical approach for commercial production of Ni-rich electrode materials for Li-ion batteries.

Method of synthesizing small-diameter carbon nanotubes with electron field emission properties

NASA Technical Reports Server (NTRS)

Liu, Jie (Inventor); Du, Chunsheng (Inventor); Qian, Cheng (Inventor); Gao, Bo (Inventor); Qiu, Qi (Inventor); Zhou, Otto Z. (Inventor)

2009-01-01

Carbon nanotube material having an outer diameter less than 10 nm and a number of walls less than ten are disclosed. Also disclosed are an electron field emission device including a substrate, an optionally layer of adhesion-promoting layer, and a layer of electron field emission material. The electron field emission material includes a carbon nanotube having a number of concentric graphene shells per tube of from two to ten, an outer diameter from 2 to 8 nm, and a nanotube length greater than 0.1 microns. One method to fabricate carbon nanotubes includes the steps of (a) producing a catalyst containing Fe and Mo supported on MgO powder, (b) using a mixture of hydrogen and carbon containing gas as precursors, and (c) heating the catalyst to a temperature above 950.degree. C. to produce a carbon nanotube. Another method of fabricating an electron field emission cathode includes the steps of (a) synthesizing electron field emission materials containing carbon nanotubes with a number of concentric graphene shells per tube from two to ten, an outer diameter of from 2 to 8 nm, and a length greater than 0.1 microns, (b) dispersing the electron field emission material in a suitable solvent, (c) depositing the electron field emission materials onto a substrate, and (d) annealing the substrate.

Photodegradation of rhodamine B over biomass-derived activated carbon supported CdS nanomaterials under visible irradiation

NASA Astrophysics Data System (ADS)

Huang, Hai-Bo; Wang, Yu; Cai, Feng-Ying; Jiao, Wen-Bin; Zhang, Ning; Liu, Cheng; Cao, Hai-Lei; Lü, Jian

2017-12-01

A family of new CdS@SAC composite materials was successfully prepared through the deposition of as-synthesized CdS nanomaterials on various lotus-seedpod-derived activated carbon (SAC) materials. The SAC supports derived at different activation temperatures exhibited considerably large surface areas and various microstructures that were responsible for the enhanced photocatalytic performance of CdS@SAC composite materials towards the photodegradation of rhodamine B (RhB) under visible irradiation. The best-performing CdS@SAC-800 showed excellent photocatalytic activity with a rate constant of ca. 2.40×10–2 min–1, which was approximately 13 times higher than that of the CdS precursor. Moreover, the estimated band gap energy of CdS@SAC-800 (1.99 eV) was significantly lower than that of the CdS precursor (2.22 eV), which suggested considerable strength of interface contact between the CdS and carbon support, as well as efficient light harvesting capacity of the composite material. Further photocatalytic study indicated that the SAC supports enhanced synergistically the accessibility of organic substrates, the efficiency of solar energy harvesting, as well as the separation of photogenerated electrons and holes in this system. Improved photocatalytic activity of the composite materials was largely due to the increased generation of active species such as h+, OH•, O2•‑ etc. This work provides a facile and low-cost pathway to fabricate composite photocatalysts for viable degradation of organic pollutants.

Study of silicon carbide formation by liquid silicon infiltration of porous carbon structures

NASA Astrophysics Data System (ADS)

Margiotta, Jesse C.

Silicon carbide (SiC) materials are prime candidates for high temperature heat exchangers for next generation nuclear reactors due to their refractory nature and high thermal conductivity at elevated temperatures. This research has focused on demonstrating the potential of liquid silicon infiltration (LSI) for making SiC to achieve this goal. The major advantage of this method over other ceramic processing techniques is the enhanced capability of making fully dense, high purity SiC materials in complex net shapes. For successful formation of net shape SiC using LSI techniques, the carbon preform reactivity and pore structure must be controlled to allow the complete infiltration of the porous carbon structure followed by conversion of this carbon to SiC. We have established a procedure for achieving desirable carbon properties by using carbon precursors consisting of two readily available high purity organic materials, crystalline cellulose and phenolic resin. Phenolic resin yields a glassy carbon with low reactivity and porosity, and cellulose carbon is highly reactive and porous. By adjusting the ratio of these two materials in the precursor mixtures, the properties of the carbons produced can be controlled. We have identified the most favorable carbon precursor composition to be a cellulose:resin mass ratio of 6:4 for LSI formation of SiC. The optimum reaction conditions are a temperature of 1800°C, a pressure of 0.5 Torr of argon, and a time of 120 minutes. The fully dense net shape SiC material produced has a density of 2.96 g cm-3 (about 92% of pure SiC) and a SiC volume fraction of over 0.82. Kinetics of the LSI SiC formation process were studied by optical microscopy and quantitative digital image analysis. This study identified six reaction stages and provided important understanding of the process. Such knowledge can be used to further refine the LSI technique. Although the thermal conductivity of pure SiC at elevated temperatures is very high, thermal conductivities of most commercial SiC materials are much lower due to phonon scattering by impurities (e.g., sintering aids located at the grain boundaries of these materials). The thermal conductivity of our SiC was determined using the laser flash method and it is 214 W/mK at 373 K and 64 W/mK at 1273 K. These values are very close to those of pure SiC and are much higher than those of SiC materials made by industrial processes. Thus, SiC made by our LSI process is an ideally suited material for use in high temperature heat exchanger applications. Electron probe microanalysis (EPMA) and Auger electron spectroscopy (AES) were used to study the chemical composition of LSI SiC materials. Optimized low voltage microanalysis conditions for EPMA of SiC were theoretically determined. EPMA and AES measurements indicate that the SiC phase in our materials is slightly carbon rich. Carbon contamination was identified as a possible source of error during EPMA of SiC, and this error was corrected by using high purity SiC standards. Cellulose and phenolic resin carbons lack the well-defined atomic structures associated with common carbon allotropes. Atomic-scale structure was studied using high resolution transmission electron microscopy (HRTEM), nitrogen gas adsorption and helium gas pycnometry. These studies revealed that cellulose carbon exhibits a very high degree of atomic disorder and angstrom-scale porosity. It has a density of only 93% of that of pure graphite, with primarily sp2 bonding character and a low concentration of graphene clusters. Phenolic resin carbon shows more structural order and substantially less angstrom-scale porosity. Its density is 98% of that of pure graphite, and Fourier transform analysis of its TEM micrographs has revealed high concentrations of sp3 diamond and sp 2 graphene nano-clusters. This is the first time that diamond nano-clusters have been observed in carbons produced from phenolic resin.

Double Soft-Template Synthesis of Nitrogen/Sulfur-Codoped Hierarchically Porous Carbon Materials Derived from Protic Ionic Liquid for Supercapacitor.

PubMed

Sun, Li; Zhou, Hua; Li, Li; Yao, Ying; Qu, Haonan; Zhang, Chengli; Liu, Shanhu; Zhou, Yanmei

2017-08-09

Heteroatom-doped hierarchical porous carbon materials derived from the potential precursors and prepared by a facile, effective, and low-pollution strategy have recently been particularly concerned in different research fields. In this study, the interconnected nitrogen/sulfur-codoped hierarchically porous carbon materials have been successfully obtained via one-step carbonization of the self-assembly of [Phne][HSO 4 ] (a protic ionic liquid originated from dilute sulfuric acid and phenothiazine by a straightforward acid-base neutralization) and the double soft-template of OP-10 and F-127. During carbonization process, OP-10 as macroporous template and F-127 as mesoporous template were removed, while [Phne][HSO 4 ] not only could be used as carbon, nitrogen, and sulfur source, but also as a pore forming agent to create micropores. The acquired carbon materials for supercapacitor not only hold a large specific capacitance of 302 F g -1 even at 1.0 A g -1 , but also fine rate property with 169 F g -1 at 10 A g -1 and excellent capacitance retention of nearly 100% over 5000 circulations in 6 M KOH electrolyte. Furthermore, carbon materials also present eximious rate performance with 70% in 1 M Na 2 SO 4 electrolyte.

Method for the preparation of carbon fiber from polyolefin fiber precursor, and carbon fibers made thereby

DOEpatents

Naskar, Amit Kumar; Hunt, Marcus Andrew; Saito, Tomonori

2015-08-04

Methods for the preparation of carbon fiber from polyolefin fiber precursor, wherein the polyolefin fiber precursor is partially sulfonated and then carbonized to produce carbon fiber. Methods for producing hollow carbon fibers, wherein the hollow core is circular- or complex-shaped, are also described. Methods for producing carbon fibers possessing a circular- or complex-shaped outer surface, which may be solid or hollow, are also described.

Effect of Precursor Selection on the Photocatalytic Performance of Indium Oxide Nanomaterials for Gas-Phase CO 2 Reduction

DOE PAGES

Hoch, Laura B.; He, Le; Qiao, Qiao; ...

2016-06-01

Nonstoichiometric indium oxide nanoparticles, In 2O 3–x(OH)y, have been shown to function as active photocatalysts for gas-phase CO 2 reduction under simulated solar irradiation. We demonstrate that the choice of starting material has a strong effect on the photocatalytic activity of indium oxide nanoparticles. We also examine three indium oxide materials prepared via the thermal decomposition of either indium(III) hydroxide or indium(III) nitrate and correlate their stability and photocatalytic activity to the number and type of defect present in the material. Furthermore, we use 13CO 2 isotope-tracing experiments to clearly identify the origins of the observed carbon-containing products. Significantly, wemore » find that the oxidizing nature of the precursor anion has a substantial impact on the defect formation within the sample. Our study demonstrates the importance of surface defects in designing an active heterogeneous photocatalyst and provides valuable insight into key parameters for the precursor design, selection, and performance optimization of materials for gas-phase CO 2 reduction.« less

Porous carbon materials synthesized using IRMOF-3 and furfuryl alcohol as precursor

NASA Astrophysics Data System (ADS)

Deka, Pemta Tia; Ediati, Ratna

2016-03-01

IRMOF-3 crystals have been synthesized using solvothermal method by adding zinc nitrate hexahydrate with 2-amino-1,4-benzenedicarboxylic acid in N'N-dimethylformamide (DMF) at 100°C for 24 (note as IR-24) and 72 h (note as IR-72). The obtained crystals were characterized using X-ray Diffraction (XRD), SEM (Scanning Electron Microscopy) and Scanning Electron Microscopy-Energy Dispersive X-ray (SEM-EDX), FTIR and Isothermal adsorption-desorption N2. The diffractogram solids synthesized show characteristic peak at 2θ 6.8, 9.6 and 13.7°. SEM micrograph show cubic shape of IRMOF-3 crystal. Based on FTIR characterization, IRMOF-3 appear at wavelength (1691,46; 1425,3; 1238,21; 1319,22 dan 3504,42)cm-1. The Isotherm of crystal IRMOF-3 at heating time 24 h and 72 h are type IV. The surface area of IR-24 and IR-72 are respectively 24,758 m2/g and 29,139 m2/g with its dominant mesopores. Carbonaceous materials has been successfully synthesized using IR-24, IR-72 and furfuryl alcohol (FA) as second carbon precursor with variation of carbonation temperature 550, 700 and 850°C. The XRD result from both carbonaceous materials show formation of amorphous carbon and caharacteristic peak of ZnO oxide. Micrograph SEM show that carbonaceous materials have cubic shape as IRMOF-3 and SEM-EDX result indicate Zn and nitrogen content of these materials has decrease until temperature 850°C. Porous carbon using IR-24 and FA (notes as C-24) has increased surface area with higher carbonation temperature. The highest surface area is 1495,023 m2/g. Total pore volume and pore size of C-24 from low to high temperature respectively as (0,338; 0,539 and 1,598) cc/g; (0,107; 0,152 and 0,610) cc/g. Porous carbon using IR-72 and FA (notes as C-72) has smaller surface area than C-24 but its also increased during higher carbonation heating. The highest surface area is 1029,668 m2/g.The total pore volume and pore size of these carbon materials from low to high temperature respectively as (0,390; 0,727 and 1,345) cc/g and (0,065; 0,157 and 0,381) cc/g. Carbonaceous materials with high porosity and nitrogen content will be expected increase mechanical properties and hydrogen storage from these materials.

Effects of Carbon Structure and Surface Oxygen on the Carbon's Performance as the Anode in Lithium-Ion Battery Determined

NASA Technical Reports Server (NTRS)

Hung, Ching-Cheh

2000-01-01

Four carbon materials (C1, C2, C3, and C4) were tested electrochemically at the NASA Glenn Research Center at Lewis Field to determine their performance in lithium-ion batteries. They were formed as shown in the figure. This process caused very little carbon loss. Products C1 and C3 contained very little oxygen because of the final overnight heating at 540 C. Products C2 and C4, on the other hand, contained small amounts of basic oxide. The electrochemical test involved cycles of lithium intercalation and deintercalation using C/saturated LiI-50/50 (vol %) ethylene carbonate (EC) and dimethyl carbonate (DMC)/Li half cell. The cycling test, which is summarized in the table, resulted in three major conclusions. The capacity of the carbon with a basic oxide surface converges to a constant 1. value quickly (within 4 cycles), possibly because the oxide prevents solvent from entering the carbon structure and, therefore, prolongs the carbon s cycle life. Under certain conditions, the disordered carbon can store more lithium than its 2. precursor. These samples and their precursor can intercalate at 200 mA/g and deintercalate at 3. a rate of 2000 mA/g without significant capacity loss.

Pyrolytic carbon membranes containing silica: morphological approach on gas transport behavior

NASA Astrophysics Data System (ADS)

Park, Ho Bum; Lee, Sun Yong; Lee, Young Moo

2005-04-01

Pyrolytic carbon membrane containing silica (C-SiO 2) is a new-class material for gas separation, and in the present work we will deal with it in view of the morphological changes arising from the difference in the molecular structure of the polymeric precursors. The silica embedded carbon membranes were fabricated by a predetermined pyrolysis step using imide-siloxane copolymers (PISs) that was synthesized from benzophenone tetracarboxylic dianhydrides (BTDA), 4,4'-oxydianiline (ODA), and amine-terminated polydimethylsiloxane (PDMS). To induce different morphologies at the same chemical composition, the copolymers were prepared using one-step (preferentially a random segmented copolymer) sand two-step polymerization (a block segmented copolymer) methods. The polymeric precursors and their pyrolytic C-SiO 2 membranes were analyzed using thermal analysis, atomic force microscopy, and transmission electron microscopy, etc. It was found that the C-SiO 2 membrane derived from the random PIS copolymer showed a micro-structure containing small well-dispersed silica domains, whereas the C-SiO 2 membrane from the block PIS copolymer exhibited a micro-structure containing large silica domains in the continuous carbon matrix. Eventually, the gas transport through these C-SiO 2 membranes was significantly affected by the morphological changes of the polymeric precursors.

Method for the preparation of carbon fiber from polyolefin fiber precursor

DOEpatents

Naskar, Amit Kumar; Hunt, Marcus Andrew; Saito, Tomonori

2017-11-28

Methods for the preparation of carbon fiber from polyolefin fiber precursor, wherein the polyolefin fiber precursor is partially sulfonated and then carbonized to produce carbon fiber. Methods for producing hollow carbon fibers, wherein the hollow core is circular- or complex-shaped, are also described. Methods for producing carbon fibers possessing a circular- or complex-shaped outer surface, which may be solid or hollow, are also described.

Carbon nanotubes on nanoporous alumina: from surface mats to conformal pore filling

PubMed Central

2014-01-01

Control over nucleation and growth of multi-walled carbon nanotubes in the nanochannels of porous alumina membranes by several combinations of posttreatments, namely exposing the membrane top surface to atmospheric plasma jet and application of standard S1813 photoresist as an additional carbon precursor, is demonstrated. The nanotubes grown after plasma treatment nucleated inside the channels and did not form fibrous mats on the surface. Thus, the nanotube growth mode can be controlled by surface treatment and application of additional precursor, and complex nanotube-based structures can be produced for various applications. A plausible mechanism of nanotube nucleation and growth in the channels is proposed, based on the estimated depth of ion flux penetration into the channels. PACS 63.22.Np Layered systems; 68. Surfaces and interfaces; Thin films and nanosystems (structure and non-electronic properties); 81.07.-b Nanoscale materials and structures: fabrication and characterization PMID:25177216

Conversion of Langmuir-Blodgett monolayers and bilayers of poly(amic acid) through polyimide to graphene

NASA Astrophysics Data System (ADS)

Jo, Hye Jin; Lyu, Ji Hong; Ruoff, Rodney S.; Lim, Hyunseob; In Yoon, Seong; Jeong, Hu Young; Shin, Tae Joo; Bielawski, Christopher W.; Shin, Hyeon Suk

2017-03-01

Various solid carbon sources, particularly poly(methyl methacrylate), have been used as precursors to graphene. The corresponding growth process generally involves the decomposition of the solids to hydrocarbon gases followed by their adsorption on metallic substrates (e.g., Cu). We report a different approach that uses a thermally-resistant polyimide (PI) as a carbon precursor. Langmuir-Blodgett films of poly(amic acid) (PAA) were transferred to copper foils and then converted to graphene via a PI intermediate. The Cu foil substrate was also discovered to facilitate the orientation of aromatic moieties upon carbonization process of the PI. As approximately 50% of the initial quantity of the PAA was found to remain at 1000 °C, thermally-stable polymers may reduce the quantity of starting material required to prepare high quality films of graphene. Graphene grown using this method featured a relatively large domain size and an absence of adventitious adlayers.

Formation of brown carbon via reactions of ammonia with secondary organic aerosols from biogenic and anthropogenic precursors

NASA Astrophysics Data System (ADS)

Updyke, Katelyn M.; Nguyen, Tran B.; Nizkorodov, Sergey A.

2012-12-01

Filter samples of secondary organic aerosols (SOA) generated from the ozone (O3)- and hydroxyl radical (OH)-initiated oxidation of various biogenic (isoprene, α-pinene, limonene, α-cedrene, α-humulene, farnesene, pine leaf essential oils, cedar leaf essential oils) and anthropogenic (tetradecane, 1,3,5-trimethylbenzene, naphthalene) precursors were exposed to humid air containing approximately 100 ppb of gaseous ammonia (NH3). Reactions of SOA compounds with NH3 resulted in production of light-absorbing "brown carbon" compounds, with the extent of browning ranging from no observable change (isoprene SOA) to visible change in color (limonene SOA). The aqueous phase reactions with dissolved ammonium (NH4+) salts, such as ammonium sulfate, were equally efficient in producing brown carbon. Wavelength-dependent mass absorption coefficients (MAC) of the aged SOA were quantified by extracting known amounts of SOA material in methanol and recording its UV/Vis absorption spectra. For a given precursor, the OH-generated SOA had systematically lower MAC compared to the O3-generated SOA. The highest MAC values, for brown carbon from SOA resulting from O3 oxidation of limonene and sesquiterpenes, were comparable to MAC values for biomass burning particles but considerably smaller than MAC values for black carbon aerosols. The NH3/NH4+ + SOA brown carbon aerosol may contribute to aerosol optical density in regions with elevated concentrations of NH3 or ammonium sulfate and high photochemical activity.

Biomass-derived nitrogen-doped porous carbons with tailored hierarchical porosity and high specific surface area for high energy and power density supercapacitors

NASA Astrophysics Data System (ADS)

Sun, Junting; Niu, Jin; Liu, Mengyue; Ji, Jing; Dou, Meiling; Wang, Feng

2018-01-01

Porous carbon materials with hierarchical structures attract intense interest for the development of high-performance supercapacitors. Herein, we demonstrate a facile and efficient strategy to synthesize nitrogen-doped hierarchically porous carbons with tailored porous structure combined with high specific surface area (SSA), which involves a pre-carbonization and a subsequent carbonization combined with KOH activation of silkworm cocoon precursors. Through adjusting the mass ratio of the activator (KOH) to pre-carbonized precursor in the activation process, the hierarchically porous carbon prepared at the mass ratio of 2 (referred to as NHPC-2) possesses a high defect density and a high SSA of 3386 m2 g-1 as well as the relatively high volumetric proportion of mesopores and macropores (45.5%). As a result, the energy density and power density of the symmetric supercapacitor based on NHPC-2 electrode are as high as 34.41 Wh kg-1 and 31.25 kW kg-1 in organic-solvent electrolyte, and are further improved to 112.1 Wh kg-1 and 23.91 kW kg-1 in ionic-liquid electrolyte.

Facilely Fabricating Multifunctional N-Enriched Carbon.

PubMed

Wan, Mi Mi; Sun, Xiao Dan; Li, Yan Yan; Zhou, Jun; Wang, Ying; Zhu, Jian Hua

2016-01-20

A new synthetic strategy, named "carbonization in limited space" and based on the specific interaction between eutectic salt and dual-ionic liquids (dual-ILs), is reported in this article. N-Containing dual-ILs (1,4-diethyl-1,4-diazaniabicyclo[2,2,2]octane imidazolide-4,5-dicyanoiazolide, [2C2DABCO](2+)[Im](-)[CN-Im](-)) were synthesized as new carbon-nitrogen precursors, while eutectic salt was chosen as a reuseable template in order to facilely fabricate the N-doped porous carbon with sheetlike morphology. Nitrogen can be directly and efficiently incorporated into the porous carbon, resulting in the materials with suitable N content, tunable pore structure, and controllable thickness of sheet as well as high surface area. They exhibited good performance as electrodes for supercapacitors, photocatalysts in degradation of methyl orange (MO) under visible light, and the sorbent to capture tobacco-specific N-nitrosamines (TSNAs) in solution, offering a new simplified but effective method to prepare versatile carbon material.

Oxygen-rich hierarchical porous carbon derived from artemia cyst shells with superior electrochemical performance.

PubMed

Zhao, Yufeng; Ran, Wei; He, Jing; Song, Yanfang; Zhang, Chunming; Xiong, Ding-Bang; Gao, Faming; Wu, Jinsong; Xia, Yongyao

2015-01-21

In this study, three-dimensional (3D) hierarchical porous carbon with abundant functional groups is produced through a very simple low-cost carbonization of Artemia cyst shells. The unique hierarchical porous structure of this material, combining large numbers of micropores and macropores, as well as reasonable amount of mesopores, is proven favorable to capacitive behavior. The abundant oxygen functional groups from the natural carbon precursor contribute stable pseudocapacitance. As-prepared sample exhibits high specific capacitance (369 F g(-1) in 1 M H2SO4 and 349 F g(-1) in 6 M KOH), excellent cycling stability with capacitance retention of 100% over 10 000 cycles, and promising rate performance. This work not only describes a simple way to produce high-performance carbon electrode materials for practical application, but also inspires an idea for future structure design of porous carbon.

Large-deformation and high-strength amorphous porous carbon nanospheres

NASA Astrophysics Data System (ADS)

Yang, Weizhu; Mao, Shimin; Yang, Jia; Shang, Tao; Song, Hongguang; Mabon, James; Swiech, Wacek; Vance, John R.; Yue, Zhufeng; Dillon, Shen J.; Xu, Hangxun; Xu, Baoxing

2016-04-01

Carbon is one of the most important materials extensively used in industry and our daily life. Crystalline carbon materials such as carbon nanotubes and graphene possess ultrahigh strength and toughness. In contrast, amorphous carbon is known to be very brittle and can sustain little compressive deformation. Inspired by biological shells and honeycomb-like cellular structures in nature, we introduce a class of hybrid structural designs and demonstrate that amorphous porous carbon nanospheres with a thin outer shell can simultaneously achieve high strength and sustain large deformation. The amorphous carbon nanospheres were synthesized via a low-cost, scalable and structure-controllable ultrasonic spray pyrolysis approach using energetic carbon precursors. In situ compression experiments on individual nanospheres show that the amorphous carbon nanospheres with an optimized structure can sustain beyond 50% compressive strain. Both experiments and finite element analyses reveal that the buckling deformation of the outer spherical shell dominates the improvement of strength while the collapse of inner nanoscale pores driven by twisting, rotation, buckling and bending of pore walls contributes to the large deformation.

Trihalomethanes formed from natural organic matter isolates: Using isotopic and compositional data to help understand sources

USGS Publications Warehouse

Bergamaschi, Brian A.; Fram, Miranda S.; Fujii, Roger; Aiken, George R.; Kendall, Carol; Silva, Steven R.

2000-01-01

Over 20 million people drink water from the Sacramento-San Joaquin Delta despite problematic levels of natural organic matter (NOM) and bromide in Delta water, which can form trihalomethanes (THMs) during the treatment process. It is widely believed that NOM released from Delta peat islands is a substantial contributor to the pool of THM precursors present in Delta waters. Dissolved NOM was isolated from samples collected at five channel sites within the Sacramento-San Joaquin Rivers and Delta, California, USA, and from a peat island agricultural drain. To help understand the sources of THM precursors, samples were analyzed to determine their chemical and isotopic composition, their propensity to form THMs, and the isotopic composition of the THMs.The chemical composition of the isolates was quite variable, as indicated by significant differences in carbon-13 nuclear magnetic resonance spectra and carbon-to-nitrogen concentration ratios. The lowest propensity to form THMs per unit of dissolved organic carbon was observed in the peat island agricultural drain isolate, even though it possessed the highest fraction of aromatic material and the highest specific ultraviolet absorbance. Changes in the chemical and isotopic composition of the isolates and the isotopic composition of the THMs suggest that the source of the THMs precursors was different between samples and between isolates. The pattern of variability in compositional and isotopic data for these samples was not consistent with simple mixing of river- and peat-derived organic material.

Molding mineral within microporous hydrogels by a polymer-induced liquid-precursor (PILP) process.

PubMed

Cheng, Xingguo; Gower, Laurie B

2006-01-01

Natural biominerals often have exquisite morphologies, where the cells exercise a high degree of crystallographic control through secretion of biological macromolecules and regulation of ion transport. One important example is the sea urchin spine. It has recently been shown to be formed through deposition of a transient amorphous calcium carbonate (ACC) precursor phase that later transforms to single-crystalline calcite, ultimately forming an elaborate three-dimensional microporous calcium carbonate structure with interconnected pores. Macromolecules associated with the mineral phase are thought to play a key role in regulating this transformation. The work described here mimics this type of morphological control by "molding" an amorphous calcium carbonate precursor within a porous poly(2-hydroxyethyl methacrylate) (PHEMA) hydrogel that has been prepared as a negative replica from the void space of an urchin spine. Using an acidic biomimetic polymer as a process-directing agent, we show that polyaspartic acid induces amorphous calcium carbonate (ACC) nanoparticles, which have fluidic character and therefore are able to infiltrate the PHEMA hydrogel replica and coalesce into the convoluted morphology that replicates the original microporous structure of the sea urchin spine. By "molding" calcium carbonate into a complex morphology at room temperature, using a precursor process that is induced by a biomimetic acidic macromolecule, the PILP process is a useful in vitro model for examining different aspects of the amorphous-to-crystalline transformation process that is apparently used by a variety of biomineralizing organisms. For example, although we were able to replicate the overall morphology of the spine, it had polycrystalline texture; further studies with this system will focus on controlling the nucleation event, which may help to elucidate how such a convoluted structure can be prepared with single-crystalline texture via an amorphous precursor. Through a better understanding of the mechanisms used by organisms to regulate crystal properties, such biomimetic processes can lead to the synthesis of materials with superior electronic, mechanical, and optical properties.

Damage Precursor Investigation of Fiber-Reinforced Composite Materials Under Fatigue Loads

DTIC Science & Technology

2013-09-01

19.21, 215713. Thostenson, E. T.; Chou, T.‐W. Carbon Nanotube Networks: Sensing of Distributed Strain and Damage for Life Prediction and Self Healing ...composite structural life and the goal of the proposed research program to develop self -responsive engineered composites. Over 80%‒90% of the life of a...composite material. It is also envisaged to investigate and develop self -responsive engineered composite materials that provide an accurate health

Expanding pore sizes of ZIF-8-derived nitrogen-doped microporous carbon via C60 embedding: toward improved anode performance for the lithium-ion battery.

PubMed

Guan, Jian; Zhong, Xiongwu; Chen, Xiang; Zhu, Xianjun; Li, Panlong; Wu, Jianhua; Lu, Yalin; Yu, Yan; Yang, Shangfeng

2018-02-01

Porous carbon and nanocarbons have been extensively applied as anode materials for high-energy density lithium-ion batteries (LIBs). However, as another representative nanocarbon, fullerenes, such as C 60 , have been scarcely utilized in LIBs because of their poor electrochemical reversibility. Herein, we designed a novel C 60 -embedded nitrogen-doped microporous carbon material (denoted as C 60 @N-MPC), which was derived from a zeolitic imidazolate framework-8 (ZIF-8) precursor, demonstrating its promising application as a superior anode material for LIB. We first embedded C 60 in situ into a ZIF-8 matrix via a facile solid-state mechanochemical route, which acted as a precursor and was transformed to C 60 @N-MPC after carbonization. The C 60 @N-MPC was applied as a novel anode for LIBs, showing an improved reversible specific capacity of ≈1351 mA h g -1 at 0.1 A g -1 and a better rate capacity (≈1077 mA h g -1 at 1 A g -1 after 400 cycles) relative to those based on the unmodified N-MPC anode. The role of C 60 in the superior lithium storage performance of C 60 @N-MPC was elucidated, revealing that C 60 functioned as a pore expander for N-MPC with 3-20 nm mesopores (versus sub-1 nm micropores for the unmodified N-MPC), which facilitated the rapid diffusion of the organic electrolyte.

Ionic Liquid Directed Mesoporous Carbon Nanoflakes as an Effiencient Electrode material

NASA Astrophysics Data System (ADS)

Kong, Lirong; Chen, Wei

2015-12-01

Supercapacitors are considered to be the most promising approach to meet the pressing requirements for energy storage devices. The electrode materials for supercapacitors have close relationship with their electrochemical properties and thus become the key point to improve their energy storage efficiency. Herein, by using poly (vinylidene fluoride-co-hexafluoropropylene) and ionic liquid as the dual templates, polyacrylonitrile as the carbon precursor, a flake-like carbon material was prepared by a direct carbonization method. In this method, poly (vinylidene fluoride-co-hexafluoropropylene) worked as the separator for the formation of isolated carbon flakes while aggregated ionic liquid worked as the pore template. The obtained carbon flakes exhibited a specific capacitance of 170 F/g at 0.1 A/g, a high energy density of 12.2 Wh/kg and a high power density of 5 kW/kg at the current of 10 A/g. It also maintained a high capacitance retention capability with almost no declination after 500 charge-discharge cycles. The ionic liquid directed method developed here also provided a new idea for the preparation of hierarchically porous carbon nanomaterials.

Low temperature stabilization process for production of carbon fiber having structural order

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

Rios, Orlando; McGuire, Michael Alan; More, Karren Leslie

A method for producing a carbon fiber, the method comprising: (i) subjecting a continuous carbon fiber precursor having a polymeric matrix in which strength-enhancing particles are incorporated to a stabilization process during which the carbon fiber precursor is heated to within a temperature range ranging from the glass transition temperature to no less than 20.degree. C. below the glass transition temperature of the polymeric matrix, wherein the maximum temperature employed in the stabilization process is below 400.degree. C., for a processing time within said temperature range of at least 1 hour in the presence of oxygen and in the presencemore » of a magnetic field of at least 1 Tesla, while said carbon fiber precursor is held under an applied axial tension; and (ii) subjecting the stabilized carbon fiber precursor, following step (i), to a carbonization process. The stabilized carbon fiber precursor, resulting carbon fiber, and articles made thereof are also described.« less

Preparation and characterisation of CNF/MWCNT carbon aerogel as efficient adsorbents.

PubMed

Xu, Zhaoyang; Jiang, Xiangdong; Tan, Sicong; Wu, Weibing; Shi, Jiangtao; Zhou, Huan; Chen, Peng

2018-06-01

In recent years, carbon aerogels have attracted much attention in basic research and as potential applications in many fields. Herein, the authors report a novel approach using bamboo powder as raw material to fabricate cellulose nanofibers (CNFs)/multi-walled carbon nanotubes (MWCNTs) carbon aerogels by a simple dipping and carbonisation process. The developed material exhibits many exciting properties including low density (0.056 g cm -3 ), high porosity (95%), efficient capability for separation of oily droplets from water, and high adsorption capacity for a variety of oils and organic solvents by up to 110 times its own weight. Furthermore, the CNF/MWCNT carbon aerogels (CMCA) can be recycled many times by distillation and combustion, satisfying the requirements of practical oil-water separation. Taken together with its economical, environmentally benign manufacturing process, sustainability of the precursor and versatility of material, the CMCA developed in this study will be a promising candidate for addressing the problems arising from the spills of oily compounds.

Reactive Melt Infiltration of Silicon-Niobium Alloys in Microporous Carbons

NASA Technical Reports Server (NTRS)

Singh, M.; Behrendt, D. R.

1994-01-01

Studies of the reactive melt infiltration of silicon-niobium alloys in microporous carbon preforms prepared by the pyrolysis of a polymer precursor have been carried out using modeling, Differential Thermal Analysis (DTA), and melt infiltration. Mercury porosimetry results indicate a very narrow pore size distribution with virtually all the porosity within the carbon preforms open to infiltrants. The morphology and amount of the residual phases (niobium disilicide and silicon) in the infiltrated material can be tailored according to requirements by careful control of the properties (pore size and pore volume) of the porous carbon preforms and alloy composition. The average room temperature four-point flexural strength of a reaction-formed silicon carbide material (made by the infiltration of medium pore size carbon preform with Si - 5 at. % Nb alloy) is 290 +/- 40 MPa (42 +/- 6 ksi) and the fracture toughness is 3.7 +/- 0.3 MPa square root of m. The flexural strength decreases at high temperatures due to relaxation of residual thermal stresses and the presence of free silicon in the material.

A Nanopore-Structured Nitrogen-Doped Biocarbon Electrocatalyst for Oxygen Reduction from Two-Step Carbonization of Lemna minor Biomass

NASA Astrophysics Data System (ADS)

Guo, Chaozhong; Li, Zhongbin; Niu, Lidan; Liao, Wenli; Sun, Lingtao; Wen, Bixia; Nie, Yunqing; Cheng, Jing; Chen, Changguo

2016-05-01

So far, the development of highly active and stable carbon-based electrocatalysts for oxygen reduction reaction (ORR) to replace commercial Pt/C catalyst is a hot topic. In this study, a new nanoporous nitrogen-doped carbon material was facilely designed by two-step pyrolysis of the renewable Lemna minor enriched in crude protein under a nitrogen atmosphere. Electrochemical measurements show that the onset potential for ORR on this carbon material is around 0.93 V (versus reversible hydrogen electrode), slightly lower than that on the Pt/C catalyst, but its cycling stability is higher compared to the Pt/C catalyst in an alkaline medium. Besides, the ORR at this catalyst approaches to a four-electron transfer pathway. The obtained ORR performance can be basically attributed to the formation of high contents of pyridinic and graphitic nitrogen atoms inside this catalyst. Thus, this work opens up the path in the ORR catalysis for the design of nitrogen-doped carbon materials utilizing aquatic plants as starting precursors.

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

Milbrandt, Anelia; Booth, Samuel

Carbon fiber (CF), known also as graphite fiber, is a lightweight, strong, and flexible material used in both structural (load-bearing) and non-structural applications (e.g., thermal insulation). The high cost of precursors (the starting material used to make CF, which comes predominately from fossil sources) and manufacturing have kept CF a niche market with applications limited mostly to high-performance structural materials (e.g., aerospace). Alternative precursors to reduce CF cost and dependence on fossil sources have been investigated over the years, including biomass-derived precursors such as rayon, lignin, glycerol, and lignocellulosic sugars. The purpose of this study is to provide a comprehensivemore » overview of CF precursors from biomass and their market potential. We examine the potential CF production from these precursors, the state of technology and applications, and the production cost (when data are available). We discuss their advantages and limitations. We also discuss the physical properties of biomass-based CF, and we compare them to those of polyacrylonitrile (PAN)-based CF. We also discuss manufacturing and end-product considerations for bio-based CF, as well as considerations for plant siting and biomass feedstock logistics, feedstock competition, and risk mitigation strategies. The main contribution of this study is that it provides detailed technical and market information about each bio-based CF precursor in one document while other studies focus on one precursor at a time or a particular topic (e.g., processing). Thus, this publication allows for a comprehensive view of the CF potential from all biomass sources and serves as a reference for both novice and experienced professionals interested in CF production from alternative sources.« less

Sources and characteristics of organic matter in the Clackamas River, Oregon, related to the formation of disinfection by-products in treated drinking water

USGS Publications Warehouse

Carpenter, Kurt D.; Kraus, Tamara E.C.; Goldman, Jami H.; Saraceno, John Franco; Downing, Bryan D.; Bergamaschi, Brian A.; McGhee, Gordon; Triplett, Tracy

2013-01-01

This study characterized the amount and quality of organic matter in the Clackamas River, Oregon, to gain an understanding of sources that contribute to the formation of chlorinated and brominated disinfection by-products (DBPs), focusing on regulated DBPs in treated drinking water from two direct-filtration treatment plants that together serve approximately 100,000 customers. The central hypothesis guiding this study was that natural organic matter leaching out of the forested watershed, in-stream growth of benthic algae, and phytoplankton blooms in the reservoirs contribute different and varying proportions of organic carbon to the river. Differences in the amount and composition of carbon derived from each source affects the types and concentrations of DBP precursors entering the treatment plants and, as a result, yield varying DBP concentrations and species in finished water. The two classes of DBPs analyzed in this study-trihalomethanes (THMs) and haloacetic acids (HAAs)-form from precursors within the dissolved and particulate pools of organic matter present in source water. The five principal objectives of the study were to (1) describe the seasonal quantity and character of organic matter in the Clackamas River; (2) relate the amount and composition of organic matter to the formation of DBPs; (3) evaluate sources of DBP precursors in the watershed; (4) assess the use of optical measurements, including in-situ fluorescence, for estimating dissolved organic carbon (DOC) concentrations and DBP formation; and (5) assess the removal of DBP precursors during treatment by conducting treatability "jar-test" experiments at one of the treatment plants. Data collection consisted of (1) monthly sampling of source and finished water at two drinking-water treatment plants; (2) event-based sampling in the mainstem, tributaries, and North Fork Reservoir; and (3) in-situ continuous monitoring of fluorescent dissolved organic matter (FDOM), turbidity, chlorophyll-a, and other constituents to continuously track source-water conditions in near real-time. Treatability tests were conducted during the four event-based surveys to determine the effectiveness of coagulant and powdered activated carbon (PAC) on the removal of DBP precursors. Sample analyses included DOC, total particulate carbon (TPC), total and dissolved nutrients, absorbance and fluorescence spectroscopy, and, for regulated DBPs, concentrations of THMs and HAAs in finished water and laboratory-based THM and HAA formation potentials (THMFP and HAAFP, respectively) for source water and selected locations throughout the watershed. The results of this study may not be typical given the record and near record amounts of precipitation that occurred during spring that produced streamflow much higher than average in 2010-11. Although there were algal blooms, lower concentrations of chlorophyll-a were observed in the water column during the study period compared to historical data. Concentrations of DBPs in finished (treated) water averaged 0.024 milligrams per liter (mg/L) for THMs and 0.022 mg/L for HAAs; maximum values were about 0.040 mg/L for both classes of DBPs. Although DBP concentrations were somewhat higher within the distribution system, none of the samples collected for this study or for the quarterly compliance monitoring by the water utilities exceeded levels permissible under existing U.S. Environmental Protection Agency (USEPA) regulations: 0.080 mg/L for THMs and 0.060 mg/L for HAAs. DOC concentrations were generally low in the Clackamas River, typically about 1.0-1.5 mg/L. Concentrations in the mainstem occasionally increased to nearly 2.5 mg/L during storms; DOC concentrations in tributaries were sometimes much higher (up to 7.8 mg/L). The continuous in-situ FDOM measurements indicated sharp rises in DOC concentrations in the mainstem following rainfall events; concentrations were relatively stable during summer base flow. Even though the first autumn storm mobilized appreciable quantities of carbon, higher concentrations of DBPs in finished water were observed 3-weeks later, after the ground was saturated from additional rainfall. The majority of the DOC in the lower Clackamas River appears to originate from the upper basin, suggesting terrestrial carbon was commonly the dominant source. Lower-basin tributaries typically contained the highest concentrations of DOC and DBP precursors and contributed substantially to the overall loads in the mainstem during storms. During low-flow periods, tributaries were not major sources of DOC or DBP precursors to the Clackamas River. Although the dissolved fraction of organic carbon contributed the majority of DBP precursors, at times the particulate fraction (inorganic sediment and organic particles including detritus and algal material) contributed a substantial fraction of DBP precursors. Considering just the main-stem sites, on average, 10 percent of THMFP and 32 percent of HAAFP were attributed to particulate carbon. This finding suggests water-treatment methods that remove particles prior to chlorination would reduce finished-water DBP concentrations to some degree. Overall, concentrations of THM and HAA precursors were closely linked to DOC concentrations; laboratory DBP formation potentials (DBPFPs) clearly showed that THMFP and HAAFP were greatest in the downstream tributaries that contained elevated carbon concentrations. However, carbon-normalized "specific" formation potentials for THMs and HAAs (STHMFP and SHAAFP, respectively) revealed changes in carbon character over time that affected the two types of DBP classes differently. HAA precursors were elevated in waters containing aromatic-rich soil-derived material arising from forested areas. In contrast, THM precursors were associated with carbon having a lower aromatic content; highest STHMFP occurred in autumn 2011 in the mainstem from North Fork Reservoir downstream to LO DWTP. This pattern suggests the potential for a link between THM precursors and algal-derived carbon. The highest STHMFP value was measured within North Fork Reservoir, indicating reservoir derived carbon may be important for this class of DBPs. Weak correlations between STHMFP and SHAAFP emphasize that precursor sources for these types of DBPs may be different. This highlights not only that different locations within the watershed produce carbon with different reactivity (specific DBPFP), but also that different management approaches for each class of DBP precursors could be required for control. Treatability tests conducted on source water during four basin-wide surveys demonstrated that an average of about 40 percent of DOC can be removed by coagulation. While the decrease in THMFP following coagulation was similar to DOC, the decrease in HAAFP was much greater (approximately 70 percent), indicating coagulation is particularly effective at removing HAA precursors'likely because of the aromatic nature of the carbon associated with HAA precursors. Several findings from this study have direct implications for managing drinking-water resources and for providing useful information that may help improve treatment-plant operations. For example, the use of in-situ fluorometers that measure FDOM provided an excellent proxy for DOC concentration in this system and revealed short-term, rapid changes in DOC concentration during storm events. In addition, the strong correlation between FDOM values measured in-situ and HAA5 concentrations in finished water may permit estimation of continuous HAA concentrations, as was done here. As part of this study, multiple in-situ FDOM sensors were deployed continuously and in real-time to characterize the composition of dissolved organic matter. Although the initial results were promising, additional research and engineering developments will be needed to demonstrate the full utility of these sensors for this purpose. In conclusion, although DBPFPs were strongly correlated to DOC concentration, some DBPs formed from particulate carbon, including terrestrial leaf material and algal material such as planktonic species of blue-green algae and sloughed filaments, stalks, and cells of benthic algae. Different precursor sources in the watershed were evident from the data, suggesting specific actions may be available to address some of these sources. In-situ measurements of FDOM proved to be an excellent proxy for DOC concentration as well as HAA formation during treatment, which suggests further development and refinement of these sensors have the potential to provide real-time information about complex watershed processes to operators at the drinking-water treatment plants. Follow-up studies could examine the relative roles that terrestrial and algal sources have on the DBP precursor pool to better understand how watershed-management activities may be affecting the transport of these compounds to Clackamas River drinking-water intakes. Given the low concentrations of algae in the water column during this study, additional surveys during more typical river conditions could provide a more complete understanding of how algae contribute DBP precursors. Further development of FDOM-sensor technology can improve our understanding of carbon dynamics in the river and how concentrations may be trending over time. This study was conducted in collaboration with Clackamas River Water and the City of Lake Oswego water utilities. Other research partners included Oregon Health and Science University in Hillsboro, Oregon, Alexin Laboratory in Tigard, Oregon, U.S. Geological Survey National Research Program Laboratory in Denver, Colorado, and the U.S. Geological Survey Water Science Centers in Portland, Oregon, and Sacramento, California. This project was supported with funding from Clackamas River Water, City of Lake Oswego, the U.S. Geological Survey, and the Water Research Foundation.

Three-dimensional hierarchical and interconnected honeycomb-like porous carbon derived from pomelo peel for high performance supercapacitors

NASA Astrophysics Data System (ADS)

Liu, Jingyuan; Li, Hongpeng; Zhang, Hongsen; Liu, Qi; Li, Rumin; Li, Bin; Wang, Jun

2018-01-01

The urgent need for sustainable development of human society has forced material scientists to explore novel materials starting from cheap natural precursors for next-generation energy storage devices by using environmentally friendly strategies. In this work, heteroatom-functionalized porous carbonaceous materials with 3D hierarchical and interconnected honeycomb-like structure have been successfully synthesized by using waste biomass pomelo peel as raw material through the combination of hydrothermal carbonization and followed KOH activation procedure. Benefiting from the unique honeycomb-like structure and high specific surface area, the as-obtained carbon material exhibits satisfactory capacitive behavior: 374 F/g at 0.1 A/g; excellent cycling stability of 92.5% capacitance retention over continuous 5000 cycles. More importantly, the as-assembled symmetric supercapacitors based on as-prepared electrode material can deliver high gravimetric and volumetric energy density of 20 W h/kg and 18.7 W h/L in 6 M KOH, respectively, as well as outstanding cycling stability. The obtained results demonstrate the possibility for taking full advantage of sustainable and large scale advanced carbon materials by choosing waste biomass, particularly the pomelo peel as a raw material.

Porous carbons prepared by direct carbonization of MOFs for supercapacitors

NASA Astrophysics Data System (ADS)

Yan, Xinlong; Li, Xuejin; Yan, Zifeng; Komarneni, Sridhar

2014-07-01

Three porous carbons were prepared by direct carbonization of HKUST-1, MOF-5 and Al-PCP without additional carbon precursors. The carbon samples obtained by carbonization at 1073 K were characterized by XRD, TEM and N2 physisorption techniques followed by testing for electrochemical performance. The BET surface areas of the three carbons were in the range of 50-1103 m2/g. As electrode materials for supercapacitor, the MOF-5 and Al-PCP derived carbons displayed the ideal capacitor behavior, whereas the HKUST-1 derived carbon showed poor capacitive behavior at various sweep rates and current densities. Among those carbon samples, Al-PCP derived carbons exhibited highest specific capacitance (232.8 F/g) in 30% KOH solution at the current density of 100 mA/g.

The Conversion of Starch and Sugars into Branched C10 and C11 Hydrocarbons.

PubMed

Sutton, Andrew D; Kim, Jin K; Wu, Ruilian; Hoyt, Caroline B; Kimball, David B; Silks, Louis A; Gordon, John C

2016-09-08

Oligosaccharides, such as starch, cellulose, and hemicelluloses, are abundant and easily obtainable bio-derived materials that can potentially be used as precursors for fuels and chemical feedstocks. To access the pertinent molecular building blocks (i.e., 5- or 6-carbon containing sugar units) located within these biopolymers and transform them into useful fuel precursors, oligosaccharide depolymerization followed by chain extension is required. This chain extension can readily be performed via a Garcia-Gonzalez-like approach using β-diketones under mild conditions to provide fuel precursors containing an increased carbon atom content that meets fuel requirements. In a subsequent step, ring opening and hydrodeoxygenation chemistry of these species allows for the preparation of branched alkanes under relatively mild conditions. This approach can be applied to monomeric sugars (glucose and xylose), oligosaccharides (starch), and potentially to hydrolyzed dedicated energy crops to allow the conversion of real biomass into fuel type molecules. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Low-loss binder for hot pressing boron nitride

DOEpatents

Maya, Leon

1991-01-01

Borazine derivatives used as low-loss binders and precursors for making ceramic boron nitride structures. The derivative forms the same composition as the boron nitride starting material, thereby filling the voids with the same boron nitride material upon forming and hot pressing. The derivatives have a further advantage of being low in carbon thus resulting in less volatile byproduct that can result in bubble formation during pressing.

Effect of cetyl trimethyl ammonium bromide concentration on structure, morphology and carbon dioxide adsorption capacity of calcium hydroxide based sorbents

NASA Astrophysics Data System (ADS)

Hlaing, Nwe Ni; Vignesh, K.; Sreekantan, Srimala; Pung, Swee-Yong; Hinode, Hirofumi; Kurniawan, Winarto; Othman, Radzali; Thant, Aye Aye; Mohamed, Abdul Rahman; Salim, Chris

2016-02-01

Calcium hydroxide (Ca(OH)2) has been proposed as an important material for industrial, architectural, and environmental applications. In this study, calcium acetate was used as a precursor and cetyl trimethyl ammonium bromide (CTAB) was used as a surfactant to synthesize Ca(OH)2 based adsorbents for carbon dioxide (CO2) capture. The effect of CTAB concentration (0.2-0.8 M) on the structure, morphology and CO2 adsorption performance of Ca(OH)2 was studied in detail. The synthesized samples were characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, field emission scanning electron microscopy (FESEM), BET surfaced area and thermogravimetry-differential thermal analysis (TG-DTA) techniques. The phase purity, crystallite size, Brunauer-Emmett-Teller (BET) surface area and CO2 adsorption performance of Ca(OH)2 precursor adsorbents were significantly increased when the concentration of CTAB was increased. XRD results showed that pure Ca(OH)2 phase was obtained at the CTAB concentration of 0.8 M. TGA results exhibited that 0.8 M of CTAB-assisted Ca(OH)2 precursor adsorbent possessed a residual carbonation conversion of ∼56% after 10 cycles.

Co@Carbon and Co 3 O4@Carbon nanocomposites derived from a single MOF for supercapacitors.

PubMed

Dai, Engao; Xu, Jiao; Qiu, Junjie; Liu, Shucheng; Chen, Ping; Liu, Yi

2017-10-03

Developing a composite electrode containing both carbon and transition metal/metal oxide as the supercapacitor electrode can combine the merits and mitigate the shortcomings of both the components. Herein, we report a simple strategy to prepare the hybrid nanostructure of Co@Carbon and Co 3 O 4 @Carbon by pyrolysis a single MOFs precursor. Co-based MOFs (Co-BDC) nanosheets with morphology of regular parallelogram slice have been prepared by a bottom-up synthesis strategy. One-step pyrolysis of Co-BDC, produces a porous carbon layer incorporating well-dispersed Co and Co 3 O 4 nanoparticles. The as-prepared cobalt-carbon composites exhibit the thin layer morphology and large specific surface area with hierarchical porosity. These features significantly improve the ion-accessible surface area for charge storage and shorten the ion transport length in thin dimension, thus contributing to a high specific capacitance. Improved capacitance performance was successfully realized for the asymmetric supercapacitors (ASCs) (Co@Carbon//Co 3 O 4 @Carbon), better than those of the symmetric supercapacitors (SSCs) based on Co@Carbon and Co 3 O 4 @Carbon materials (i.e., Co@Carbon//Co@Carbon and Co 3 O 4 @Carbon//Co 3 O 4 @Carbon). The working voltage of the ASCs can be extended to 1.5 V and show a remarkable high power capability in aqueous electrolyte. This work provides a controllable strategy for nanostructured carbon-metal and carbon-metal oxide composite electrodes from a single precursor.

Recent advances in functionalized micro and mesoporous carbon materials: synthesis and applications.

PubMed

Benzigar, Mercy R; Talapaneni, Siddulu Naidu; Joseph, Stalin; Ramadass, Kavitha; Singh, Gurwinder; Scaranto, Jessica; Ravon, Ugo; Al-Bahily, Khalid; Vinu, Ajayan

2018-04-23

Functionalized nanoporous carbon materials have attracted the colossal interest of the materials science fraternity owing to their intriguing physical and chemical properties including a well-ordered porous structure, exemplary high specific surface areas, electronic and ionic conductivity, excellent accessibility to active sites, and enhanced mass transport and diffusion. These properties make them a special and unique choice for various applications in divergent fields such as energy storage batteries, supercapacitors, energy conversion fuel cells, adsorption/separation of bulky molecules, heterogeneous catalysts, catalyst supports, photocatalysis, carbon capture, gas storage, biomolecule detection, vapour sensing and drug delivery. Because of the anisotropic and synergistic effects arising from the heteroatom doping at the nanoscale, these novel materials show high potential especially in electrochemical applications such as batteries, supercapacitors and electrocatalysts for fuel cell applications and water electrolysis. In order to gain the optimal benefit, it is necessary to implement tailor made functionalities in the porous carbon surfaces as well as in the carbon skeleton through the comprehensive experimentation. These most appealing nanoporous carbon materials can be synthesized through the carbonization of high carbon containing molecular precursors by using soft or hard templating or non-templating pathways. This review encompasses the approaches and the wide range of methodologies that have been employed over the last five years in the preparation and functionalisation of nanoporous carbon materials via incorporation of metals, non-metal heteroatoms, multiple heteroatoms, and various surface functional groups that mostly dictate their place in a wide range of practical applications.

Lightweight Ceramic Composition of Carbon Silicon Oxygen and Boron

NASA Technical Reports Server (NTRS)

Leiser, Daniel B. (Inventor); Hsu, Ming-Ta (Inventor); Chen, Timothy S. (Inventor)

1997-01-01

Lightweight, monolithic ceramics resistant to oxidation in air at high temperatures are made by impregnating a porous carbon preform with a sol which contains a mixture of tetraethoxysilane, dimethyldiethoxysilane and trimethyl borate. The sol is gelled and dried on the carbon preform to form a ceramic precursor. The precursor is pyrolyzed in an inert atmosphere to form the ceramic which is made of carbon, silicon, oxygen and boron. The carbon of the preform reacts with the dried gel during the pyrolysis to form a component of the resulting ceramic. The ceramic is of the same size, shape and form as the carbon precursor. Thus, using a porous, fibrous carbon precursor, such as a carbon felt, results in a porous, fibrous ceramic. Ceramics of the invention are useful as lightweight tiles for a reentry spacecraft.

Microbial degradation of plant leachate alters lignin phenols and trihalomethane precursors

USGS Publications Warehouse

Pellerin, Brian A.; Hernes, Peter J.; Saraceno, John Franco; Spencer, Robert G.M.; Bergamaschi, Brian A.

2010-01-01

Although the importance of vascular plant-derived dissolved organic carbon (DOC) in freshwater systems has been studied, the role of leached DOC as precursors of disinfection byproducts (DBPs) during drinking water treatment is not well known. Here we measured the propensity of leachates from four crops and four aquatic macrophytes to form trihalomethanes (THMs)—a regulated class of DBPs—before and after 21 d of microbial degradation. We also measured lignin phenol content and specific UV absorbance (SUVA254) to test the assumption that aromatic compounds from vascular plants are resistant to microbial degradation and readily form DBPs. Leaching solubilized 9 to 26% of total plant carbon, which formed 1.93 to 6.72 mmol THM mol C-1 However, leachate DOC concentrations decreased by 85 to 92% over the 21-d incubation, with a concomitant decrease of 67 to 92% in total THM formation potential. Carbon-normalized THM yields in the residual DOC pool increased by 2.5 times on average, consistent with the preferential uptake of nonprecursor material. Lignin phenol concentrations decreased by 64 to 96% over 21 d, but a lack of correlation between lignin content and THM yields or SUVA254 suggested that lignin-derived compounds are not the source of increased THM precursor yields in the residual DOC pool. Our results indicate that microbial carbon utilization alters THM precursors in ecosystems with direct plant leaching, but more work is needed to identify the specific dissolved organic matter components with a greater propensity to form DBPs and affect watershed management, drinking water quality, and human health.

Silk-regulated hierarchical hollow magnetite/carbon nanocomposite spheroids for lithium-ion battery anodes.

PubMed

Sheng, Weiqin; Zhu, Guobin; Kaplan, David L; Cao, Chuanbao; Zhu, Hesun; Lu, Qiang

2015-03-20

Hierarchical olive-like structured carbon-Fe3O4 nanocomposite particles composed of a hollow interior and a carbon coated surface are prepared by a facile, silk protein-assisted hydrothermal method. Silk nanofibers as templates and carbon precursors first regulate the formation of hollow Fe2O3 microspheres and then they are converted into carbon by a reduction process into Fe3O4. This process significantly simplifies the fabrication and carbon coating processes to form complex hollow structures. When tested as anode materials for lithium-ion batteries, these hollow carbon-coated particles exhibit high capacity (900 mAh g(-1)), excellent cycle stability (180 cycles) and rate performance due to their unique hierarchical hollow structure and carbon coating.

Carbonized Micro- and Nanostructures: Can Downsizing Really Help?

PubMed Central

Naraghi, Mohammad; Chawla, Sneha

2014-01-01

In this manuscript, we discuss relationships between morphology and mechanical strength of carbonized structures, obtained via pyrolysis of polymeric precursors, across multiple length scales, from carbon fibers (CFs) with diameters of 5–10 μm to submicron thick carbon nanofibers (CNFs). Our research points to radial inhomogeneity, skin–core structure, as a size-dependent feature of polyacrylonitrile-based CFs. This inhomogeneity is a surface effect, caused by suppressed diffusion of oxygen and stabilization byproducts during stabilization through skin. Hence, reducing the precursor diameters from tens of microns to submicron appears as an effective strategy to develop homogeneous carbonized structures. Our research establishes the significance of this downsizing in developing lightweight structural materials by comparing intrinsic strength of radially inhomogeneous CFs with that of radially homogeneous CNF. While experimental studies on the strength of CNFs have targeted randomly oriented turbostratic domains, via continuum modeling, we have estimated that strength of CNFs can reach 14 GPa, when the basal planes of graphitic domains are parallel to nanofiber axis. The CNFs in our model are treated as composites of amorphous carbon (matrix), reinforced with turbostratic domains, and their strength is predicted using Tsai–Hill criterion. The model was calibrated with existing experimental data. PMID:28788651

A cheap and non-destructive approach to increase coverage/loading of hydrophilic hydroxide on hydrophobic carbon for lightweight and high-performance supercapacitors.

PubMed

Zhang, Liuyang; Gong, Hao

2015-12-08

Carbon-based substrates offer unprecedented advantages in lightweight supercapacitors. However, it is still challenging to achieve high coverage or loading. Different from the traditional belief that a lack of defects or functional groups is the cause of poor growth on carbon-based substrates, we reckon that the major cause is the discrepancy between the hydrophilic nature of the metal oxide/hydroxide and the hydrophobic nature of carbon. To solve this incompatibility, we introduced ethanol into the precursor solution. The method to synthesize nickel copper hydroxide on carbon fiber paper employs only water and ethanol, in addition to nickel acetate and copper acetate. The results revealed good growth and tight adhesion of active materials on carbon fiber paper substrates. The specific capacitance and energy density per total weight of the active material plus substrate (carbon fiber paper, current collector) reached 770 F g(-1) and 33 Wh kg(-1) (1798 F g(-1) and 54 Wh kg(-1) per weight of the active materials), owing to the high loading of active material and the light weight of carbon fiber paper. These results signified the achievability of light, cheap and high-performance supercapacitors by an environmental-friendly approach.

A cheap and non-destructive approach to increase coverage/loading of hydrophilic hydroxide on hydrophobic carbon for lightweight and high-performance supercapacitors

NASA Astrophysics Data System (ADS)

Zhang, Liuyang; Gong, Hao

2015-12-01

Carbon-based substrates offer unprecedented advantages in lightweight supercapacitors. However, it is still challenging to achieve high coverage or loading. Different from the traditional belief that a lack of defects or functional groups is the cause of poor growth on carbon-based substrates, we reckon that the major cause is the discrepancy between the hydrophilic nature of the metal oxide/hydroxide and the hydrophobic nature of carbon. To solve this incompatibility, we introduced ethanol into the precursor solution. The method to synthesize nickel copper hydroxide on carbon fiber paper employs only water and ethanol, in addition to nickel acetate and copper acetate. The results revealed good growth and tight adhesion of active materials on carbon fiber paper substrates. The specific capacitance and energy density per total weight of the active material plus substrate (carbon fiber paper, current collector) reached 770 F g-1 and 33 Wh kg-1 (1798 F g-1 and 54 Wh kg-1 per weight of the active materials), owing to the high loading of active material and the light weight of carbon fiber paper. These results signified the achievability of light, cheap and high-performance supercapacitors by an environmental-friendly approach.

A cheap and non-destructive approach to increase coverage/loading of hydrophilic hydroxide on hydrophobic carbon for lightweight and high-performance supercapacitors

PubMed Central

Zhang, Liuyang; Gong, Hao

2015-01-01

Carbon-based substrates offer unprecedented advantages in lightweight supercapacitors. However, it is still challenging to achieve high coverage or loading. Different from the traditional belief that a lack of defects or functional groups is the cause of poor growth on carbon-based substrates, we reckon that the major cause is the discrepancy between the hydrophilic nature of the metal oxide/hydroxide and the hydrophobic nature of carbon. To solve this incompatibility, we introduced ethanol into the precursor solution. The method to synthesize nickel copper hydroxide on carbon fiber paper employs only water and ethanol, in addition to nickel acetate and copper acetate. The results revealed good growth and tight adhesion of active materials on carbon fiber paper substrates. The specific capacitance and energy density per total weight of the active material plus substrate (carbon fiber paper, current collector) reached 770 F g−1 and 33 Wh kg−1 (1798 F g−1 and 54 Wh kg−1 per weight of the active materials), owing to the high loading of active material and the light weight of carbon fiber paper. These results signified the achievability of light, cheap and high-performance supercapacitors by an environmental-friendly approach. PMID:26643665

Hard Carbon Originated from Polyvinyl Chloride Nanofibers As High-Performance Anode Material for Na-Ion Battery

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

Bai, Ying; Wang, Zhen; Wu, Chuan

2015-02-27

Two types of hard carbon materials were synthesized through direct pyrolysis of commercial polyvinyl chloride (PVC) particles and pyrolysis of PVC nanofibers at 600-800 degrees C, respectively, where the nanofibers were prepared by an electrospinning PVC precursors method. These as-prepared hard carbon samples were used as anode materials for Na-ion batteries. The hard carbon obtained from PVC nanofibers achieved a high reversible capacity of 271 mAh/g and an initial Coulombic efficiency of 69.9%, which were much superior to the one from commercial PVC, namely, a reversible capacity of 206 mAh/g and an initial Coulombic efficiency of 60.9%. In addition, themore » hard carbon originated from the PVC nanofibers exhibited good cycling stability and rate performance: the initial discharge capacities were 389, 228, 194, 178, 147 mAh/g at the current density of 12, 24, 60, 120, and 240 mA/g, respectively, retaining 211 mAh/g after 150 cycles. Such excellent cycle performance, high reversible capacity, and good rate capability enabled this hard carbon to be a promising candidate as anode material for Na-ion battery application.« less

Hard carbon originated from polyvinyl chloride nanofibers as high-performance anode material for Na-ion battery.

PubMed

Bai, Ying; Wang, Zhen; Wu, Chuan; Xu, Rui; Wu, Feng; Liu, Yuanchang; Li, Hui; Li, Yu; Lu, Jun; Amine, Khalil

2015-03-11

Two types of hard carbon materials were synthesized through direct pyrolysis of commercial polyvinyl chloride (PVC) particles and pyrolysis of PVC nanofibers at 600-800 °C, respectively, where the nanofibers were prepared by an electrospinning PVC precursors method. These as-prepared hard carbon samples were used as anode materials for Na-ion batteries. The hard carbon obtained from PVC nanofibers achieved a high reversible capacity of 271 mAh/g and an initial Coulombic efficiency of 69.9%, which were much superior to the one from commercial PVC, namely, a reversible capacity of 206 mAh/g and an initial Coulombic efficiency of 60.9%. In addition, the hard carbon originated from the PVC nanofibers exhibited good cycling stability and rate performance: the initial discharge capacities were 389, 228, 194, 178, 147 mAh/g at the current density of 12, 24, 60, 120, and 240 mA/g, respectively, retaining 211 mAh/g after 150 cycles. Such excellent cycle performance, high reversible capacity, and good rate capability enabled this hard carbon to be a promising candidate as anode material for Na-ion battery application.

Pectin, Hemicellulose, or Lignin? Impact of the Biowaste Source on the Performance of Hard Carbons for Sodium-Ion Batteries.

PubMed

Dou, Xinwei; Hasa, Ivana; Hekmatfar, Maral; Diemant, Thomas; Behm, R Jürgen; Buchholz, Daniel; Passerini, Stefano

2017-06-22

Hard carbons are currently the most widely used negative electrode materials in Na-ion batteries. This is due to their promising electrochemical performance with capacities of 200-300 mAh g -1 and stable long-term cycling. However, an abundant and cheap carbon source is necessary in order to comply with the low-cost philosophy of Na-ion technology. Many biological or waste materials have been used to synthesize hard carbons but the impact of the precursors on the final properties of the anode material is not fully understood. In this study the impact of the biomass source on the structural and electrochemical properties of hard carbons is unraveled by using different, representative types of biomass as examples. The systematic structural and electrochemical investigation of hard carbons derived from different sources-namely corncobs, peanut shells, and waste apples, which are representative of hemicellulose-, lignin- and pectin-rich biomass, respectively-enables understanding and interlinking of the structural and electrochemical properties. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Design and synthesis of single-source molecular precursors to homogeneous multi-component oxide materials

NASA Astrophysics Data System (ADS)

Fujdala, Kyle Lee

This dissertation describes the syntheses of single-source molecular precursors to multi-component oxide materials. These molecules possess a core metal or element with various combinations of -OSi(O tBu)3, -O2P(OtBu) 2, and -OB[OSi(OtBu)3] 2 ligands. Such molecules decompose under mild thermolytic conditions (<200°C) to provide homogeneous carbon-free materials via the elimination of isobutylene and water. A gel is formed when thermolyses are performed in non-polar solvents, and subsequent drying of the gel in a conventional manner yields high surface area xerogels. This thermolytic molecular precursor (TMP) approach has been utilized to provide a variety of oxide materials with tailored properties. In addition, the oxygen rich environment of the molecular precursors coupled with the presence of M-O-E heterolinkages permits use of them as models for oxide-supported metal species and multi-component oxides. Significantly, the first complexes to contain three or more heteroelements suitable for use in the TMP method have been synthesized. Compounds for use as single-source molecular precursors have been synthesized containing Al, B, Cr, Hf, Mo, V, W, and Zr, and their thermal transformations have been examined. Heterogeneous catalytic reactions have been examined for selected materials. Also, cothermolyses of molecular precursors and additional molecules (i.e., metal alkoxides) have been utilized to provide materials with several components for potential use as catalysts or catalyst supports. Reactions of one and two equivs of HOSi(OtBu) 3 with Cr(OtBu)4 afforded the first Cr(IV) alkoxysiloxy complexes (tBuO) 3CrOSi(OtBu)3 and ( tBuO)2Cr[OSi(OtBu) 3]2, respectively. The high-yielding, convenient synthesis of (tBuO)3CrOSi(O tBu)3 make this complex a useful single-source molecular precursor, via the TMP method, to Cr/Si/O materials. The thermal transformations of (tBuO)3CrOSi(O tBu)3 and (tBuO) 2Cr[OSi(OtBu)3]2 to chromia-silica materials occurr at low temperatures (≤180°C), to give isobutene as the major carbon-containing product. The material generated from the solid-state conversion of (tBuO) 3CrOSi(OtBu)3 (CrOS ss) has an unexpectedly high surface area of 315 m2 g-1 that is slightly reduced to 275 m2 g-1 after calcination at 500°C in O2. The xerogel obtained by the thermolysis of an n-octane solution of (tBuO)3CrOSi(O tBu)3 (CrOSixg) has a surface area of 315 m2 g-1 that is reduced to 205 m2 g-1 upon calcination at 500°C. Powder X-ray diffraction (PXRD) analysis revealed that Cr2O 3 is the only crystalline species present in CrOSiss and CrOSixg after calcination at temperatures up to 1200°C in O2. (Abstract shortened by UMI.)

N- and S-doped high surface area carbon derived from soya chunks as scalable and efficient electrocatalysts for oxygen reduction

NASA Astrophysics Data System (ADS)

Rana, Moumita; Arora, Gunjan; Gautam, Ujjal K.

2015-02-01

Highly stable, cost-effective electrocatalysts facilitating oxygen reduction are crucial for the commercialization of membrane-based fuel cell and battery technologies. Herein, we demonstrate that protein-rich soya chunks with a high content of N, S and P atoms are an excellent precursor for heteroatom-doped highly graphitized carbon materials. The materials are nanoporous, with a surface area exceeding 1000 m2 g-1, and they are tunable in doping quantities. These materials exhibit highly efficient catalytic performance toward oxygen reduction reaction (ORR) with an onset potential of -0.045 V and a half-wave potential of -0.211 V (versus a saturated calomel electrode) in a basic medium, which is comparable to commercial Pt catalysts and is better than other recently developed metal-free carbon-based catalysts. These exhibit complete methanol tolerance and a performance degradation of merely ˜5% as compared to ˜14% for a commercial Pt/C catalyst after continuous use for 3000 s at the highest reduction current. We found that the fraction of graphitic N increases at a higher graphitization temperature, leading to the near complete reduction of oxygen. It is believed that due to the easy availability of the precursor and the possibility of genetic engineering to homogeneously control the heteroatom distribution, the synthetic strategy is easily scalable, with further improvement in performance.

N- and S-doped high surface area carbon derived from soya chunks as scalable and efficient electrocatalysts for oxygen reduction

PubMed Central

Rana, Moumita; Arora, Gunjan; Gautam, Ujjal K

2015-01-01

Highly stable, cost-effective electrocatalysts facilitating oxygen reduction are crucial for the commercialization of membrane-based fuel cell and battery technologies. Herein, we demonstrate that protein-rich soya chunks with a high content of N, S and P atoms are an excellent precursor for heteroatom-doped highly graphitized carbon materials. The materials are nanoporous, with a surface area exceeding 1000 m2 g−1, and they are tunable in doping quantities. These materials exhibit highly efficient catalytic performance toward oxygen reduction reaction (ORR) with an onset potential of −0.045 V and a half-wave potential of −0.211 V (versus a saturated calomel electrode) in a basic medium, which is comparable to commercial Pt catalysts and is better than other recently developed metal-free carbon-based catalysts. These exhibit complete methanol tolerance and a performance degradation of merely ∼5% as compared to ∼14% for a commercial Pt/C catalyst after continuous use for 3000 s at the highest reduction current. We found that the fraction of graphitic N increases at a higher graphitization temperature, leading to the near complete reduction of oxygen. It is believed that due to the easy availability of the precursor and the possibility of genetic engineering to homogeneously control the heteroatom distribution, the synthetic strategy is easily scalable, with further improvement in performance. PMID:27877746

Strongly coupled inorganic-nano-carbon hybrid materials for energy storage.

PubMed

Wang, Hailiang; Dai, Hongjie

2013-04-07

The global shift of energy production from fossil fuels to renewable energy sources requires more efficient and reliable electrochemical energy storage devices. In particular, the development of electric or hydrogen powered vehicles calls for much-higher-performance batteries, supercapacitors and fuel cells than are currently available. In this review, we present an approach to synthesize electrochemical energy storage materials to form strongly coupled hybrids (SC-hybrids) of inorganic nanomaterials and novel graphitic nano-carbon materials such as carbon nanotubes and graphene, through nucleation and growth of nanoparticles at the functional groups of oxidized graphitic nano-carbon. We show that the inorganic-nano-carbon hybrid materials represent a new approach to synthesize electrode materials with higher electrochemical performance than traditional counterparts made by simple physical mixtures of electrochemically active inorganic particles and conducting carbon materials. The inorganic-nano-carbon hybrid materials are novel due to possible chemical bonding between inorganic nanoparticles and oxidized carbon, affording enhanced charge transport and increased rate capability of electrochemical materials without sacrificing specific capacity. Nano-carbon with various degrees of oxidation provides a novel substrate for nanoparticle nucleation and growth. The interactions between inorganic precursors and oxidized-carbon substrates provide a degree of control over the morphology, size and structure of the resulting inorganic nanoparticles. This paper reviews the recent development of inorganic-nano-carbon hybrid materials for electrochemical energy storage and conversion, including the preparation and functionalization of graphene sheets and carbon nanotubes to impart oxygen containing groups and defects, and methods of synthesis of nanoparticles of various morphologies on oxidized graphene and carbon nanotubes. We then review the applications of the SC-hybrid materials for high performance lithium ion batteries, rechargeable Li-S and Li-O2 batteries, supercapacitors and ultrafast Ni-Fe batteries, and new electrocatalysts for oxygen reduction, oxygen evolution and hydrogen evolution reactions.

Low-Temperature Fluorination of Soft-Templated Mesoporous Carbons for a High-Power Lithium/Carbon Fluoride Battery

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

Fulvio, Pasquale F; Dai, Sheng; Guo, Bingkun

Soft-templated mesoporous carbons and activated mesoporous carbons were fluorinated using elemental fluorine between room temperature and 235 C. The mesoporous carbons were prepared via self-assembly synthesis of phloroglucinol formaldehyde as a carbon precursor in the presence of triblock ethylene oxide propylene oxide ethylene oxide copolymer BASF Pluronic F127 as the template. The F/C ratios ranged from 0.15 to 0.75 according to gravimetric, energy dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy analysis. Materials have mesopore diameters up to 11 nm and specific surface areas as high as 850 m2 g 1 after fluorination as calculated from nitrogen adsorption isotherms at 196more » C. Furthermore, the materials exhibit higher discharge potentials and energy and power densities as well as faster reaction kinetics under high current densities than commercial carbon fluorides with similar fluorine contents when tested as cathodes for Li/CFx batteries.« less

Using carbonized low-cost materials for removal of chemicals of environmental concern from water.

PubMed

Weidemann, Eva; Niinipuu, Mirva; Fick, Jerker; Jansson, Stina

2018-06-01

Adsorption on low-cost biochars would increase the affordability and availability of water treatment in, for example, developing countries. The aim of this study was to identify the precursor materials and hydrochar surface properties that yield efficient removal of compounds of environmental concern (CEC). We determined the adsorption kinetics of a mixture containing ten CECs (octhilinone, triclosan, trimethoprim, sulfamethoxasole, ciprofloxacin, diclofenac, paracetamol, diphenhydramine, fluconazole, and bisphenol A) to hydrochars prepared from agricultural waste (including tomato- and olive-press wastes, rice husks, and horse manure). The surface characteristics of the hydrochars were evaluated via diffuse reflectance infrared spectroscopy (DRIFTS), X-ray photoelectron spectroscopy (XPS), and N 2 -adsorption. Kinetic adsorption tests revealed that removal efficiencies varied substantially among different materials. Similarly, surface analysis revealed differences among the studied hydrochars and the degree of changes that the materials undergo during carbonization. According to the DRIFTS data, compared with the least efficient adsorbent materials, the most efficient hydrochars underwent more substantial changes during carbonization.

Synthesis of thin films in boron-carbon-nitrogen ternary system by microwave plasma enhanced chemical vapor deposition

NASA Astrophysics Data System (ADS)

Kukreja, Ratandeep Singh

The Boron Carbon Nitorgen (B-C-N) ternary system includes materials with exceptional properties such as wide band gap, excellent thermal conductivity, high bulk modulus, extreme hardness and transparency in the optical and UV range that find application in most fields ranging from micro-electronics, bio-sensors, and cutting tools to materials for space age technology. Interesting materials that belong to the B-C-N ternary system include Carbon nano-tubes, Boron Carbide, Boron Carbon Nitride (B-CN), hexagonal Boron Nitride ( h-BN), cubic Boron Nitride (c-BN), Diamond and beta Carbon Nitride (beta-C3N4). Synthesis of these materials requires precisely controlled and energetically favorable conditions. Chemical vapor deposition is widely used technique for deposition of thin films of ceramics, metals and metal-organic compounds. Microwave plasma enhanced chemical vapor deposition (MPECVD) is especially interesting because of its ability to deposit materials that are meta-stable under the deposition conditions, for e.g. diamond. In the present study, attempt has been made to synthesize beta-carbon nitride (beta-C3N4) and cubic-Boron Nitride (c-BN) thin films by MPECVD. Also included is the investigation of dependence of residual stress and thermal conductivity of the diamond thin films, deposited by MPECVD, on substrate pre-treatment and deposition temperature. Si incorporated CNx thin films are synthesized and characterized while attempting to deposit beta-C3N4 thin films on Si substrates using Methane (CH4), Nitrogen (N2), and Hydrogen (H2). It is shown that the composition and morphology of Si incorporated CNx thin film can be tailored by controlling the sequence of introduction of the precursor gases in the plasma chamber. Greater than 100mum size hexagonal crystals of N-Si-C are deposited when Nitrogen precursor is introduced first while agglomerates of nano-meter range graphitic needles of C-Si-N are deposited when Carbon precursor is introduced first in the deposition chamber. Hexagonal -- BN thin films are successfully deposited using Diborane (B2H6) (5% in H2), Ammonia (NH3) and H2 as precursor gases in the conventional MPECVD mode with and without the negative DC bias. The quality of h-BN in the films improved with pressure and when NH3 used as the first precursor gas in the deposition chamber. c-BN thin films are successfully deposited using Boron-Trifluoride (BF3) (10% in Argon (Ar)), N2, H2, Ar and Helium (He) gases in the electron cyclotron resonance (ECR) mode of the MPECVD system with negative DC bias. Up-to 66% c-BN in the films is achieved under deposition conditions of lower gas flow rates and higher deposition pressures than that reported in the literature for film deposited by ECR-MPECVD. It is shown that the percentage c-BN in the films correlates with the deposition pressure, BF3/H2 ratio and, negative DC bias during nucleation and growth. Diamond thin films are deposited using 60%Ar, 39% H2 and, 1%CH4 at 600°C, 700°C and 800°C substrate temperatures, measured by an IR pyrometer, on Si substrates pre-treated with 3-6nm diamond sol and 20-40mum diamond slurry. Raman spectroscopy, FTIR, X-Ray diffraction (XRD) and, photo-thermal reflectivity methods are used to characterize the thin films. Residual stresses observed for the diamond thin films deposited in this study are tensile in nature and increased with deposition temperature. Better quality diamond films with lower residual stresses are obtained for films deposited on Si substrate pre-treated with 3-6nm diamond sol. Preliminary results on thermal conductivity, k, suggest that k is directly dependent on the deposition temperature and independent of substrate pre-treatment signifying that the nano-seeding technique can be used to replace conventional surface activation technique for diamond seeding where needed.

Effect of Cerium Doped on the Poly(3-(Trimethoxysilyl)propyl methacrylate) Characteristic as Corrosion Protection Material of Carbon Steel

NASA Astrophysics Data System (ADS)

Rochmah, D. N.; Syakir, N.; Susilawati, T.; Suryaningsih, S.; Fitrilawati

2017-05-01

The hybrid polymer precursor was synthesized from monomer of 3-(trimethoxysilyl) propyl methacrylate (TMSPMA) using sol-gel method and doped with inhibitor of Cerium Nitrate Hexahydrate with a concentration of 0.2%. The synthesized material was coated on a carbon steel surface by solution casting technique and followed by a photopolymerisation process. Corrosion tests were performed by using Electrochemical Impedance Spectroscopy (EIS) in 3.5% NaCl at the critical temperature of 75°C. Result of EIS data and their fitting analysis using an equivalent circuit model shows that a coating of poly(TMSPMA)-Cerium on the surface of carbon steel form a layer of protection and caused increasing of impedance value significantly. The impedance is higher compared to the carbon steel that coated with poly(TMSPMA) only.

Carbon nanofibers with highly dispersed tin and tin antimonide nanoparticles: Preparation via electrospinning and application as the anode materials for lithium-ion batteries

NASA Astrophysics Data System (ADS)

Li, Zhi; Zhang, Jiwei; Shu, Jie; Chen, Jianping; Gong, Chunhong; Guo, Jianhui; Yu, Laigui; Zhang, Jingwei

2018-03-01

One-dimensional carbon nanofibers with highly dispersed tin (Sn) and tin antimonide (SnSb) nanoparticles are prepared by electrospinning in the presence of antimony-doped tin oxide (denoted as ATO) wet gel as the precursor. The effect of ATO dosage on the microstructure and electrochemical properties of the as-fabricated Sn-SnSb/C composite nanofibers is investigated. Results indicate that ATO wet gel as the precursor can effectively improve the dispersion of Sn nanoparticles in carbon fiber and prevent them from segregation during the electrospinning and subsequent calcination processes. The as-prepared Sn-SnSb/C nanofibers as the anode materials for lithium-ion batteries exhibit high reversible capacity and stable cycle performance. Particularly, the electrode made from Sn-SnSb/C composite nanofibers obtained with 0.9 g of ATO gel has a high specific capacity of 779 mAh·g-1 and 378 mAh·g-1 at the current density of 50 mA·g-1 and 5 A·g-1, respectively, and it exhibits a capacity retention of 97% after 1200 cycles under the current density of 1 A·g-1. This is because the carbon nanofibers can form a continuous conductive network to buffer the volume change of the electrodes while Sn and Sn-SnSb nanoparticles uniformly distributed in the carbon nanofibers are free of segregation, thereby contributing to electrochemical performances of the electrodes.

Heteroatom Polymer-Derived 3D High-Surface-Area and Mesoporous Graphene Sheet-Like Carbon for Supercapacitors.

PubMed

Sheng, Haiyang; Wei, Min; D'Aloia, Alyssa; Wu, Gang

2016-11-09

Current supercapacitors suffer from low energy density mainly due to the high degree of microporosity and insufficient hydrophilicity of their carbon electrodes. Development of a supercapacitor capable of simultaneously storing as much energy as a battery, along with providing sufficient power and long cycle stability would be valued for energy storage applications and innovations. Differing from commonly studied reduced graphene oxides, in this work we identified an inexpensive heteroatom polymer (polyaniline-PANI) as a carbon/nitrogen precursor, and applied a controlled thermal treatment at elevated temperature to convert PANI into 3D high-surface-area graphene-sheet-like carbon materials. During the carbonization process, various transition metals including Fe, Co, and Ni were added, which play critical roles in both catalyzing the graphitization and serving as pore forming agents. Factors including post-treatments, heating temperatures, and types of metal were found crucial for achieving enhanced capacitance performance on resulting carbon materials. Using FeCl 3 as precursor along with optimal heating temperature 1000 °C and mixed acid treatment (HCl+HNO 3 ), the highest Brunauer-Emmett-Teller (BET) surface area of 1645 m 2 g -1 was achieved on the mesopore dominant graphene-sheet-like carbon materials. The unique morphologies featured with high-surface areas, dominant mesopores, proper nitrogen doping, and 3D graphene-like structures correspond to remarkably enhanced electrochemical specific capacitance up to 478 Fg -1 in 1.0 M KOH at a scan rate of 5 mV s -1 . Furthermore, in a real two-electrode system of a symmetric supercapacitor, a specific capacitance of 235 Fg -1 using Nafion binder is obtained under a current density of 1 Ag -1 by galvanostatic charge-discharge tests in 6.0 M KOH. Long-term cycle stability up to 5000 cycles by using PVDF binder in electrode was systematically evaluated as a function of types of metals and current densities.

Nitrogen-Functionalized Hydrothermal Carbon Materials by Using Urotropine as the Nitrogen Precursor.

PubMed

Straten, Jan Willem; Schleker, Philipp; Krasowska, Małgorzata; Veroutis, Emmanouil; Granwehr, Josef; Auer, Alexander A; Hetaba, Walid; Becker, Sylvia; Schlögl, Robert; Heumann, Saskia

2018-03-25

Nitrogen-containing hydrothermal carbon (N-HTC) materials of spherical particle morphology were prepared by means of hydrothermal synthesis with glucose and urotropine as precursors. The molar ratio of glucose to urotropine has been varied to achieve a continuous increase in nitrogen content. By raising the ratio of urotropine to glucose, a maximal nitrogen fraction of about 19 wt % could be obtained. Decomposition products of both glucose and urotropine react with each other; this opens up a variety of possible reaction pathways. The pH has a pronounced effect on the reaction pathway of the corresponding reaction steps. For the first time, a comprehensive analytical investigation, comprising a multitude of analytical tools and instruments, of a series of nitrogen-containing HTC materials was applied. Functional groups and structural motifs identified were analyzed by means of FTIR spectroscopy, thermogravimetric MS, and solid-state NMR spectroscopy. Information on reaction mechanisms and structural details were obtained by electronic structure calculations that were compared with vibrational spectra of polyfuran or polypyrrole-like groups, which represent structural motifs occurring in the present samples. © 2018 The Authors. Published by Wiley-VCH Verlag GmbH & Co. KGaA.

EASY SYNTHESIS OF Li4Ti5O12/C MICROSPHERES CONTAINING NANOPARTICLES AS ANODE MATERIAL FOR HIGH-RATE Li-ION BATTERIES

NASA Astrophysics Data System (ADS)

Zheng, Xiaodong; Dong, Lina; Dong, Chenchu

2014-01-01

A microspherical Li4Ti5O12/C composite composed of interconnected nanoparticles with BP-2000 carbon black as carbon source is synthesized for use as an anode material in high-power lithium-ion batteries. The composite is prepared through precursor pretreatment including pre-sintering, ball-milling, and spray-drying. The structure, size and surface morphology of the as-prepared particles are investigated by X-ray diffraction and scanning electron microscopy. Results show that the obtained material has a microspherical morphology consisting of nanosized prime particles with compact structure. The precursor pretreatment effectively reduced the agglomeration of the prime particles caused by high temperature sintering and led to a more uniform distribution of BP-2000 on the surface of prime particles generating highly efficient conductive network. The specific capacity of the electrode at 20 C rate is 131 mAh g-1 and the loss of capacity is less than 2% after the 60 variation cycles (from 1 C to 20 C and back to 1 C). This excellent performance is attributed to the effective conductive network between the prime particles and the reduction of the lithium-ion diffusion pathway.

Polyacrylonitrile/Carbon Nanotube Composite: Precursor for Next Generation Carbon Fiber

DTIC Science & Technology

2010-02-23

difficult to get the accurate time for the end of reactions. The curing process of thermosetting materials has been widely studied by investigating...Ramis X, Cadenato A, Morancho JM, Salla JM. Curing of a thermosetting powder coating by means of DMTA, TMA and DSC. Polymer. 2003;44(7):2067-79. [17...Cadenato A, Salla JM, Ramis X, Morancho JM, Marroyo LM, Martin JL. Determination of gel and vitrification times of thermoset curing process by means of

Potassium vapor assisted preparation of highly graphitized hierarchical porous carbon for high rate performance supercapacitors

NASA Astrophysics Data System (ADS)

Liu, Zheng; Zeng, Ying; Tang, Qunli; Hu, Aiping; Xiao, Kuikui; Zhang, Shiying; Deng, Weina; Fan, Binbin; Zhu, Yanfei; Chen, Xiaohua

2017-09-01

Ultrahigh graphitized carbon microspheres with rich hierarchical pores (AGHPCM-1) have been successfully synthesized through the one-step activation-carbonization strategy (OACS) with porous sulfonated poly-divinylbenzene as the carbon precursor, iron as the hard template and catalyst, and potassium hydroxide (KOH) as activation agent. Through the XRD, TEM, Raman and BET analysis, AGHPCM-1 shows very high graphitization degree and rich micro-, meso- and macro-pores. More importantly, the mechanism for KOH to improve the graphitization degree of carbon materials in OACS has been illustrated by the thermodynamical theory. The tremendous heat releasing from the reaction between the catalyst precursor of Fe2O3 and potassium vapor plays a key role in the formation of graphitized carbon. It may provide a general direction to prepare highly graphitized porous carbon at a moderate temperature. Integrating the advantages of high graphitization degree and rich hierarchical porous structure, the AGHPCM-1 exhibits an excellent rate performance with a response to up to the high current density of 150 A g-1 and high scan rate of 2000 mV s-1. No obvious capacitance decay can be observed after 10000 charge/discharge cycles even at the high current density of 20 A g-1.

Rapid feedback of chemical vapor deposition growth mechanisms by operando X-ray diffraction

DOE PAGES

Martin, Aiden A.; Depond, Philip J.; Bagge-Hansen, Michael; ...

2018-03-14

An operando x-ray diffraction system is presented for elucidating optimal laser assisted chemical vapor deposition growth conditions. The technique is utilized to investigate deposition dynamics of boron-carbon materials using trimethyl borate precursor. Trimethyl borate exhibits vastly reduced toxicological and flammability hazards compared to existing precursors, but has previously not been applied to boron carbide growth. Crystalline boron-rich carbide material is produced in a narrow growth regime on addition of hydrogen during the growth phase at high temperature. Finally, the use of the operando x-ray diffraction system allows for the exploration of highly nonequilibrium conditions and rapid process control, which aremore » not possible using ex situ diagnostics.« less

Rapid feedback of chemical vapor deposition growth mechanisms by operando X-ray diffraction

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

Martin, Aiden A.; Depond, Philip J.; Bagge-Hansen, Michael

An operando x-ray diffraction system is presented for elucidating optimal laser assisted chemical vapor deposition growth conditions. The technique is utilized to investigate deposition dynamics of boron-carbon materials using trimethyl borate precursor. Trimethyl borate exhibits vastly reduced toxicological and flammability hazards compared to existing precursors, but has previously not been applied to boron carbide growth. Crystalline boron-rich carbide material is produced in a narrow growth regime on addition of hydrogen during the growth phase at high temperature. Finally, the use of the operando x-ray diffraction system allows for the exploration of highly nonequilibrium conditions and rapid process control, which aremore » not possible using ex situ diagnostics.« less

The composite capacitive behaviors of the N and S dual doped ordered mesoporous carbon with ultrahigh doping level

NASA Astrophysics Data System (ADS)

Zhang, Deyi; Lei, Longyan; Shang, Yonghua; Wang, Kunjie; Wang, Yi

2016-01-01

Heteroatoms doping provides a promising strategy for improving the energy density of supercapacitors based on the carbon electrodes. In this paper, we present a N and S dual doped ordered mesoporous carbon with ultrahigh doping level using dimethylglyoxime as pristine precursor. The N doping content of the reported materials varies from 6.6 to 15.6 at.% dependent on the carbonization temperature, and the S doping content varies from 0.46 to 1.01 at.%. Due to the ultrahigh heteroatoms doping content, the reported materials exhibit pronounced pseudo-capacitance. Meanwhile, the reported materials exhibit high surface areas (640⿿869 m2 g⿿1), large pore volume (0.71⿿1.08 cm2 g⿿1) and ordered pore structure. The outstanding textual properties endow the reported materials excellent electrical double-layer capacitance (EDLC). By effectively combining the pseudo-capacitance with EDLC, the reported materials exhibit a surprising energy storage/relax capacity with the highest specific capacitance of 565 F g⿿1, which value is 3.3 times higher than that of pristine CMK-3, and can compete against some conventional pseudo-capacitance materials.

Catalytic Graphitization for Preparation of Porous Carbon Material Derived from Bamboo Precursor and Performance as Electrode of Electrical Double-Layer Capacitor

NASA Astrophysics Data System (ADS)

Tsubota, Toshiki; Maguchi, Yuta; Kamimura, Sunao; Ohno, Teruhisa; Yasuoka, Takehiro; Nishida, Haruo

2015-12-01

The combination of addition of Fe (as a catalyst for graphitization) and CO2 activation (a kind of gaseous activation) was applied to prepare a porous carbon material from bamboo powder (a waste product of superheated steam treatment). Regardless of the heat treatment temperature, many macropores were successfully formed after the heating process by removal of Fe compounds. A turbostratic carbon structure was generated in the Fe-added sample heated at 850°C. It was confirmed that the added Fe acted as a template for pore formation. Moreover, it was confirmed that the added Fe acted as a catalyst for graphitization. The resulting electrochemical performance as the electrode of an electrical double-layer capacitor, as demonstrated by cyclic voltammetry, electrochemical impedance spectroscopy, and charge-discharge testing, could be explained based on the graphitization and activation effects. Addition of Fe could affect the electrical properties of carbon material derived from bamboo.

Nitrogen-doped carbon nanofibers derived from polypyrrole coated bacterial cellulose as high-performance electrode materials for supercapacitors and Li-ion batteries

DOE PAGES

Lei, Wen; Han, Lili; Xuan, Cuijuan; ...

2016-05-24

Here, nitrogen-doped carbon nanofiber (NDCN) was synthesized via carbonization of polypyrrole (PPy) coated bacterial cellulose (BC) composites, where BC serves as templates as well as precursor, and PPy serves as the nitrogen source. The synthesized NDCN was employed as electrode for both supercapacitors and Li-ion batteries. The large surface area exposed to electrolyte resulting from the 3D carbon networks leads to sufficient electrode/electrolyte interface and creates shorter transport paths of electrolyte ions and Li + ion. Besides, the three types of N dopants in NDCN improve the electronic conductivity, as well as superior electrochemical performance.

Origin and sources of dissolved organic matter in snow on the East Antarctic ice sheet.

PubMed

Antony, Runa; Grannas, Amanda M; Willoughby, Amanda S; Sleighter, Rachel L; Thamban, Meloth; Hatcher, Patrick G

2014-06-03

Polar ice sheets hold a significant pool of the world's carbon reserve and are an integral component of the global carbon cycle. Yet, organic carbon composition and cycling in these systems is least understood. Here, we use ultrahigh resolution mass spectrometry to elucidate, at an unprecedented level, molecular details of dissolved organic matter (DOM) in Antarctic snow. Tens of thousands of distinct molecular species are identified, providing clues to the nature and sources of organic carbon in Antarctica. We show that many of the identified supraglacial organic matter formulas are consistent with material from microbial sources, and terrestrial inputs of vascular plant-derived materials are likely more important sources of organic carbon to Antarctica than previously thought. Black carbon-like material apparently originating from biomass burning in South America is also present, while a smaller fraction originated from soil humics and appears to be photochemically or microbially modified. In addition to remote continental sources, we document signals of oceanic emissions of primary aerosols and secondary organic aerosol precursors. The new insights on the diversity of organic species in Antarctic snowpack reinforce the importance of studying organic carbon associated with the Earth's polar regions in the face of changing climate.

Structure-property relationships of a biological mesocrystal in the adult sea urchin spine

PubMed Central

Seto, Jong; Ma, Yurong; Davis, Sean A.; Meldrum, Fiona; Gourrier, Aurelien; Kim, Yi-Yeoun; Schilde, Uwe; Sztucki, Michael; Burghammer, Manfred; Maltsev, Sergey; Jäger, Christian; Cölfen, Helmut

2012-01-01

Structuring over many length scales is a design strategy widely used in Nature to create materials with unique functional properties. We here present a comprehensive analysis of an adult sea urchin spine, and in revealing a complex, hierarchical structure, show how Nature fabricates a material which diffracts as a single crystal of calcite and yet fractures as a glassy material. Each spine comprises a highly oriented array of Mg-calcite nanocrystals in which amorphous regions and macromolecules are embedded. It is postulated that this mesocrystalline structure forms via the crystallization of a dense array of amorphous calcium carbonate (ACC) precursor particles. A residual surface layer of ACC and/or macromolecules remains around the nanoparticle units which creates the mesocrystal structure and contributes to the conchoidal fracture behavior. Nature’s demonstration of how crystallization of an amorphous precursor phase can create a crystalline material with remarkable properties therefore provides inspiration for a novel approach to the design and synthesis of synthetic composite materials. PMID:22343283

Structure-property relationships of a biological mesocrystal in the adult sea urchin spine.

PubMed

Seto, Jong; Ma, Yurong; Davis, Sean A; Meldrum, Fiona; Gourrier, Aurelien; Kim, Yi-Yeoun; Schilde, Uwe; Sztucki, Michael; Burghammer, Manfred; Maltsev, Sergey; Jäger, Christian; Cölfen, Helmut

2012-03-06

Structuring over many length scales is a design strategy widely used in Nature to create materials with unique functional properties. We here present a comprehensive analysis of an adult sea urchin spine, and in revealing a complex, hierarchical structure, show how Nature fabricates a material which diffracts as a single crystal of calcite and yet fractures as a glassy material. Each spine comprises a highly oriented array of Mg-calcite nanocrystals in which amorphous regions and macromolecules are embedded. It is postulated that this mesocrystalline structure forms via the crystallization of a dense array of amorphous calcium carbonate (ACC) precursor particles. A residual surface layer of ACC and/or macromolecules remains around the nanoparticle units which creates the mesocrystal structure and contributes to the conchoidal fracture behavior. Nature's demonstration of how crystallization of an amorphous precursor phase can create a crystalline material with remarkable properties therefore provides inspiration for a novel approach to the design and synthesis of synthetic composite materials.

"Bricks and mortar" self-assembly approach to graphitic mesoporous carbon nanocomposites

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

Fulvio, P. F.; Mayes, R.; Wang, X. Q.

2011-04-20

Mesoporous carbon materials do not have sufficient ordering at the atomic scale to exhibit good electronic conductivity. To date, mesoporous carbons having uniform mesopores and high surface areas have been prepared from partially-graphitizable precursors in the presence of templates. High temperature thermal treatments above 2000 °C, which are usually required to increase conductivity, result in a partial or total collapse of the mesoporous structures and reduced surface areas induced by growth of graphitic domains, limiting their applications in electric double layer capacitors and lithium-ion batteries. In this work, we successfully implemented a “brick-and-mortar” approach to obtain ordered graphitic mesoporous carbonmore » nanocomposites with tunable mesopore sizes below 850 °C without using graphitization catalysts or high temperature thermal treatments. Phenolic resin-based mesoporous carbons act as mortar to highly conductive carbon blacks and carbon onions (bricks). The capacitance and resistivity of final materials can be tailored by changing the mortar to brick ratios.« less

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.

Liquefaction of oak tree bark with different biomass/phenol mass ratios and utilizing bio-based polyols for carbon foam production

NASA Astrophysics Data System (ADS)

Ozbay, N.; Yargic, A. S.

2017-02-01

Carbon foam is sponge like carbonaceous material with low density, high conductivity and high strength; which is used in various applications such as catalyst supports, membrane separations, high thermally conductive heat sinks, energy absorption materials, high temperature thermal insulation. Coal or fossil oils are conventionally used to fabricate pitch, phenolic resin and polyurethane as carbon foam precursor. Biomass liquefaction is a developing technique to convert biomass resources into the industrial chemicals. In this study, oak tree bark was liquefied under mild conditions with different mass ratio of biomass/phenol; and the liquefaction product was used as polyol to produce porous resin foams. Obtained resin foams were carbonized at 400 °C, and then activated at 800 °C under nitrogen atmosphere. Structure evaluation of resin foams, carbonized foams and activated carbon foams from liquefied oak tree bark was investigated by using elemental analysis, x-ray diffraction, nitrogen adsorption/desorption isotherms, scanning electron microscopy, bulk density and compressive strength tests.

Brick-and-Mortar Self-Assembly Approach to Graphitic Mesoporous Carbon Nanocomposites

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

Dai, Sheng; Fulvio, Pasquale F; Mayes, Richard T

2011-01-01

Mesoporous carbon materials do not have sufficient ordering at the atomic scale to exhibit good electronic conductivity. To date, mesoporous carbons having uniform mesopores and high surface areas have been prepared from partially-graphitizable precursors in the presence of templates. High temperature thermal treatments above 2000 C, which are usually required to increase conductivity, result in a partial or total collapse of the mesoporous structures and reduced surface areas induced by growth of graphitic domains, limiting their applications in electric double layer capacitors and lithium-ion batteries. In this work, we successfully implemented a 'brick-and-mortar' approach to obtain ordered graphitic mesoporous carbonmore » nanocomposites with tunable mesopore sizes below 850 C without using graphitization catalysts or high temperature thermal treatments. Phenolic resin-based mesoporous carbons act as mortar to highly conductive carbon blacks and carbon onions (bricks). The capacitance and resistivity of final materials can be tailored by changing the mortar to brick ratios.« less

Polymeric routes to silicon carbide and silicon oxycarbide CMC

NASA Technical Reports Server (NTRS)

Hurwitz, Frances I.; Heimann, Paul J.; Gyekenyesi, John Z.; Masnovi, John; Bu, Xin YA

1991-01-01

An overview of two approaches to the formation of ceramic composite matrices from polymeric precursors is presented. Copolymerization of alkyl- and alkenylsilanes (RSiH3) represents a new precursor system for the production of Beta-SiC on pyrolysis, with copolymer composition controlling polymer structure, char yield, and ceramic stoichiometry and morphology. Polysilsesquioxanes which are synthesized readily and can be handled in air serve as precursors to Si-C-O ceramics. Copolymers of phenyl and methyl silsesquioxanes display rheological properties favorable for composite fabrication; these can be tailored by control of pH, water/methoxy ratio and copolymer composition. Composites obtained from these utilize a carbon coated, eight harness satin weave Nicalon cloth reinforcement. The material exhibits nonlinear stress-strain behavior in tension.

Carbon-Encapsulated Co3O4 Nanoparticles as Anode Materials with Super Lithium Storage Performance

NASA Astrophysics Data System (ADS)

Leng, Xuning; Wei, Sufeng; Jiang, Zhonghao; Lian, Jianshe; Wang, Guoyong; Jiang, Qing

2015-11-01

A high-performance anode material for lithium storage was successfully synthesized by glucose as carbon source and cobalt nitrate as Co3O4 precursor with the assistance of sodium chloride surface as a template to reduce the carbon sheet thickness. Ultrafine Co3O4 nanoparticles were homogeneously embedded in ultrathin porous graphitic carbon in this material. The carbon sheets, which have large specific surface area, high electronic conductivity, and outstanding mechanical flexibility, are very effective to keep the stability of Co3O4 nanoparticales which has a large capacity. As a consequence, a very high reversible capacity of up to 1413 mA h g-1 at a current density of 0.1 A g-1 after 100 cycles, a high rate capability (845, 560, 461 and 345 mA h g-1 at 5, 10, 15 and 20 C, respectively, 1 C = 1 A g-1), and a superior cycling performance at an ultrahigh rate (760 mA h g-1 at 5 C after 1000 cycles) are achieved by this lithium-ion-battery anode material.

A Nanopore-Structured Nitrogen-Doped Biocarbon Electrocatalyst for Oxygen Reduction from Two-Step Carbonization of Lemna minor Biomass.

PubMed

Guo, Chaozhong; Li, Zhongbin; Niu, Lidan; Liao, Wenli; Sun, Lingtao; Wen, Bixia; Nie, Yunqing; Cheng, Jing; Chen, Changguo

2016-12-01

So far, the development of highly active and stable carbon-based electrocatalysts for oxygen reduction reaction (ORR) to replace commercial Pt/C catalyst is a hot topic. In this study, a new nanoporous nitrogen-doped carbon material was facilely designed by two-step pyrolysis of the renewable Lemna minor enriched in crude protein under a nitrogen atmosphere. Electrochemical measurements show that the onset potential for ORR on this carbon material is around 0.93 V (versus reversible hydrogen electrode), slightly lower than that on the Pt/C catalyst, but its cycling stability is higher compared to the Pt/C catalyst in an alkaline medium. Besides, the ORR at this catalyst approaches to a four-electron transfer pathway. The obtained ORR performance can be basically attributed to the formation of high contents of pyridinic and graphitic nitrogen atoms inside this catalyst. Thus, this work opens up the path in the ORR catalysis for the design of nitrogen-doped carbon materials utilizing aquatic plants as starting precursors.

Comparison of unusual carbon-based working electrodes for electrochemiluminescence sensors.

PubMed

Noman, Muhammad; Sanginario, Alessandro; Jagadale, Pravin; Demarchi, Danilo; Tagliaferro, Alberto

2017-06-01

In this work, unconventional carbon-based materials were investigated for use in electrochemiluminescence (ECL) working electrodes. Precursors such as bamboo, pistachio shells, kevlar ® fibers and camphor were differently treated and used as working electrodes in ECL experiments. After a proper process they were assembled as electrodes and tested in an electrochemical cell. Comparison among them and with a commercial glassy carbon electrode (GCE) shows a very good response for all of them thus demonstrating their potential use as disposable low-cost electrodes for early detection electrochemical analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

Methanesulfonic acid-assisted synthesis of N/S co-doped hierarchically porous carbon for high performance supercapacitors

NASA Astrophysics Data System (ADS)

Huo, Silu; Liu, Mingquan; Wu, Linlin; Liu, Mingjie; Xu, Min; Ni, Wei; Yan, Yi-Ming

2018-05-01

Nitrogen and sulfur co-doped carbons are considered as electrode materials for high performance supercapacitors, while their further development is still limited by complicated synthesis procedure, unsatisfied structure and low energy density. Developing a simple synthetic strategy to obtain rationally structured carbon materials and high supercapacitor performance is remaining a grand challenge. Herein, we describe the synthesis of nitrogen and sulfur co-doped hierarchical porous carbons as high performance supercapacitors electrode by a methanesulfonic acid-assisted one-step carbonization and activation of the freeze-dried precursors mixture. The as-prepared carbon material not only exhibits ideally hierarchical pores, but also realizes uniform nitrogen and sulfur co-doping. In 6.0 M KOH electrolyte, the material can achieve a high specific capacitance of 272 F g-1 at 1.0 A g-1 and a promising rate performance retaining 172 F g-1 even at 100 A g-1. Moreover, a fabricated symmetric supercapacitor based on as-prepared nitrogen and sulfur co-doped hierarchical porous carbon delivers high energy densities of 12.4 W h kg-1 and 8.0 W h kg-1 in 6.0 M KOH liquid and KOH/PVA solid-state electrolytes, respectively. This work presents a simple and effective methanesulfonic acid-assisted approach for mass production of heteroatomic doping hierarchical porous carbons for future energy storage applications.

PAF-derived nitrogen-doped 3D Carbon Materials for Efficient Energy Conversion and Storage.

PubMed

Xiang, Zhonghua; Wang, Dan; Xue, Yuhua; Dai, Liming; Chen, Jian-Feng; Cao, Dapeng

2015-06-05

Owing to the shortage of the traditional fossil fuels caused by fast consumption, it is an urgent task to develop the renewable and clean energy sources. Thus, advanced technologies for both energy conversion (e.g., solar cells and fuel cells) and storage (e.g., supercapacitors and batteries) are being studied extensively. In this work, we use porous aromatic framework (PAF) as precursor to produce nitrogen-doped 3D carbon materials, i.e., N-PAF-Carbon, by exposing NH3 media. The "graphitic" and "pyridinic" N species, large surface area, and similar pore size as electrolyte ions endow the nitrogen-doped PAF-Carbon with outstanding electronic performance. Our results suggest the N-doping enhance not only the ORR electronic catalysis but also the supercapacitive performance. Actually, the N-PAF-Carbon obtains ~70 mV half-wave potential enhancement and 80% increase as to the limiting current after N doping. Moreover, the N-PAF-Carbon displays free from the CO and methanol crossover effect and better long-term durability compared with the commercial Pt/C benchmark. Moreover, N-PAF-Carbon also possesses large capacitance (385 F g(-1)) and excellent performance stability without any loss in capacitance after 9000 charge-discharge cycles. These results clearly suggest that PAF-derived N-doped carbon material is promising metal-free ORR catalyst for fuel cells and capacitor electrode materials.

Structural insights into photocatalytic performance of carbon nitrides for degradation of organic pollutants

NASA Astrophysics Data System (ADS)

Oh, Junghoon; Shim, Yeonjun; Lee, Soomin; Park, Sunghee; Jang, Dawoon; Shin, Yunseok; Ohn, Saerom; Kim, Jeongho; Park, Sungjin

2018-02-01

Degradation of organic pollutants has a large environmental impact, with graphitic carbon nitride (g-C3N4) being a promising metal-free, low cost, and environment-friendly photocatalyst well suited for this purpose. Herein, we investigate the photocatalytic performance of g-C3N4-based materials and correlate it with their structural properties, using three different precursors (dicyandiamide, melamine, and urea) and two heating processes (direct heating at 550 °C and sequential heating at 300 and 550 °C) to produce the above photocatalysts. We further demonstrate that sequential heating produces photocatalysts with grain sizes and activities larger than those of the catalysts produced by direct heating and that the use of urea as a precursor affords photocatalysts with larger surface areas, allowing efficient rhodamine B degradation under visible light.

Major structural components in freshwater dissolved organic matter.

PubMed

Lam, Buuan; Baer, Andrew; Alaee, Mehran; Lefebvre, Brent; Moser, Arvin; Williams, Antony; Simpson, André J

2007-12-15

Dissolved organic matter (DOM) contains a complex array of chemical components that are intimately linked to many environmental processes, including the global carbon cycle, and the fate and transport of chemical pollutants. Despite its importance, fundamental aspects, such as the structural components in DOM remain elusive, due in part to the molecular complexity of the material. Here, we utilize multidimensional nuclear magnetic resonance spectroscopy to demonstrate the major structural components in Lake Ontario DOM. These include carboxyl-rich alicyclic molecules (CRAM), heteropolysaccharides, and aromatic compounds, which are consistent with components recently identified in marine dissolved organic matter. In addition, long-range proton-carbon correlations are obtained for DOM, which support the existence of material derived from linear terpenoids (MDLT). It is tentatively suggested that the bulk of freshwater dissolved organic matter is aliphatic in nature, with CRAM derived from cyclic terpenoids, and MDLT derived from linear terpenoids. This is in agreement with previous reports which indicate terpenoids as major precursors of DOM. At this time it is not clear in Lake Ontario whether these precursors are of terrestrial or aquatic origin or whether transformations proceed via biological and/ or photochemical processes.

Synthesis of nanostructured iron oxides dispersed in carbon materials and in situ XRD study of the changes caused by thermal treatment

NASA Astrophysics Data System (ADS)

Gonçalves, Gustavo R.; Schettino, Miguel A.; Morigaki, Milton K.; Nunes, Evaristo; Cunha, Alfredo G.; Emmerich, Francisco G.; Passamani, Edson C.; Baggio-Saitovitch, Elisa; Freitas, Jair C. C.

2015-07-01

Carbon-based magnetic nanocomposites are of large interest for applications in catalysis, magnetic separation, water cleaning, and magnetic resonance imaging, among others. This work describes the synthesis of nanocomposites consisting of iron oxides dispersed into a char (obtained from the carbonization at 700 °C of a lignocellulosic precursor) and the study of the thermal transformations occurring in these materials as a consequence of heat treatments. The materials were prepared by impregnation of the char with iron nitrate in the presence of ammonium hydroxide in aqueous suspension. X-ray diffraction experiments performed using synchrotron radiation and Mössbauer spectroscopy showed that the as-prepared material was composed of amorphous Fe3+ oxides. Scanning electron microscopy images combined with energy-dispersive X-ray spectrometry indicated a homogeneous dispersion of iron oxides and of silica particles (naturally present in the lignocellulosic precursor) throughout the char. X-ray diffractograms recorded in situ during the heat treatment of the as-prepared material showed the presence of small hematite crystallites (average size 22 nm) starting from ca. 300 °C. Further heating caused a progressive growth of the hematite crystallites up to ca. 500 °C, when the conversion to magnetite (Fe3O4) started to take place. At higher temperatures, wüstite (Fe1-xO) was detected as an intermediate phase and austenitic iron (γ-Fe) became the dominant phase at temperatures from 900 °C. A steep weight loss was observed in the TG curve accompanying this last reduction stage; upon cooling, γ-Fe was converted into α-Fe (ferrite), which was the dominant phase at room temperature in this heat-treated sample.

Assembling a supercapacitor electrode with dual metal oxides and activated carbon using a liquid phase plasma.

PubMed

Ki, Seo Jin; Jeon, Ki-Joon; Park, Young-Kwon; Park, Hyunwoong; Jeong, Sangmin; Lee, Heon; Jung, Sang-Chul

2017-12-01

Developing supercapacitor electrodes at an affordable cost while improving their energy and/or power density values is still a challenging task. This study introduced a recipe which assembled a novel electrode composite using a liquid phase plasma that was applied to a reactant solution containing an activated carbon (AC) powder with dual metal precursors of iron and manganese. A comparison was made between the composites doped with single and dual metal components as well as among those synthesized under different precursor concentrations and plasma durations. The results showed that increasing the precursor concentration and plasma duration raised the content of both metal oxides in the composites, whereas the deposition conditions were more favorable to iron oxide than manganese oxide, due to its higher standard potential. The composite treated with the longest plasma duration and highest manganese concentration was superior to the others in terms of cyclic stability and equivalent series resistance. In addition, the new composite selected out of them showed better electrochemical performance than the raw AC material only and even two types of single metal-based composites, owing largely to the synergistic effect of the two metal oxides. Therefore, the proposed methodology can be used to modify existing and future composite electrodes to improve their performance with relatively cheap host and guest materials. Copyright © 2017 Elsevier Ltd. All rights reserved.

Template synthesis of hollow MoS2-carbon nanocomposites using microporous organic polymers and their lithium storage properties.

PubMed

Jin, Jaewon; Kim, Bolyong; Kim, Mincheol; Park, Nojin; Kang, Sungah; Lee, Sang Moon; Kim, Hae Jin; Son, Seung Uk

2015-07-14

This work shows that hollow and microporous organic polymers (H-MOPs) are good templating materials for the synthesis of inorganic material-carbon nanocomposites. The precursor compound, (NH4)2MoS4, was incorporated into H-MOPs. Heat treatment under argon resulted in the formation of hollow MoS2-carbon nanocomposites (MSC). According to microscopic analysis, the MoS2 in the MSC has a layered structure with an elongated interlayer distance. The MSC showed high reversible discharge capacities up to 802 mA h g(-1) after 30 cycles and excellent rate performance for lithium ion batteries. The promising electrochemical performance of the MSC is attributed to the very thin and disordered nature of MoS2 in the carbon skeleton. The role of chemical components of the MSC in the electrochemical process was suggested.

Conversion of agricultural residues into activated carbons for water purification: Application to arsenate removal.

PubMed

Torres-Perez, Jonatan; Gerente, Claire; Andres, Yves

2012-01-01

The conversion of two agricultural wastes, sugar beet pulp and peanut hulls, into sustainable activated carbons is presented and their potential application for the treatment of arsenate solution is investigated. A direct and physical activation is selected as well as a simple chemical treatment of the adsorbents. The material properties, such as BET surface areas, porous volumes, elemental analysis, ash contents and pH(PZC), of these alternative carbonaceous porous materials are determined and compared with a commercial granular activated carbon. An adsorption study based on experimental kinetic and equilibrium data is conducted in a batch reactor and completed by the use of different models (intraparticle diffusion, pseudo-second-order, Langmuir and Freundlich) and by isotherms carried out in natural waters. It is thus demonstrated that sugar beet pulp and peanut hulls are good precursors to obtain activated carbons for arsenate removal.

Nanoscale Transforming Mineral Phases in Fresh Nacre.

PubMed

DeVol, Ross T; Sun, Chang-Yu; Marcus, Matthew A; Coppersmith, Susan N; Myneni, Satish C B; Gilbert, Pupa U P A

2015-10-21

Nacre, or mother-of-pearl, the iridescent inner layer of many mollusk shells, is a biomineral lamellar composite of aragonite (CaCO3) and organic sheets. Biomineralization frequently occurs via transient amorphous precursor phases, crystallizing into the final stable biomineral. In nacre, despite extensive attempts, amorphous calcium carbonate (ACC) precursors have remained elusive. They were inferred from non-nacre-forming larval shells, or from a residue of amorphous material surrounding mature gastropod nacre tablets, and have only once been observed in bivalve nacre. Here we present the first direct observation of ACC precursors to nacre formation, obtained from the growth front of nacre in gastropod shells from red abalone (Haliotis rufescens), using synchrotron spectromicroscopy. Surprisingly, the abalone nacre data show the same ACC phases that are precursors to calcite (CaCO3) formation in sea urchin spicules, and not proto-aragonite or poorly crystalline aragonite (pAra), as expected for aragonitic nacre. In contrast, we find pAra in coral.

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

DeVol, Ross T.; Sun, Chang-Yu; Marcus, Matthew A.

Nacre, or mother-of-pearl, the iridescent inner layer of many mollusk shells, is a biomineral lamellar composite of aragonite (CaCO 3) and organic sheets. Biomineralization frequently occurs via transient amorphous precursor phases, crystallizing into the final stable biomineral. In nacre, despite extensive attempts, amorphous calcium carbonate (ACC) precursors have remained elusive. They were inferred from non-nacre-forming larval shells, or from a residue of amorphous material surrounding mature gastropod nacre tablets, and have only once been observed in bivalve nacre. Here we present the first direct observation of ACC precursors to nacre formation, obtained from the growth front of nacre in gastropodmore » shells from red abalone (Haliotis rufescens), using synchrotron spectromicroscopy. Surprisingly, the abalone nacre data show the same ACC phases that are precursors to calcite (CaCO 3) formation in sea urchin spicules, and not proto-aragonite or poorly crystalline aragonite (pAra), as expected for aragonitic nacre. In contrast, we find pAra in coral.« less

Poly(diiododiacetylene): A Potential Precursor for New All-Carbon Materials

NASA Astrophysics Data System (ADS)

Resch, Daniel Joseph

Poly(diiododiacetylene) (PIDA) is a polymer consisting entirely of carbon and iodine. The polymer is prepared by cocrystallizing a bis(nitrile) oxalamide host with the monomer diiodobutadiyne. These compounds are held together by a halogen bond and an ordered 1,4-topochemical polymerization occurs in the solid state. The formation of the monomer cocrystals was found to be highly solvent dependent. Acetonitrile was found to greatly improve the yield of cocrystals over solvents used in the past. Cocrystals could not be obtained from other solvents such as dimethoxyethane and acetone. THF did give some cocrystal but the yield was poor. The use of acetonitrile as a solvent now allows for PIDA cocrystals to be reliably prepared in excellent yield for detailed studies. The weak C-I bonds in PIDA can be broken under mild conditions with simple Lewis bases like pyrrolidine and iodide ion. Studies with small molecule models show that the mechanism of elimination is E2-like and highly solvent dependent. Polar aprotic solvents favor the reaction while non-polar solvents disfavor it. Reaction occurs in protic solvents, but the rate is much slower. Iodide was found to carry out the reaction in 1 hour d5-PhNO 2 while reaction with pyrrolidine did not reach completion in 15 hours. When PIDA is subjected to deiodination the product is an amorphous graphite-like material that contains non-carbon atoms. Depending on the reaction conditions, it is possible to incorporate sulfur or phosphorus into the final product. The source of these elements is the reducing agent that is typically added to sequester molecular iodine. Sequestering the iodine prevents it from reacting with the carbon species. New insights into the deiodination reaction have made PIDA more promising as a precursor to prepare all-carbon materials or heteroatom-functionalized carbon under mild conditions.

QCM gas phase detection with ceramic materials--VOCs and oil vapors.

PubMed

Latif, Usman; Rohrer, Andreas; Lieberzeit, Peter A; Dickert, Franz L

2011-06-01

Titanate sol-gel layers imprinted with carbonic acids were used as sensitive layers on quartz crystal microbalance. These functionalized ceramics enable us detection of volatile organic compounds such as ethanol, n-propanol, n-butanol, n-hexane, n-heptane, n-/iso-octane, and n-decane. Variation of the precursors (i.e., tetrabutoxy titanium, tetrapropoxy titanium, tetraethoxy titanium) allows us to tune the sensitivity of the material by a factor of 7. Sensitivity as a function of precursors leads to selective inclusion of n-butanol vapors down to 1 ppm. The selectivity of materials is optimized to differentiate between isomers, e.g., n- and iso-octane. The results can be rationalized by correlating the sensor effects of hydrocarbons with the Wiener index. A mass-sensitive sensor based on titanate layer was also developed for monitoring emanation of degraded engine oil. Heating the sensor by a meander avoids vapor condensation. Thus, a continuously working oil quality sensor was designed.

Nanostructured nonprecious metal catalysts for oxygen reduction reaction.

PubMed

Wu, Gang; Zelenay, Piotr

2013-08-20

Platinum-based catalysts represent a state of the art in the electrocatalysis of oxygen reduction reaction (ORR) from the point of view of their activity and durability in harnessing the chemical energy via direct electrochemical conversion. However, because platinum is both expensive and scarce, its widespread implementation in such clean energy applications is limited. Recent breakthroughs in the synthesis of high-performance nonprecious metal catalysts (NPMCs) make replacement of Pt in ORR electrocatalysts with earth-abundant elements, such as Fe, Co, N, and C, a realistic possibility. In this Account, we discuss how we can obtain highly promising M-N-C (M: Fe and/or Co) catalysts by simultaneously heat-treating precursors of nitrogen, carbon, and transition metals at 800-1000 °C. The activity and durability of resulting catalysts depend greatly on the selection of precursors and synthesis chemistry. In addition, they correlate quite well with the catalyst nanostructure. While chemists have presented no conclusive description of the active catalytic site for this class of NPMCs, they have developed a designed approach to making active and durable materials, focusing on the catalyst nanostructure. The approach consists of nitrogen doping, in situ carbon graphitization, and the usage of graphitic structures (possibly graphene and graphene oxides) as carbon precursors. Various forms of nitrogen, particularly pyridinic and quaternary, can act as n-type carbon dopants in the M-N-C catalysts, assisting in the formation of disordered carbon nanostructures and donating electrons to the carbon. The CNx structures are likely a crucial part of the ORR active site(s). Noteworthy, the ORR activity is not necessarily governed by the amount of nitrogen, but by how the nitrogen is incorporated into the nanostructures. Apart from the possibility of a direct participation in the active site, the transition metal often plays an important role in the in situ formation of various carbon nanostructures by catalyzing the decomposition of the nitrogen/carbon precursor. We can control the formation of different nanostructures during the synthesis of M-N-C catalysts. For example, in situ formed nitrogen-doped graphene-sheets can only be derived from polyaniline (PANI), probably due to structural similarities between the aromatic structures of PANI and graphene. Highly-graphitized carbon nanostructures may serve as a matrix for the formation of ORR-active groups with improved catalytic activity and durability, containing nitrogen and most probably also metal atoms. In the future, we will likely focus NPMC synthesis approaches on precise control of interactions between precursors of the metal and carbon/nitrogen during the heat treatment. The main purposes will be to maximize the number of active sites, optimize nitrogen doping levels, and generate morphologies capable of hosting active and stable ORR sites.

Deposition of Ni nanoparticles onto porous supports using supercritical CO2: effect of the precursor and reduction methodology.

PubMed

Morère, Jacobo; Royuela, Sergio; Asensio, Guillermo; Palomino, Pablo; Enciso, Eduardo; Pando, Concepción; Cabañas, Albertina

2015-12-28

The deposition of Ni nanoparticles into porous supports is very important in catalysis. In this paper, we explore the use of supercritical CO(2) (scCO(2)) as a green solvent to deposit Ni nanoparticles on mesoporous SiO2 SBA-15 and a carbon xerogel. The good transport properties of scCO(2) allowed the efficient penetration of metal precursors dissolved in scCO(2) within the pores of the support without damaging its structure. Nickel hexafluoroacetylacetonate hydrate, nickel acetylacetonate, bis(cyclopentadienyl)nickel, Ni(NO(3))2⋅6H(2)O and NiCl(2)⋅6H(2)O were tried as precursors. Different methodologies were used: impregnation in scCO(2) and reduction in H(2)/N(2) at 400°C and low pressure, reactive deposition using H(2) at 200-250°C in scCO(2) and reactive deposition using ethanol at 150-200°C in scCO(2). The effect of precursor and methodology on the nickel particle size and the material homogeneity (on the different substrates) was analysed. This technology offers many opportunities in the preparation of metal-nanostructured materials. © 2015 The Author(s).

Synthesis and Characterization of Some Alkaline-Earth-Oxide Nanoparticles

NASA Astrophysics Data System (ADS)

Singh, Jitendra Pal; Lim, Weon Cheol; Won, Sung Ok; Song, Jonghan; Chae, Keun Hwa

2018-04-01

The present work reports the synthesis of MgO and CaO nanoparticles by using the sol-gel autocombustion method. The annealing of the precursor at 1200 °C was observed to lead the formation of MgO nanoparticles having average crystallite size of 31 nm. Annealing the precursor at same temperature produced materials having a CaO phase with a minor impure phase of calcium carbonate ( 3%). The crystallite size corresponding to the CaO phase was 38 nm. A change of thermal history in the precursor was observed not to result in an improvement of the CaO phase. The change of thermal history in the precursor gave rise to mixed phases of CaCO3 and Ca(OH)2 rather than the phase of CaO. Further, annealing at 1200 °C for 12 h resulted in the formation of the CaO phase along with almost 1 - 5% of calcium hydroxide as an impurity phase. X-ray absorption spectroscopic measurements carried out on these materials revealed that the local electronic/atomic structure of these oxides was not only affected by the impurity phases but also influenced by the carbaneous impurities attached to the crystallites.

Method for synthesizing carbon nanotubes

DOEpatents

Fan, Hongyou

2012-09-04

A method for preparing a precursor solution for synthesis of carbon nanomaterials, where a polar solvent is added to at least one block copolymer and at least one carbohydrate compound, and the precursor solution is processed using a self-assembly process and subsequent heating to form nanoporous carbon films, porous carbon nanotubes, and porous carbon nanoparticles.

Graphitic carbon stabilized silver nanoparticles synthesized by a simple chemical precursor method

NASA Astrophysics Data System (ADS)

Soni, Bhasker; Biswas, Somnath

2018-04-01

Monodispersed graphitic carbon stabilized silver nanoparticles (AgNPs) were synthesized following a simple chemical precursor method. The precursor was obtained by a controlled reduction of Ag+ in aqueous solution of poly-vinyl alcohol (PVA) and sucrose. The process allows precise control over the morphology of the AgNPs along with in situ formation of a surface stabilization layer of graphitic carbon.

Superior performance of nanoscaled Fe3O4 as anode material promoted by mosaicking into porous carbon framework

NASA Astrophysics Data System (ADS)

Wan, Wang; Wang, Chao; Zhang, Weidong; Chen, Jitao; Zhou, Henghui; Zhang, Xinxiang

2014-01-01

A nanoscale Fe3O4/porous carbon-multiwalled carbon nanotubes (MWCNTs) composite is synthesized through a simple hard-template method by using Fe2O3 nanoparticles as the precursor and SiO2 nanoparticles as the template. The composite shows good cycle performance (941 mAh g-1 for the first cycle at 0.1 C, with 106% capacity retention at the 80th cycle) and high rate capability (71% capacity retained at 5 C rate). Its excellent electrical properties can be attributed to the porous carbon framework structure, which is composed of carbon and MWCNTs. In this composite, the porous structure provides space for the change in Fe3O4 volume during cycling and shortens the lithium ion diffusion distance, the MWCNTs increase the electron conductivity, and the carbon coating reduces the risk of side reactions. The results provide clear evidences for the utility of porous carbon framework to improve the electrochemical performances of nanosized transition-metal oxides as anode materials for lithium-ion batteries.

Infiltrating sulfur into a highly porous carbon sphere as cathode material for lithium–sulfur batteries

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

Zhao, Xiaohui; Kim, Dul-Sun; Ahn, Hyo-Jun

2014-10-15

Highlights: • A highly porous carbon (HPC) with regular spherical morphology was synthesized. • Sulfur/HPC composites were prepared by melt–diffusion method. • Sulfur/HPC composites showed improved cyclablity and long-term cycle life. - Abstract: Sulfur composite material with a highly porous carbon sphere as the conducting container was prepared. The highly porous carbon sphere was easily synthesized with resorcinol–formaldehyde precursor as the carbon source. The morphology of the carbon was observed with field emission scanning electron microscope and transmission electron microscope, which showed a well-defined spherical shape. Brunauer–Emmett–Teller analysis indicated that it possesses a high specific surface area of 1563 m{supmore » 2} g{sup −1} and a total pore volume of 2.66 cm{sup 3} g{sup −1} with a bimodal pore size distribution, which allow high sulfur loading and easy transportation of lithium ions. Sulfur carbon composites with varied sulfur contents were prepared by melt–diffusion method and lithium sulfur cells with the sulfur composites showed improved cyclablity and long-term cycle life.« less

De-agglomeration and homogenisation of nanoparticles in coal tar pitch-based carbon materials

NASA Astrophysics Data System (ADS)

Gubernat, Maciej; Tomala, Janusz; Frohs, Wilhelm; Fraczek-Szczypta, Aneta; Blazewicz, Stanislaw

2016-03-01

The aim of the work was to characterise coal tar pitch (CTP) modified with selected nanoparticles as a binder precursor for the manufacture of synthetic carbon materials. Different factors influencing the preliminary preparative steps in the preparation of homogenous nanoparticle/CTP composition were studied. Graphene flakes, carbon black and nano-sized silicon carbide were used to modify CTP. Prior to introducing them into liquid CTP, nanoparticles were subjected to sonication. Various dispersants were used to prepare the suspensions, i.e. water, ethanol, dimethylformamide (DMF) and N-methylpyrrolidone (NMP).The results showed that proper dispersant selection is one of the most important factors influencing the de-agglomeration process of nanoparticles. DMF and NMP were found to be effective dispersants for the preparation of homogenous nanoparticle-containing suspensions. The presence of SiC and carbon black nanoparticles in the liquid pitch during heat treatment up to 2000 °C leads to the inhibition of crystallite growth in carbon residue.

A highly resilient mesoporous SiOx lithium storage material engineered by oil-water templating.

PubMed

Park, Eunjun; Park, Min-Sik; Lee, Jaewoo; Kim, Ki Jae; Jeong, Goojin; Kim, Jung Ho; Kim, Young-Jun; Kim, Hansu

2015-02-01

Mesoporous silicon-based materials gained considerable attention as high-capacity lithium-storage materials. However, the practical use is still limited by the complexity and limited number of available synthetic routes. Here, we report carbon-coated porous SiOx as high capacity lithium storage material prepared by using a sol-gel reaction of hydrogen silsesquioxane and oil-water templating. A hydrophobic oil is employed as a pore former inside the SiOx matrix and a precursor for carbon coating on the SiOx . The anode exhibits a high capacity of 730 mAh g(-1) and outstanding cycling performance over 100 cycles without significant dimensional changes. Carbon-coated porous SiOx also showed highly stable thermal reliability comparable to that of graphite. These promising properties come from the mesopores in the SiOx matrix, which ensures reliable operation of lithium storage in SiOx . The scalable sol-gel process presented here can open up a new avenue for the versatile preparation of porous SiOx lithium storage materials. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A Supercompressible, Elastic, and Bendable Carbon Aerogel with Ultrasensitive Detection Limits for Compression Strain, Pressure, and Bending Angle.

PubMed

Zhuo, Hao; Hu, Yijie; Tong, Xing; Chen, Zehong; Zhong, Linxin; Lai, Haihong; Liu, Linxiang; Jing, Shuangshuang; Liu, Qingzhong; Liu, Chuanfu; Peng, Xinwen; Sun, Runcang

2018-05-01

Ultralight and compressible carbon materials have promising applications in strain and pressure detection. However, it is still difficult to prepare carbon materials with supercompressibility, elasticity, stable strain-electrical signal response, and ultrasensitive detection limits, due to the challenge in structural regulation. Herein, a new strategy to prepare a reduced graphene oxide (rGO)-based lamellar carbon aerogels with unexpected and integrated performances by designing wave-shape rGO layers and enhancing the interaction among the rGO layers is demonstrated. Addition of cellulose nanocrystalline and low-molecular-weight carbon precursors enhances the interaction among rGO layers and thus produces an ultralight, flexible, and superstable structure. The as-prepared carbon aerogel displays a supercompressibility (undergoing an extreme strain of 99%) and elasticity (100% height retention after 10 000 cycles at a strain of 30%), as well as stable strain-current response (at least 10 000 cycles). Particularly, the carbon aerogel is ultrasensitive for detecting tiny change in strain (0.012%) and pressure (0.25 Pa), which are the lowest detection limits for compressible carbon materials reported in the literature. Moreover, the carbon aerogel exhibits excellent bendable performance and can detect an ultralow bending angle of 0.052°. Additionally, the carbon aerogel also demonstrates its promising application as wearable devices. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Material Transport in ASDEX Upgrade

NASA Astrophysics Data System (ADS)

Rohde, V.; Dux, R.; Mayer, M.; Neu, R.; PA~ 1/4 tterich, T.; Schneider, W.; ASDEX Upgrade-Team,

Today carbon is the most common first wall material in fusion experiments, whereas the first wall of the next step device will consist of a mixture of elements. Especially tungsten has been shown to be an alternative to low-Z materials. However, even with 40% of tungsten coated plasma facing components, carbon is still the dominant impurity at ASDEX Upgrade. A consistent picture of the carbon migration in ASDEX Upgrade has been achieved. Primary carbon sources are the protection limiters at the low field side of the main chamber. Eroded carbon is distributed all over the main chamber. So, the initially tungsten coated central column acts as the main carbon source during discharges, even though a considerable amount of tungsten surfaces persists. Carbon coverage of the central column can significantly change on a shot to shot basis. The divertor target plates act as a strong carbon sink. Deposits are found at the inner and outer divertor, which may be re-eroded forming precursors for layer production at remote areas. In ASDEX Upgrade, deposits on the subdivertor structure are formed by hydro-carbons with a high effective sticking coefficient. A parasitic plasma at these locations may enhance the surface loss probability by surface activation. At more remote areas, such as the pump ducts, a very small deposition is found. Non sticking hydro-carbons are effectively pumped by the cryopump and turbo molecular pumps.

Effects of Different Fabrication Techniques on the Yttrium-Barium-Copper Oxide High Temperature Superconductor

DTIC Science & Technology

1988-12-01

and barium peroxide. The eperimental design includes barium carbonate as a precursor since it is a comronly used starting material for the ccupound...Kerans, Materials Laboratory, for his assistance in designing this project. I would also like to thank Tim Peterson for his patient instructing. I...the design of the devices used for taking measurements was detailed. Chapter IV showed the results of each type of measurement on each individual

Highly microporous carbons derived from a complex of glutamic acid and zinc chloride for use in supercapacitors

NASA Astrophysics Data System (ADS)

Dong, Xiao-Ling; Lu, An-Hui; He, Bin; Li, Wen-Cui

2016-09-01

The selection of carbon precursor is an important factor when designing carbon materials. In this study, a complex derived from L-glutamic acid and zinc chloride was used to prepare highly microporous carbons via facile pyrolysis. L-glutamic acid, a new carbon precursor with nitrogen functionality, coordinated with zinc chloride resulted in a homogeneous distribution of Zn2+ on the molecular level. During pyrolysis, the evaporation of the in situ formed zinc species creates an abundance of micropores together with the inert gases. The obtained carbons exhibit high specific surface area (SBET: 1203 m2 g-1) and a rich nitrogen content (4.52 wt%). In excess of 89% of the pore volume consists of micropores with pore size ranging from 0.5 to 1.2 nm. These carbons have been shown to be suitable for use as supercapacitor electrodes, and have been tested in 6 M KOH where a capacitance of 217 F g-1 was achieved at a current density of 0.5 A g-1. A long cycling life of 30 000 cycles was achieved at a current density of 1 A g-1, with only a 9% loss in capacity. The leakage current through a two-electrode device was measured as 2.3 μA per mg of electrode and the self-discharge characteristics were minimal.

Microporous Co@C Nanoparticles Prepared by Dealloying CoAl@C Precursors: Achieving Strong Wideband Microwave Absorption via Controlling Carbon Shell Thickness.

PubMed

Li, Da; Liao, Haoyan; Kikuchi, Hiroaki; Liu, Tong

2017-12-27

Excellent magnetic features make Co-based materials promising candidates as high-performance microwave absorbers. However, it is still a significant challenge for Co-based absorbers to possess high-intensity and broadband absorption simultaneously, owing to the lack of dielectric loss and impedance matching. Herein, microporous Co@C nanoparticles (NPs) with carbon shell thicknesses ranging from 1.8-4.9 nm have been successfully synthesized by dealloying CoAl@C precursors. All of the samples exhibit high microwave absorption performance. The microporous Co@C sample possessing a carbon shell of 1.8 nm exhibits the highest absorption intensity among these samples with a minimum reflection loss (RL) of -141.1 dB, whose absorption bandwidth for RL ≤ -10 dB is 7.3 GHz. As the thickness of the carbon shell increases, the absorption bandwidth of the NPs becomes wider. For the sample with the carbon shell thickness of 4.9 nm, the absorption bandwidth for RL ≤ -10 dB reaches a record high of 13.2 GHz. The outstanding microwave attenuation properties are attributed to the dielectric loss of the carbon shell, the magnetic loss of the Co core, and the cooperation of the core-shell structure and microporous morphology. The strong wideband microwave absorption of the carbon-coated microporous Co NPs highlights their potential applications in microwave absorbing systems.

Radiochemical synthesis of a carbon-supported Pt-SnO2 bicomponent nanostructure exhibiting enhanced catalysis of ethanol oxidation

NASA Astrophysics Data System (ADS)

Okazaki, Tomohisa; Seino, Satoshi; Nakagawa, Takashi; Kugai, Junichiro; Ohkubo, Yuji; Akita, Tomoki; Nitani, Hiroaki; Yamamoto, Takao A.

2015-03-01

Carbon-supported Pt-SnO2 electrocatalysts with various Sn/Pt molar ratios were prepared by an electron beam irradiation method. These catalysts were composed of metallic Pt particles approximately 5 nm in diameter together with low crystalline SnO2. The contact between the Pt and SnO2 in these materials varied with the amount of dissolved oxygen in the precursor solutions and it was determined that intimate contact between the Pt and SnO2 significantly enhanced the catalytic activity of these materials during the ethanol oxidation reaction. The mechanism by which the contact varies is discussed based on the radiochemical reduction process.

The effect of synthesis time on graphene growth from palm oil as green carbon precursor

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

Salifairus, M. J., E-mail: salifairus-mj85@yahoo.co.uk; Faculty of Applied Sciences, Universiti Teknologi MARA; NANO-ElecTronic Centre - Faculty of Electrical Engineering, Universiti Teknologi MARA

2016-07-06

Graphene is the new material that arises after carbon nanotubes (CNTs) era and has extraordinary optical, electronic and mechanical properties compared to CNTs. The 2D graphene is the sp{sup 2} carbon allotropes compared to other dimensionality. It also can be in three forms that are zero-dimensional, one-dimensional or three-dimensional. The different dimensionality also called fullerenes, nanotubes and graphite. Therefore, the graphene is known as centre potential materials in expanding research area than others ever. The 2 cm × 2 cm silicon wafer was seeded with nickel (Ni) at different thickness by using sputter coater. The palm oil, carbon source, wasmore » placed in the precursor furnace and the silicon was placed in the second furnace (deposition furnace). The palm oil will mix with Nitrogen gas was used as carrier gas in the CVD under certain temperature and pressure to undergo pyrolysis proses. The deposition temperature was set at 1000 °C. The deposition time varied from 3 minutes, 5 minutes and 7 minutes. The graphene was growth at ambient pressure in the CVD system. Electron microscopy and Raman Spectrometer revealed the structural properties and surface morphology of the grapheme on the substrate. The D and G band appear approximately at 1350 cm{sup −1} and 1850 cm{sup −1}. It can be concluded that the growth of graphene varies at different deposition time.« less

Waterproof Silicone Coatings of Thermal Insulation and Vaporization Method

NASA Technical Reports Server (NTRS)

Cagliostro, Domenick E. (Inventor)

1999-01-01

Thermal insulation composed of porous ceramic material can be waterproofed by producing a thin silicone film on the surface of the insulation by exposing it to volatile silicone precursors at ambient conditions. When the silicone precursor reactants are multi-functional siloxanes or silanes containing alkenes or alkynes carbon groups higher molecular weight films can be produced. Catalyst are usually required for the silicone precursors to react at room temperature to form the films. The catalyst are particularly useful in the single component system e.g. dimethylethoxysilane (DNMS) to accelerate the reaction and decrease the time to waterproof and protect the insulation. In comparison to other methods, the chemical vapor technique assures better control over the quantity and location of the film being deposited on the ceramic insulation to improve the waterproof coating.

Template-free fabrication of hollow N-doped carbon sphere (h-NCS) to synthesize h-NCS@PANI positive material for MoO3//h-NCS@PANI asymmetric supercapacitor

NASA Astrophysics Data System (ADS)

Li, Xiaoqin; Xiang, Xinxin; Liu, Yunhua; Xiao, Dan

2018-06-01

Asymmetric supercapacitors (ASCs) based on pseudocapacitor electrode materials are vital to improve the electrochemical properties of devices in aqueous electrolytes. This study fabricates hollow N-doped carbon sphere (h-NCS) to produce h-NCS@PANI nanocomposite as positive electrode and α-MoO3 as negative electrode to assemble ASC device. In particular, a facile template-free synthesis method, catalyzed by Cu2+, is used to prepare hollow PANI nanosphere precursor to build h-NCS. The mechanism of the precursor formation is illustrated in detail. After polymerization of PANI on the surface of h-NCS, the capacitance increases to 327 F g-1 at 1 A g-1. Furthermore, a hydrothermal reaction is carried out to produce α-MoO3 negative electrode material. The maximum specific capacitance of 720 F g-1 is achieved at 1 A g-1. The obtained h-NCS@PANI and α-MoO3 are utilized to construct an ASC device. The electrochemical properties of this device are investigated comprehensively. The maximum energy density of 34.1 W h kg-1 and power density of 9350.6 W kg-1 are observed, which provide an insight into the development of ASCs.

SiCO-doped carbon fibers with unique dual superhydrophilicity/superoleophilicity and ductile and capacitance properties.

PubMed

Lu, Ping; Huang, Qing; Mukherjee, Amiya; Hsieh, You-Lo

2010-12-01

Silicon oxycarbide (SiCO) glass-doped carbon fibers with an average diameter of 163 nm were successfully synthesized by electrospinning polymer mixtures of preceramic precursor polyureasilazane (PUS) and carbon precursor polyacrylonitrile (PAN) into fibers then converting to ceramic/carbon hybrid via cross-linking, stabilization, and pyrolysis at temperatures up to 1000 °C. The transformation of PUS/PAN polymer precursors to SiCO/carbon structures was confirmed by EDS and FTIR. Both carbon and SiCO/carbon fibers were amorphous and slightly oxidized. Doping with SiCO enhanced the thermal stability of carbon fibers and acquired new ductile behavior in the SiCO/carbon fibers with significantly improved flexibility and breaking elongation. Furthermore, the SiCO/carbon fibers exhibited dual superhydrophilicity and superoleophilicity with water and decane absorbing capacities of 873 and 608%, respectively. The cyclic voltammetry also showed that SiCO/carbon composite fibers possess better capacitor properties than carbon fibers.

Preparation of activated carbon monolith by application of phenolic resins as carbon precursors

NASA Astrophysics Data System (ADS)

Sajad, Mehran; Kazemzad, Mahmood; Hosseinnia, Azarmidokht

2014-04-01

In the current work, activated carbon monoliths have been prepared by application of different phenolic hydrocarbons namely catechol and resorcinol as carbon precursors. For synthesis of carbon monolith, the precursors have been mixed with Genapol PF-10 as template and then polymerized in the presence of lysine as catalyst. Then the polymerized monolith carbonized in inert atmosphere at 700°C and activated by water steam at 550°C. It was found that resorcinol polymerization is easier than catechol and occurred at 90°C while for polymerization of catechol elevated temperature of 120°C at hydrothermal condition is necessary. The prepared activated carbon samples have been characterized by various analysis methods including scanning electron microscopy (SEM), surface area measurement, and transmission electron microscopy (TEM). The adsorptions of three different aromatic hydrocarbons by the prepared activated carbon samples have also been investigated by high performance liquid chromatography (HPLC) and UV-Vis spectroscopy. It was found that carbon monolith prepared by catechol as carbon precursor has higher adsorpability and strength in comparison with the other sample. The higher performance of carbon monolith prepared by catechol can be associated with its higher active sites in comparison with resorcinol.

Preparation of nitrogen-doped carbon using graphene Quantum dots-chitosan as the precursor and its supercapacitive behaviors.

PubMed

Tan, Wensheng; Fu, Renjun; Ji, Hong; Kong, Yong; Xu, Yueguo; Qin, Yong

2018-06-01

Nitrogen-doped carbon (N-C) is pyrolytically prepared by using the nanocomposites of graphene Quantum dots (GQDs) and chitosan (CS) as the precursor. Due to the existence of GQDs nanofiller, the three-dimensional (3D) interconnected frameworks of CS are well preserved after the pyrolysis treatment; meanwhile, CS in the nanocomposites functions as nitrogen source for the N-C. The obtained N-C exhibits a considerable specific capacitance (545Fg -1 at 1Ag -1 ), high rate capability and excellent cyclic stability (88.9% capacitance retention after 5000cycles at 10Ag -1 ) when it is used as the electrode materials in supercapacitors. The well-preserved 3D frameworks and N-doping are believed to be responsible for the excellent supercapacitive behaviors of the N-C. Copyright © 2018 Elsevier B.V. All rights reserved.

Preparation of macrocycles with high carbon content: Toward the synthesis of endohedral metal fullerene complexes

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

Parker, T.C.; Rubin, Y.

1995-12-31

This research is focused on the synthesis of macrocycles with high carbon content for the purpose of total synthesis of fullerenes or fullerene-like structures with the ultimate goal of obtaining endohedral metal complexes of fullerene C{sub 60}. Toward this goal, the authors have utilized organometallic chemistry to synthesize novel cyclophanes such as 1 which are constituted primarily of acetylenic units. The authors believe such macrocycles may be C{sub 60} precursors since studies have shown that acetylenic macrocycles form fullerenes in the gas phase. The authors have synthesized macrocycle 1 using a highly convergent route from commercially available starting materials. Themore » macrocycle 1 is produced from copper (I) catalyzed coupling of 2 which is obtained in turn by the coupling of the copper acetylide 3 with 4. The suitability of macrocycles such as 1 for fullerene precursors is currently under investigation.« less

Purification of carbon nanotubes via selective heating

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

Rogers, John A.; Wilson, William L.; Jin, Sung Hun

The present invention provides methods for purifying a layer of carbon nanotubes comprising providing a precursor layer of substantially aligned carbon nanotubes supported by a substrate, wherein the precursor layer comprises a mixture of first carbon nanotubes and second carbon nanotubes; selectively heating the first carbon nanotubes; and separating the first carbon nanotubes from the second carbon nanotubes, thereby generating a purified layer of carbon nanotubes. Devices benefiting from enhanced electrical properties enabled by the purified layer of carbon nanotubes are also described.

Atomic Layer Epitaxy of Aluminum Nitride: Unraveling the Connection between Hydrogen Plasma and Carbon Contamination.

PubMed

Erwin, Steven C; Lyons, John L

2018-06-13

Atomistic control over the growth of semiconductor thin films, such as aluminum nitride, is a long-sought goal in materials physics. One promising approach is plasma-assisted atomic layer epitaxy, in which separate reactant precursors are employed to grow the cation and anion layers in alternating deposition steps. The use of a plasma during the growth-most often a hydrogen plasma-is now routine and generally considered critical, but the precise role of the plasma is not well-understood. We propose a theoretical atomistic model and elucidate its consequences using analytical rate equations, density functional theory, and kinetic Monte Carlo statistical simulations. We show that using a plasma has two important consequences, one beneficial and one detrimental. The plasma produces atomic hydrogen in the gas phase, which is important for removing methyl radicals left over from the aluminum precursor molecules. However, atomic hydrogen also leads to atomic carbon on the surface and, moreover, opens a channel for trapping these carbon atoms as impurities in the subsurface region, where they remain as unwanted contaminants. Understanding this dual role leads us to propose a solution for the carbon contamination problem which leaves the main benefit of the plasma largely unaffected.

The effect of precursor on the optical properties of carbon quantum dots synthesized by hydrothermal/solvothermal method

NASA Astrophysics Data System (ADS)

Mozdbar, Afsaneh; Nouralishahi, Amideddin; Fatemi, Shohreh; Mirakhori, Ghazaleh

2018-01-01

In the recent decade, Carbon Quantum Dots (CQDs) have attracted lots of attention due to their excellent properties such as tunable photoluminescence, high chemical stability, low toxicity, and biocompatibility. Among all synthesis methods, the hydrothermal/solvothermal rout has been considered as one of the most common and simplest method. The type of precursors can affect the size of CQDs and determine their surface functional groups, the essential properties that deeply influence the optical specifications. In this work, the effect of different precursors on the final properties of carbon quantum dots is investigated. The carbon quantum dots were synthesized by hydrothermal/solvothermal rout using citric acid, thiourea, ethylamine and monoethanolamine as precursors in almost the same conditions of time and temperature. Resultant CQDs were characterized by using FTIR, UV-Visible Spectroscopy and Photoluminescence (PL) analysis. The results of UV-Vis spectroscopy showed that quantum dots synthesized from monoethanolamine have wider absorption band rather than the CQDs from other precursors and the absorption edge shifted from about 270 nm for ethylamine to about 470 nm in monoethanolamine. Furthermore, the results demonstrate that using citric acid and monoethanolamine as precursor improved production efficiency and emission quantum yield of the carbon dots.

Enhancement of p-nitrophenol adsorption capacity through N2-thermal-based treatment of activated carbons

NASA Astrophysics Data System (ADS)

Álvarez-Torrellas, S.; Martin-Martinez, M.; Gomes, H. T.; Ovejero, G.; García, J.

2017-08-01

In this work several activated carbons showing different textural and chemical properties were obtained by chemical and physical activation methods, using a lignocellulosic material (peach stones) as precursor. The activated carbon resulting from the chemical activation, namely as CAC, revealed the best textural properties (SBET = 1521 m2 g-1, pore volume = 0.90 cm3 g-1) and an acidic character. It was found that the activated carbon obtained at 300 °C (under air atmosphere, PAC_air), and those synthesized at 750 °C in presence of N2 flow with bubbling of water/12 M H3PO4 solution (PAC_N2(H2O)/PAC_N2(H3PO4)), respectively, revealed worse textural properties, compared to CAC. Two functionalization treatments, by using sulphuric acid at boiling temperature (PACS) and nitric acid-urea-N2 heating at 800 °C (PAC-NUT), were applied to PAC_air, in order to enhance the adsorption ability of the carbon material. Several techniques were carried out to characterize the physical and chemical properties of the obtained carbon materials. The modification treatments had influence on the carbon surface properties, since the nitric acid-urea-N2 heating treatment led to a carbon material with highly-improved properties (SBET = 679 m2 g-1, pHIEP = 5.3). Accordingly, the original and modified-carbon materials were tested as adsorbents to remove 4-nitrophenol (4-NP), assessing batch and fixed-bed column adsorption tests. PAC-NUT carbon offered the best adsorption behavior (qe = 234 mg g-1), showing a high ability for the removal of 4-NP from water.

The synthesis of a tritium, carbon-14, and stable isotope-labeled cathepsin C inhibitors.

PubMed

Allen, Paul; Bragg, Ryan A; Caffrey, Moya; Ericsson, Cecilia; Hickey, Michael J; Kingston, Lee P; Elmore, Charles S

2017-02-01

As part of a medicinal chemistry program aimed at developing a highly potent and selective cathepsin C inhibitor, tritium, carbon-14, and stable isotope-labeled materials were required. The synthesis of tritium-labeled methanesulfonate 5 was achieved via catalytic tritiolysis of a chloro precursor, albeit at a low radiochemical purity of 67%. Tritium-labeled AZD5248 was prepared via a 3-stage synthesis, utilizing amide-directed hydrogen isotope exchange. Carbon-14 and stable isotope-labeled AZD5248 were successfully prepared through modifications of the medicinal chemistry synthetic route, enabling the use of available labeled intermediates. Copyright © 2016 John Wiley & Sons, Ltd.

Carbon nanofibers obtained from electrospinning process

NASA Astrophysics Data System (ADS)

Bovi de Oliveira, Juliana; Müller Guerrini, Lília; Sizuka Oishi, Silvia; Rogerio de Oliveira Hein, Luis; dos Santos Conejo, Luíza; Cerqueira Rezende, Mirabel; Cocchieri Botelho, Edson

2018-02-01

In recent years, reinforcements consisting of carbon nanostructures, such as carbon nanotubes, fullerenes, graphenes, and carbon nanofibers have received significant attention due mainly to their chemical inertness and good mechanical, electrical and thermal properties. Since carbon nanofibers comprise a continuous reinforcing with high specific surface area, associated with the fact that they can be obtained at a low cost and in a large amount, they have shown to be advantageous compared to traditional carbon nanotubes. The main objective of this work is the processing of carbon nanofibers, using polyacrylonitrile (PAN) as a precursor, obtained by the electrospinning process via polymer solution, with subsequent use for airspace applications as reinforcement in polymer composites. In this work, firstly PAN nanofibers were produced by electrospinning with diameters in the range of (375 ± 85) nm, using a dimethylformamide solution. Using a furnace, the PAN nanofiber was converted into carbon nanofiber. Morphologies and structures of PAN and carbon nanofibers were investigated by scanning electron microscopy, Raman Spectroscopy, thermogravimetric analyses and differential scanning calorimeter. The resulting residual weight after carbonization was approximately 38% in weight, with a diameters reduction of 50%, and the same showed a carbon yield of 25%. From the analysis of the crystalline structure of the carbonized material, it was found that the material presented a disordered structure.

Urea-based hydrothermal synthesis of LiNi0.5Co0.2Mn0.3O2 cathode material for Li-ion battery

NASA Astrophysics Data System (ADS)

Shi, Yang; Zhang, Minghao; Fang, Chengcheng; Meng, Ying Shirley

2018-08-01

A urea-based hydrothermal approach has been applied to synthesize LiNi0.5Co0.2Mn0.3O2 (NCM523) cathode materials with focus on investigating the influence of the reaction conditions on their electrochemical performance. The compositions of the carbonate precursor are precisely controlled by tuning urea concentration, hydrothermal reaction temperature, and time. The mole ratio between urea and transition metal ions and reaction temperature influence the composition of the precursor; while the reaction time influences the electrochemical performance of the final product. The optimized materials show better cyclability and rate capability compared with the materials synthesized with other hydrothermal reaction conditions. The enhancement is attributed to the larger Li+ diffusion coefficient and lower charge transfer resistance, which are due to the lower degree of Li/Ni cation mixing and more uniform distribution of transition metal ions. This work is a systematic study on the synthesis of NCM523 cathode material by a urea-based hydrothermal approach.

Method for reproducibly preparing a low-melting high-carbon yield precursor

DOEpatents

Smith, Wesley E.; Napier, Jr., Bradley

1978-01-01

The present invention is directed to a method for preparing a reproducible synthetic carbon precursor by the autoclave polymerization of indene (C.sub.9 H.sub.8) at a temperature in the range of 470.degree.-485.degree. C, and at a pressure in the range of about 1000 to about 4300 psi. Volatiles in the resulting liquid indene polymer are removed by vacuum outgassing to form a solid carbon precursor characterized by having a relatively low melting temperature, high-carbon yield, and high reproducibility which provide for the fabrication of carbon and graphite composites having strict requirements for reproducible properties.

Morphology and dispersion of FeCo alloy nanoparticles dispersed in a matrix of IR pyrolized polyvinyl alcohol

NASA Astrophysics Data System (ADS)

Vasilev, A. A.; Dzidziguri, E. L.; Muratov, D. G.; Zhilyaeva, N. A.; Efimov, M. N.; Karpacheva, G. P.

2018-04-01

Metal-carbon nanocomposites consisting of FeCo alloy nanoparticles dispersed in a carbon matrix were synthesized by the thermal decomposition method of a precursor based on polyvinyl alcohol and metals salts. The synthesized powders were investigated by X-ray diffraction (XRD), X-ray fluorescent spectrometry (XRFS), transmission electron microscopy (TEM) and scanning electron microscopy (SEM). Surface characteristics of materials were measured by BET-method. The morphology and dispersity of metal nanoparticles were studied depending on the metals ratio in the composite.

Fluorescence spectroscopy for monitoring reduction of natural organic matter and halogenated furanone precursors by biofiltration.

PubMed

Peleato, Nicolás M; McKie, Michael; Taylor-Edmonds, Lizbeth; Andrews, Susan A; Legge, Raymond L; Andrews, Robert C

2016-06-01

The application of fluorescence spectroscopy to monitor natural organic matter (NOM) reduction as a function of biofiltration performance was investigated. This study was conducted at pilot-scale where a conventional media filter was compared to six biofilters employing varying enhancement strategies. Overall reductions of NOM were identified by measuring dissolved organic carbon (DOC), and UV absorbance at 254 nm, as well as characterization of organic sub-fractions by liquid chromatography-organic carbon detection (LC-OCD) and parallel factors analysis (PARAFAC) of fluorescence excitation-emission matrices (FEEM). The biofilter using granular activated carbon media, with exhausted absorptive capacity, was found to provide the highest removal of all identified PARAFAC components. A microbial or processed humic-like component was found to be most amenable to biodegradation by biofilters and removal by conventional treatment. One refractory humic-like component, detectable only by FEEM-PARAFAC, was not well removed by biofiltration or conventional treatment. All biofilters removed protein-like material to a high degree relative to conventional treatment. The formation potential of two halogenated furanones, 3-chloro-4(dichloromethyl)-2(5H)-furanone (MX) and mucochloric acid (MCA), as well as overall treated water genotoxicity are also reported. Using the organic characterization results possible halogenated furanone and genotoxicity precursors are identified. Comparison of FEEM-PARAFAC and LC-OCD results revealed polysaccharides as potential MX/MCA precursors. Copyright © 2016 Elsevier Ltd. All rights reserved.

Composite Properties of Polyimide Resins Made From "Salt-Like" Solution Precursors

NASA Technical Reports Server (NTRS)

Cano, Roberto J.; Weiser, Erik S.; SaintClair, Terry L.; Echigo, Yoshiaki; Kaneshiro, Hisayasu

1997-01-01

Recent work in high temperature materials at NASA Langley Research Center (LaRC (trademark)) have led to the development of new polyimide resin systems with very attractive properties. The majority of the work done with these resin systems has concentrated on determining engineering mechanical properties of composites prepared from a poly(amide acid) precursor. Three NASA Langley-developed polyimide matrix resins, LaRC (trademark) -IA, LaRC (trademark) -IAX, and LaRC (trademark) -8515, were produced via a salt-like process developed by Unitika Ltd. The 'salt-like' solutions (sixty-five percent solids in NMP) were prepregged onto Hexcel IM7 carbon fiber using the NASA LaRC Multipurpose Tape Machine. Process parameters were determined and composite panels fabricated. Mechanical properties are presented for these three intermediate modulus carbon fiber/polyimide matrix composites and compared to existing data on the same polyimide resin systems and IM7 carbon fiber manufactured via poly(amide acid) solutions (thirty-five percent solids in NMP). This work studies the effects of varying the synthetic route on the processing and mechanical properties of polyimide composites.

Laser-driven coating of vertically aligned carbon nanotubes with manganese oxide from metal organic precursors for energy storage.

PubMed

Pérez Del Pino, A; György, E; Alshaikh, I; Pantoja-Suárez, F; Andújar, J L; Pascual, E; Amade, R; Bertran-Serra, E

2017-09-29

Carbon nanotubes-transition metal oxide systems are intensively studied due to their excellent properties for electrochemical applications. In this work, an innovative procedure is developed for the synthesis of vertically aligned multi-walled carbon nanotubes (VACNTs) coated with transition metal oxide nanostructures. VACNTs are grown by plasma enhanced chemical vapor deposition and coated with a manganese-based metal organic precursor (MOP) film based on manganese acetate solution. Subsequent UV pulsed laser irradiation induces the effective heating-decomposition of the MOP leading to the crystallization of manganese oxide nanostructures on the VACNT surface. The study of the morphology, structure and composition of the synthesized materials shows the formation of randomly oriented MnO 2 crystals, with few nanometers in size, and to their alignment in hundreds of nm long filament-like structures, parallel to the CNT's long axis. Electrochemical measurements reveal a significant increase of the specific capacitance of the MnO 2 -VACNT system (100 F g -1 ) as compared to the initial VACNT one (21 F g -1 ).

Laser-driven coating of vertically aligned carbon nanotubes with manganese oxide from metal organic precursors for energy storage

NASA Astrophysics Data System (ADS)

Pérez del Pino, A.; György, E.; Alshaikh, I.; Pantoja-Suárez, F.; Andújar, J. L.; Pascual, E.; Amade, R.; Bertran-Serra, E.

2017-09-01

Carbon nanotubes-transition metal oxide systems are intensively studied due to their excellent properties for electrochemical applications. In this work, an innovative procedure is developed for the synthesis of vertically aligned multi-walled carbon nanotubes (VACNTs) coated with transition metal oxide nanostructures. VACNTs are grown by plasma enhanced chemical vapor deposition and coated with a manganese-based metal organic precursor (MOP) film based on manganese acetate solution. Subsequent UV pulsed laser irradiation induces the effective heating-decomposition of the MOP leading to the crystallization of manganese oxide nanostructures on the VACNT surface. The study of the morphology, structure and composition of the synthesized materials shows the formation of randomly oriented MnO2 crystals, with few nanometers in size, and to their alignment in hundreds of nm long filament-like structures, parallel to the CNT’s long axis. Electrochemical measurements reveal a significant increase of the specific capacitance of the MnO2-VACNT system (100 F g-1) as compared to the initial VACNT one (21 F g-1).

Carbon-based torsional and tensile artificial muscles driven by thermal expansion (presentation video)

NASA Astrophysics Data System (ADS)

Haines, Carter S.; Lima, Márcio D.; Li, Na; Spinks, Geoffrey M.; Foroughi, Javad; Madden, John D. W.; Kim, Shi-Hyeong; Fang, Shaoli; Jung de Andrade, Monica; Göktepe, Fatma; Göktepe, Ozer; Mirvakili, Seyed M.; Naficy, Sina; Lepró, Xavier; Oh, Jiyoung; Kozlov, Mikhail E.; Kim, Seon Jeong; Xu, Xiuru; Swedlove, Benjamin J.; Wallace, Gordon G.; Baughman, Ray H.

2014-03-01

High-performance artificial muscles have been produced from fibers having highly anisotropic thermal expansion. Inserting twist into these precursor fibers enables thermally-driven torsional actuation and can cause the formation of helical coils. Such coiled structures provide giant-stroke tensile actuation exceeding the 20% in-vivo contraction of natural muscles. This contraction is highly reversible, with over one million cycles demonstrated, and can occur without the hysteresis that plagues competing shape-memory and piezoelectric muscles. Several materials and composites are investigated, including low-cost, commercially-available muscle precursors, potentially facilitating thermally-responsive textiles that change porosity to provide wearer comfort.

Mixed ion/electron-conductive protective soft nanomatter-based conformal surface modification of lithium-ion battery cathode materials

NASA Astrophysics Data System (ADS)

Park, Jang-Hoon; Kim, Ju-Myung; Lee, Chang Kee; Lee, Sang-Young

2014-10-01

Understanding and control of interfacial phenomena between electrode material and liquid electrolytes are of major scientific importance for boosting development of high-performance lithium ion batteries with reliable electrochemical/safety attributes. Here, as an innovative surface engineering approach to address the interfacial issues, a new concept of mixed ion/electron-conductive soft nanomatter-based conformal surface modification of the cathode material is presented. The soft nanomatter is comprised of an electron conductive carbonaceous (C) substance embedded in an ion conductive polyimide (PI) nanothin compliant film. In addition to its structural uniqueness, the newly proposed surface modification benefits from a simple fabrication process. The PI/carbon soft nanomatter is directly synthesized on LiCoO2 surface via one-pot thermal treatment of polyamic acid (=PI precursor) and sucrose (=carbon source) mixture, where the LiCoO2 powders are chosen as a model system to explore the feasibility of this surface engineering strategy. The resulting PI/carbon coating layer facilitates electronic conduction and also suppresses unwanted side reactions arising from the cathode material-liquid electrolyte interface. These synergistic coating effects of the multifunctional PI/carbon soft nanomatter significantly improve high-voltage cell performance and also mitigate interfacial exothermic reaction between cathode material and liquid electrolyte.

Synthesis of carbon nanotubes from waste polyethylene plastics

NASA Astrophysics Data System (ADS)

Zhuo, Chuanwei

Generation of non-biodegradable wastes, such as plastics, and resulting land as well as water pollution therefrom discarded plastics have been continuously increasing, while landfill space decreases and recycling markets dwindle. Exploration of novel uses of such materials becomes therefore imperative. Here I present an innovative and unique partial conversion of plastic waste to valuable carbon nanomaterials. It is an overall exothermic and scalable process based on feeding waste plastics to a multi-stage, pyrolysis/combustion-synthesis reactor. Plain stainless steel screens are used as substrates as well as low-cost catalyst for both carbon nanomaterials synthesis and pyrolyzates generation. Nano carbon yields of as high as 13.6% of the weight of the polymer precursor were recorded. This demonstration provides a sustainable solution to both plastic waste utilization, and carbon nanomaterials mass production.

Sorption studies of nickel ions onto activated carbon

NASA Astrophysics Data System (ADS)

Joshi, Parth; Vyas, Meet; Patel, Chirag

2018-05-01

Activated porous carbons are made through pyrolysis and activation of carbonaceous natural as well as synthetic precursors. The use of low-cost activated carbon derived from azadirachta indica, an agricultural waste material, has been investigated as a replacement for the current expensive methods of removing nickel ions from wastewater. The temperature variation study showed that the nickel ions adsorption is endothermic and spontaneous with increased randomness at the solid solution interface. Significant effect on adsorption was observed on varying the pH of the nickel ion solutions. Therefore, this study revealed that azadirachta indica can serve as a good source of activated carbon with multiple and simultaneous metal ions removing potentials and may serve as a better replacement for commercial activated carbons in applications that warrant their use.

Treatment of Lignin Precursors to Improve their Suitability for Carbon Fibers: A Literature Review

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

Paul, Ryan; Naskar, Amit; Gallego, Nidia

Lignin has been investigated as a carbon fiber precursor since the 1960s. Although there have been a number of reports of successful lignin-based carbon fiber production at the lab scale, lignin-based carbon fibers are not currently commercially available. This review will highlight some of the known challenges, and also the reported methods for purifying and modifying lignin to improve it as a precursor. Lignin can come from different sources (e.g. hardwood, softwood, grasses) and extraction methods (e.g. organosolv, kraft), meaning that lignin can be found with a diversity of purity and structure. The implication of these conditions on lignin asmore » carbon fiber precursor is not comprehensively known, especially as the lignin landscape is evolving. The work presented in this review will help guide the direction of a project between GrafTech and ORNL to develop lignin carbon fiber technology, as part of a cooperative agreement with the DOE Advanced Manufacturing Office.« less

Controlled chemical stabilization of polyvinyl precursor fiber, and high strength carbon fiber produced therefrom

DOEpatents

Naskar, Amit K.

2016-12-27

Method for the preparation of carbon fiber, which comprises: (i) immersing functionalized polyvinyl precursor fiber into a liquid solution having a boiling point of at least 60.degree. C.; (ii) heating the liquid solution to a first temperature of at least 25.degree. C. at which the functionalized precursor fiber engages in an elimination-addition equilibrium while a tension of at least 0.1 MPa is applied to the fiber; (iii) gradually raising the first temperature to a final temperature that is at least 20.degree. C. above the first temperature and up to the boiling point of the liquid solution for sufficient time to convert the functionalized precursor fiber to a pre-carbonized fiber; and (iv) subjecting the pre-carbonized fiber produced according to step (iii) to high temperature carbonization conditions to produce the final carbon fiber. Articles and devices containing the fibers, including woven and non-woven mats or paper forms of the fibers, are also described.

Micro-mesoporous carbon spheres derived from carrageenan as electrode material for supercapacitors

NASA Astrophysics Data System (ADS)

Fan, Yang; Yang, Xin; Zhu, Bing; Liu, Pei-Fang; Lu, Hai-Ting

2014-12-01

The polysaccharide carrageenan is used as a natural precursor to prepare micro-mesoporous carbon spheres. The carbon spheres were synthesized by hydrothermal carbonization of carrageenan, and subsequent chemical activation by KOH at different temperatures. The obtained micro-mesoporous carbon spheres have high surface area (up to 2502 m2 g-1) and large pore volume (up to 1.43 cm3 g-1). Moreover, the micro- and mesoporosity can be finely tuned be modifying the activation temperatures in the range of 700-900 °C. The carbon spheres activated at 900 °C present high specific capacitance of 230 F g-1 at a current density of 1 A g-1 and good ion transport kinetics. The good capacitive performance can be ascribed to the high specific surface area, well-controlled micro- and mesoporosity and narrow pore size distribution.

Selective growth of palladium and titanium dioxide nanostructures inside carbon nanotube membranes

NASA Astrophysics Data System (ADS)

Hevia, Samuel; Homm, Pía; Cortes, Andrea; Núñez, Verónica; Contreras, Claudia; Vera, Jenniffer; Segura, Rodrigo

2012-06-01

Hybrid nanostructured arrays based on carbon nanotubes (CNT) and palladium or titanium dioxide materials have been synthesized using self-supported and silicon-supported anodized aluminum oxide (AAO) as nanoporous template. It is well demonstrated that carbon nanotubes can be grown using these membranes and hydrocarbon precursors that decompose at temperatures closer to 600°C without the use of a metal catalyst. In this process, carbonic fragments condensate to form stacked graphitic sheets, which adopt the shape of the pores, yielding from these moulds' multi-walled carbon nanotubes. After this process, the ends of the tubes remain open and accessible to other substances, whereas the outer walls are protected by the alumina. Taking advantage of this fact, we have performed the synthesis of palladium and titanium dioxide nanostructures selectively inside carbon nanotubes using these CNT-AAO membranes as nanoreactors.

Selective growth of palladium and titanium dioxide nanostructures inside carbon nanotube membranes.

PubMed

Hevia, Samuel; Homm, Pía; Cortes, Andrea; Núñez, Verónica; Contreras, Claudia; Vera, Jenniffer; Segura, Rodrigo

2012-06-25

Hybrid nanostructured arrays based on carbon nanotubes (CNT) and palladium or titanium dioxide materials have been synthesized using self-supported and silicon-supported anodized aluminum oxide (AAO) as nanoporous template. It is well demonstrated that carbon nanotubes can be grown using these membranes and hydrocarbon precursors that decompose at temperatures closer to 600°C without the use of a metal catalyst. In this process, carbonic fragments condensate to form stacked graphitic sheets, which adopt the shape of the pores, yielding from these moulds' multi-walled carbon nanotubes. After this process, the ends of the tubes remain open and accessible to other substances, whereas the outer walls are protected by the alumina. Taking advantage of this fact, we have performed the synthesis of palladium and titanium dioxide nanostructures selectively inside carbon nanotubes using these CNT-AAO membranes as nanoreactors.

Synthesis and structural properties of (Y, Sr)(Ti, Fe, Nb)O3-δ perovskite nanoparticles fabricated by modified polymer precursor method

NASA Astrophysics Data System (ADS)

Miruszewski, T.; Gdaniec, P.; Karczewski, J.; Bochentyn, B.; Szaniawska, K.; Kupracz, P.; Prześniak-Welenc, M.; Kusz, B.

2016-09-01

The yttrium, iron and niobium doped-SrTiO3 powders have been successfully fabricated by a modified low-temperature synthesis method from a polymer complex. The usage of strontium hydroxide precursor instead of conventional strontium nitrate or strontium carbonate provides to the possibility of significant decrease of annealing temperature. It allows to prepare a material with sphere-shape grains of nanometric size (15-70 nm). The results of thermal analysis indicate that the crystallization of precursor takes place at different stages. The product after heat treatment at 600 °C for 3 h in air was also characterized by X-Ray diffraction method (XRD) and Fourier transform - infrared spectroscopy (FT-IR). After the crystallization and the impurity removal process, a single-phase material was obtained in case of all analyzed samples. The morphology of obtained nano-powders was also studied by a scanning electron microscopy (SEM). It can be concluded, that this method allows obtaining a perovskite phase of a metal doped SrTiO3 with nanometric particles.

Non-thermal plasma conversion of hydrocarbons

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

Strohm, James J.; Skoptsov, George L.; Musselman, Evan T.

A non-thermal plasma is generated to selectively convert a precursor to a product. More specifically, plasma forming material and a precursor material are provided to a reaction zone of a vessel. The reaction zone is exposed to microwave radiation, including exposing the plasma forming material and the precursor material to the microwave radiation. The exposure of the plasma forming material to the microwave radiation selectively converts the plasma forming material to a non-thermal plasma including formation of one or more streamers. The precursor material is mixed with the plasma forming material and the precursor material is exposed to the non-thermalmore » plasma including exposing the precursor material to the one or more streamers. The exposure of the precursor material to the streamers and the microwave radiation selectively converts the precursor material to a product.« less

Design, Synthesis, and Applications of Carbon Nanohoops

DTIC Science & Technology

2016-05-23

reductive transformation of a strained macrocyclic molecular precursor. These shape-persistent, conjugated structures are proposed to serve as...intersitially encapsulate analytes of interest, and to form a variety of new electronic polymer architectures. The accomplishments of this summer...produce a new-insoluble product. Initial investigations indicate that the material is highly conjugated due to the fluorescence properties. 1-H NMR is not

Determining sources of dissolved organic carbon and disinfection byproduct precursors to the McKenzie River, Oregon

USGS Publications Warehouse

Kraus, Tamara E.C.; Anderson, Chauncey W.; Morgenstern, Karl; Downing, Bryan D.; Pellerin, Brian A.; Bergamaschi, Brian A.

2010-01-01

This study was conducted to determine the main sources of dissolved organic carbon (DOC) and disinfection byproduct (DBP) precursors to the McKenzie River, Oregon (USA). Water samples collected from the mainstem, tributaries, and reservoir outflows were analyzed for DOC concentration and DBP formation potentials (trihalomethanes [THMFPs] and haloacetic acids [HAAFPs]). In addition, optical properties (absorbance and fluorescence) of dissolved organic matter (DOM) were measured to provide insight into DOM composition and assess whether optical properties are useful proxies for DOC and DBP precursor concentrations. Optical properties indicative of composition suggest that DOM in the McKenzie River mainstem was primarily allochthonous - derived from soils and plant material in the upstream watershed. Downstream tributaries had higher DOC concentrations than mainstem sites (1.6 ?? 0.4 vs. 0.7 ?? 0.3 mg L-1) but comprised <5% of mainstem flows and had minimal effect on overall DBP precursor loads. Water exiting two large upstream reservoirs also had higher DOC concentrations than the mainstem site upstream of the reservoirs, but optical data did not support in situ algal production as a source of the added DOC during the study. Results suggest that the first major rain event in the fall contributes DOM with high DBP precursor content. Although there was interference in the absorbance spectra in downstream tributary samples, fluorescence data were strongly correlated to DOC concentration (R 2 = 0.98), THMFP (R2 = 0.98), and HAAFP (R2 = 0.96). These results highlight the value of using optical measurements for identifying the concentration and sources of DBP precursors in watersheds, which will help drinking water utilities improve source water monitoring and management programs. Copyright ?? 2010 by the American Society of Agronomy.

Effect of ammonium carbonate to metal ions molar ratio on synthesis and sintering of Nd:YAG nanopowders

NASA Astrophysics Data System (ADS)

Liu, Qiang; Chen, Cong; Dai, Jiawei; Hu, Zewang; Chen, Haohong; Li, Jiang

2018-06-01

Using the nanopowders synthesized by a reverse co-precipitation method, neodymium doped yttrium aluminum garnet (Nd:YAG) transparent ceramics were fabricated by vacuum sintering method. The influence of ammonium carbonate to metal ions (NH4HCO3/M3+) molar ratio (R value) on the properties of Nd:YAG precursors and powders, as well as the densification, microstructure, and transmittance of the resultant ceramics was systematically investigated. The results show that the precursors have similar compositions and the calcined powders have pure Y3Al5O12 (YAG) phase. However, the R value is closely related to the morphologies of the precursors and powders. It is found that the powder with R = 3.0 has strongest agglomeration and the powders with R = 3.2-4.0 show better dispersity. Using these powders as starting materials, the corresponding ceramics were sintered at 1720 °C for 20 h in vacuum. As a result, the ceramic with R = 3.2 obtains the best transmittance of about 72% at the wavelength of 1064 nm. The grain growth exponent and activation energy of the Nd:YAG ceramics fabricated from the powder with R = 3.2 were also studied.

Precursor Selection for Property Optimization in Biomorphic SiC Ceramics

NASA Technical Reports Server (NTRS)

Varela-Feria, F. M.; Lopez-Robledo, M. J.; Martinez-Fernandez, J.; deArellano-Lopez, A. R.; Singh, M.; Gray, Hugh R. (Technical Monitor)

2002-01-01

Biomorphic SiC ceramics have been fabricated using different wood precursors. The evolution of volume, density and microstructure of the woods, carbon performs, and final SiC products are systematically studied in order to establish experimental guidelines that allow materials selection. The wood density is a critical characteristic, which results in a particular final SiC density, and the level of anisotropy in mechanical properties in directions parallel (axial) and perpendicular (radial) to the growth of the wood. The purpose of this work is to explore experimental laws that can help choose a type of wood as precursor for a final SiC product, with a given microstructure, density and level of anisotropy. Preliminary studies of physical properties suggest that not only mechanical properties are strongly anisotropic, but also electrical conductivity and gas permeability, which have great technological importance.

Multicomponent patterned ultrathin carbon nanomembranes by laser ablation

NASA Astrophysics Data System (ADS)

Frese, Natalie; Scherr, Julian; Beyer, André; Terfort, Andreas; Gölzhäuser, Armin; Hampp, Norbert; Rhinow, Daniel

2018-01-01

Carbon nanomembranes (CNMs) are a class of two-dimensional materials, which are obtained by electron beam-induced crosslinking of aromatic self-assembled monolayers (SAMs) on solid substrates. CNMs made from a single type of precursor molecule are uniform with homogeneous chemical and physical properties. We have developed a method for the fabrication of internally patterned CNMs resembling a key feature of biological membranes. Direct laser patterning is used to obtain multicomponent patterned SAMs on gold, which are subsequently crosslinked by electron irradiation. We demonstrate that the structure of internally patterned CNMs is preserved upon transfer to different substrates. The method enables rapid fabrication of patterned 2D materials with local variations in chemical and physical properties on the micrometer to centimeter scale.

Investigating permeability and carbonation behavior of sustainable cements

NASA Astrophysics Data System (ADS)

White, C.; Blyth, A.; Scherer, G. W.; Morandeau, A. E.

2015-12-01

The durability of new sustainable cementitious materials is intimately linked with the ability for these materials to prevent the ingress of aggressive ions through their percolated pore networks. However, it is also important to be able to control and limit the detrimental chemical degradation mechanisms that occur to the cement binder once the ions have diffused through the pore network. Here, alkali-activated materials will be discussed, and recent research on measuring the permeability of this class of cements using the beam-bending method will be presented. It will be shown that the permeability can be controlled by tailoring the activator chemistry, and that the addition of free silica in the activator has a strong (favorable) influence on the resulting percolated pore network. Carbonation is one type of chemical degradation process that is known to severely shorten the service life of concrete, especially in environments containing elevated CO­2 levels. However, the exact atomic structural changes that occur to the main binder phase (calcium-silicate-hydrate gel) during carbonation remain largely unknown. Here, X-ray pair distribution function analysis is used to elucidate the local atomic structural changes that occur during carbonation of calcium-silicate-hydrate gel and calcium-aluminosilicate-hydrate gel (alkali-activated slag binder), where distinct differences in the extent of gel decalcification are measured according to the chemistry of the starting precursor material. The results will be discussed in the context of limiting the extent of carbonation in cementitious materials, with potential applications of alkali-activated materials in geological storage of CO2 due to their increased resistance to carbonation.

Engineering Hollow Carbon Architecture for High-Performance K-Ion Battery Anode.

PubMed

Bin, De-Shan; Lin, Xi-Jie; Sun, Yong-Gang; Xu, Yan-Song; Zhang, Ke; Cao, An-Min; Wan, Li-Jun

2018-05-31

K-ion batteries (KIBs) are now drawing increasing research interest as an inexpensive alternative to Li-ion batteries (LIBs). However, due to the large size of K + , stable electrode materials capable of sustaining the repeated K + intercalation/deintercalation cycles are extremely deficient especially if a satisfactory reversible capacity is expected. Herein, we demonstrated that the structural engineering of carbon into a hollow interconnected architecture, a shape similar to the neuron-cell network, promised high conceptual and technological potential for a high-performance KIB anode. Using melamine-formaldehyde resin as the starting material, we identify an interesting glass blowing effect of this polymeric precursor during its carbonization, which features a skeleton-softening process followed by its spontaneous hollowing. When used as a KIB anode, the carbon scaffold with interconnected hollow channels can ensure a resilient structure for a stable potassiation/depotassiation process and deliver an extraordinary capacity (340 mAh g -1 at 0.1 C) together with a superior cycling stability (no obvious fading over 150 cycles at 0.5 C).

Spent coffee-based activated carbon: specific surface features and their importance for H2S separation process.

PubMed

Kante, Karifala; Nieto-Delgado, Cesar; Rangel-Mendez, J Rene; Bandosz, Teresa J

2012-01-30

Activated carbons were prepared from spent ground coffee. Zinc chloride was used as an activation agent. The obtained materials were used as a media for separation of hydrogen sulfide from air at ambient conditions. The materials were characterized using adsorption of nitrogen, elemental analysis, SEM, FTIR, and thermal analysis. Surface features of the carbons depend on the amount of an activation agent used. Even though the residual inorganic matter takes part in the H(2)S retention via salt formation, the porous surface of carbons governs the separation process. The chemical activation method chosen resulted in formation of large volume of pores with sizes between 10 and 30Å, optimal for water and hydrogen sulfide adsorption. Even though the activation process can be optimized/changed, the presence of nitrogen in the precursor (caffeine) is a significant asset of that specific organic waste. Nitrogen functional groups play a catalytic role in hydrogen sulfide oxidation. Copyright © 2011 Elsevier B.V. All rights reserved.

Synthesis and electrochemical properties of olivine LiFePO 4 prepared by a carbothermal reduction method

NASA Astrophysics Data System (ADS)

Liu, Hui-ping; Wang, Zhi-xing; Li, Xin-hai; Guo, Hua-jun; Peng, Wen-jie; Zhang, Yun-he; Hu, Qi-yang

LiFePO 4/C composite cathode material was prepared by carbothermal reduction method, which uses NH 4H 2PO 4, Li 2CO 3 and cheap Fe 2O 3 as starting materials, acetylene black and glucose as carbon sources. The precursor of LiFePO 4/C was characterized by differential thermal analysis and thermogravimetry. X-ray diffraction (XRD), scanning electron microscopy (SEM) micrographs showed that the LiFePO 4/C is olivine-type phase, and the addition of the carbon reduced the LiFePO 4 grain size. The carbon is dispersed between the grains, ensuring a good electronic contact. The products sintered at 700 °C for 8 h with glucose as carbon source possessed excellent electrochemical performance. The synthesized LiFePO 4 composites showed a high electrochemical capacity of 159.3 mAh g -1 at 0.1 C rate, and the capacity fading is only 2.2% after 30 cycles.

Nanoscale Transforming Mineral Phases in Fresh Nacre

DOE PAGES

DeVol, Ross T.; Sun, Chang-Yu; Marcus, Matthew A.; ...

2015-09-24

Nacre, or mother-of-pearl, the iridescent inner layer of many mollusk shells, is a biomineral lamellar composite of aragonite (CaCO 3) and organic sheets. Biomineralization frequently occurs via transient amorphous precursor phases, crystallizing into the final stable biomineral. In nacre, despite extensive attempts, amorphous calcium carbonate (ACC) precursors have remained elusive. They were inferred from non-nacre-forming larval shells, or from a residue of amorphous material surrounding mature gastropod nacre tablets, and have only once been observed in bivalve nacre. Here we present the first direct observation of ACC precursors to nacre formation, obtained from the growth front of nacre in gastropodmore » shells from red abalone (Haliotis rufescens), using synchrotron spectromicroscopy. Surprisingly, the abalone nacre data show the same ACC phases that are precursors to calcite (CaCO 3) formation in sea urchin spicules, and not proto-aragonite or poorly crystalline aragonite (pAra), as expected for aragonitic nacre. In contrast, we find pAra in coral.« less

Thermal insulation for high temperature microwave sintering operations and method thereof

DOEpatents

Holcombe, Cressie E.; Dykes, Norman L.; Morrow, Marvin S.

1995-01-01

Superior microwave transparent thermal insulations for high temperature microwave sintering operations were prepared. One embodiment of the thermal insulation comprises granules of boron nitride coated with a very thin layer of glassy carbon made by preparing a glassy carbon precursor and blending it with boron nitride powder to form a mixture. The blended mixture is granulated to form a grit which is dried and heated to form the granules of boron nitride coated with a glassy carbon. Alternatively, grains of glassy carbon are coated with boron nitride by blending a mixture of a slurry comprising boron nitride, boric acid binder, and methyl alcohol with glassy carbon grains to form a blended mixture. The blended mixture is dried to form grains of glassy carbon coated with boron nitride. In addition, a physical mixture of boron nitride powder and glassy carbon grains has also been shown to be an excellent thermal insulation material for microwave processing and sintering.

Method of preparing thermal insulation for high temperature microwave sintering operations

DOEpatents

Holcombe, Cressie E.; Dykes, Norman L.; Morrow, Marvin S.

1996-01-01

Superior microwave transparent thermal insulations for high temperature microwave sintering operations were prepared. One embodiment of the thermal insulation comprises granules of boron nitride coated with a very thin layer of glassy carbon made by preparing a glassy carbon precursor and blending it with boron nitride powder to form a mixture. The blended mixture is granulated to form a grit which is dried and heated to form the granules of boron nitride coated with a glassy carbon. Alternatively, grains of glassy carbon are coated with boron nitride by blending a mixture of a slurry comprising boron nitride, boric acid binder, and methyl alcohol with glassy carbon grains to form a blended mixture. The blended mixture is dried to form grains of glassy carbon coated with boron nitride. In addition, a physical mixture of boron nitride powder and glassy carbon grains has also been shown to be an excellent thermal insulation material for microwave processing and sintering.

Corn stalks char from fast pyrolysis as precursor material for preparation of activated carbon in fluidized bed reactor.

PubMed

Wang, Zhiqi; Wu, Jingli; He, Tao; Wu, Jinhu

2014-09-01

Corn stalks char from fast pyrolysis was activated by physical and chemical activation process in a fluidized bed reactor. The structure and morphology of the carbons were characterized by N2 adsorption and SEM. Effects of activation time and activation agents on the structure of activation carbon were investigated. The physically activated carbons with CO2 have BET specific surface area up to 880 m(2)/g, and exhibit microporous structure. The chemically activated carbons with H3PO4 have BET specific surface area up to 600 m(2)/g, and exhibit mesoporous structure. The surface morphology shows that physically activated carbons exhibit fibrous like structure in nature with long ridges, resembling parallel lines. Whereas chemically activated carbons have cross-interconnected smooth open pores without the fibrous like structure. Copyright © 2014 Elsevier Ltd. All rights reserved.

Polymer-Templated LiFePO4/C Nanonetworks as High-Performance Cathode Materials for Lithium-Ion Batteries.

PubMed

Fischer, Michael G; Hua, Xiao; Wilts, Bodo D; Castillo-Martínez, Elizabeth; Steiner, Ullrich

2018-01-17

Lithium iron phosphate (LFP) is currently one of the main cathode materials used in lithium-ion batteries due to its safety, relatively low cost, and exceptional cycle life. To overcome its poor ionic and electrical conductivities, LFP is often nanostructured, and its surface is coated with conductive carbon (LFP/C). Here, we demonstrate a sol-gel based synthesis procedure that utilizes a block copolymer (BCP) as a templating agent and a homopolymer as an additional carbon source. The high-molecular-weight BCP produces self-assembled aggregates with the precursor-sol on the 10 nm scale, stabilizing the LFP structure during crystallization at high temperatures. This results in a LFP nanonetwork consisting of interconnected ∼10 nm-sized particles covered by a uniform carbon coating that displays a high rate performance and an excellent cycle life. Our "one-pot" method is facile and scalable for use in established battery production methodologies.

Enhancement of electrochemical performance of LiFePO4 nanoparticles by direct nanocoating with conductive carbon layers

NASA Astrophysics Data System (ADS)

Świder, Joanna; Molenda, Marcin; Kulka, Andrzej; Molenda, Janina

2016-07-01

The results of simple and environmental-friendly method of the carbon nanocoatings on low-conductive cathode material have been shown in this work. The carbon nanocoatings were prepared during wet impregnation process of precursor derived from hydrophilic polymer based on poly(N-vinylformamide) modified by pyromellitic acid. The crystal structures and morphology of all composites were characterized by X-ray powder diffraction (XRD), low temperature nitrogen adsorption/desorption measurements (N2-BET) and transmission electronic microscopy (TEM). The electrical properties of the obtained composites were examined by EC studies. The electrochemical performance was carried out in galvanostatic mode with stable charge-discharge current and performed in Li/Li+/(CCL/LiFePO4) type cells. The process of formation CCL/LiFePO4 nanocomposite significantly enhances the electrical conductivity of the material and improves its capacity retention and electrochemical performance.

From Metal-Organic Framework to Porous Carbon Polyhedron: Toward Highly Reversible Lithium Storage.

PubMed

Peng, Hai-Jun; Hao, Gui-Xia; Chu, Zhao-Hua; Cui, Ying-Lin; Lin, Xiao-Ming; Cai, Yue-Peng

2017-08-21

By application of a newly designed T-shaped ligand 5-(4-pyridin-4-yl-benzoylamino)isophthalic acid (H 2 PBAI) to assemble with Zn(II) ions under solvothermal conditions, a novel porous polyhedral metal-organic framework (Zn-PBAI) with pcu topology has been obtained. When treated as a precursor by annealing of Zn-PBAI at various temperatures, porous carbon polyhedra (PCP) were prepared and tested as an anode material for lithium-ion batteries. The results show that PCP carbonized at 1000 °C (PCP-1000) manifest the highest reversible specific capacity of about 1125 mAh g -1 at a current of 500 mA g -1 after 200 cycles, which is supposed to benefit from the large accessible specific area and high electric conductivity. Moreover, PCP-1000 electrode materials also exhibit superior cyclic stability and good rate capacity.

TiO2 and its composites as effective photocatalyst for glucose degradation processes

NASA Astrophysics Data System (ADS)

Kukh, A. A.; Ivanenko, I. M.; Astrelin, I. M.

2018-03-01

Titanium-dioxide photocatalyst was impregnated onto the activated carbon using originally developed low-temperature sol-gel method to form a TiO2:AC composite material. 15% (mass.) solution Ti2(SO4)3 in sulphuric acid was used as a precursor for photocatalyst synthesis. The highly effective composite material was obtained through a combination of properties of titanium dioxide and activated carbon. Synthesized composites TiO2 with activated carbon demonstrate highly developed surface characteristics and exhibit significantly higher activity in comparison with samples of pure TiO2 synthesized the same way, existing analogues of pure TiO2 synthesized from TiCl3 and even industrial photocatalyst. This was testified by the degradation of 1% aqueous glucose solution using TiO2:AC, samples of pure TiO2 and commercial TiO2 AEROXIDE® TiO2 P25 produced by EVONIK Industries.

A Designed TiO2 /Carbon Nanocomposite as a High-Efficiency Lithium-Ion Battery Anode and Photocatalyst.

PubMed

Peng, Liang; Zhang, Huijuan; Bai, Yuanjuan; Feng, Yangyang; Wang, Yu

2015-10-12

Herein, a peapod-like TiO2 /carbon nanocomposite has successfully been synthesized by a rational method for the first time. The novel nanostructure exhibits a distinct feature of TiO2 nanoparticles encapsulated inside and the carbon fiber coating outside. In the synthetic process, H2 Ti3 O7 nanotubes serve as precursors and templates, and glucose molecules act as the green carbon source. With the alliciency of hydrogen bonding between H2 Ti3 O7 and glucose, a thin polymer layer is hydrothermally assembled and subsequently converted into carbon fibers through calcinations under an inert atmosphere. Meanwhile, the precursors of H2 Ti3 O7 nanotubes are transformed into the TiO2 nanoparticles encapsulated in carbon fibers. The achieved unique nanocomposites can be used as excellent anode materials in lithium-ion batteries (LIBs) and photocatalytic reagents in the degradation of rhodamine B. Due to the synergistic effect derived from TiO2 nanoparticles and carbon fibers, the obtained peapod-like TiO2 /carbon cannot only deliver a high specific capacity of 160 mAh g(-1) over 500 cycles in LIBs, but also perform a much faster photodegradation rate than bare TiO2 and P25. Furthermore, owing to the low cost, environmental friendliness as well as abundant source, this novel TiO2 /carbon nanocomposite will have a great potential to be extended to other application fields, such as specific catalysis, gas sensing, and photovoltaics. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The role of amorphous precursors in the crystallization of La and Nd carbonates

NASA Astrophysics Data System (ADS)

Vallina, Beatriz; Rodriguez-Blanco, Juan Diego; Brown, Andrew P.; Blanco, Jesus A.; Benning, Liane G.

2015-07-01

Crystalline La and Nd carbonates can be formed from poorly-ordered nanoparticulate precursors, termed amorphous lanthanum carbonate (ALC) and amorphous neodymium carbonate (ANC). When reacted in air or in aqueous solutions these precursors show highly variable lifetimes and crystallization pathways. We have characterized these precursors and the crystallization pathways and products with solid-state, spectroscopic and microscopic techniques to explain the differences in crystallization mechanisms between the La and Nd systems. ALC and ANC consist of highly hydrated, 10-20 nm spherical nanoparticles with a general formula of REE2(CO3)3.5H2O (REE = La, Nd). The stabilities differ by ~2 orders of magnitude, with ANC being far more stable than ALC. This difference is due to the Nd3+ ion having a far higher hydration energy compared to the La3+ ion. This, together with temperature and reaction times, leads to clear differences not only in the kinetics and mechanisms of crystallization of the amorphous precursor La- and Nd-carbonate phases but also in the resulting crystallite sizes and morphologies of the end products. All crystalline La and Nd carbonates developed spherulitic morphologies when crystallization occurred from hydrous phases in solution at temperatures above 60 °C (La system) and 95 °C (Nd system). We suggest that spherulitic growth occurs due to a rapid breakdown of the amorphous precursors and a concurrent rapid increase in supersaturation levels in the aqueous solution. The kinetic data show that the crystallization pathway for both La and Nd carbonate systems is dependent on the reaction temperature and the ionic potential of the REE3+ ion.Crystalline La and Nd carbonates can be formed from poorly-ordered nanoparticulate precursors, termed amorphous lanthanum carbonate (ALC) and amorphous neodymium carbonate (ANC). When reacted in air or in aqueous solutions these precursors show highly variable lifetimes and crystallization pathways. We have characterized these precursors and the crystallization pathways and products with solid-state, spectroscopic and microscopic techniques to explain the differences in crystallization mechanisms between the La and Nd systems. ALC and ANC consist of highly hydrated, 10-20 nm spherical nanoparticles with a general formula of REE2(CO3)3.5H2O (REE = La, Nd). The stabilities differ by ~2 orders of magnitude, with ANC being far more stable than ALC. This difference is due to the Nd3+ ion having a far higher hydration energy compared to the La3+ ion. This, together with temperature and reaction times, leads to clear differences not only in the kinetics and mechanisms of crystallization of the amorphous precursor La- and Nd-carbonate phases but also in the resulting crystallite sizes and morphologies of the end products. All crystalline La and Nd carbonates developed spherulitic morphologies when crystallization occurred from hydrous phases in solution at temperatures above 60 °C (La system) and 95 °C (Nd system). We suggest that spherulitic growth occurs due to a rapid breakdown of the amorphous precursors and a concurrent rapid increase in supersaturation levels in the aqueous solution. The kinetic data show that the crystallization pathway for both La and Nd carbonate systems is dependent on the reaction temperature and the ionic potential of the REE3+ ion. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr01497b

Raman studies of the interactions of fibrous carbon nanomaterials with albumin

NASA Astrophysics Data System (ADS)

Wesełucha-Birczyńska, Aleksandra; Morajka, Krzysztof; Stodolak-Zych, Ewa; Długoń, Elżbieta; Dużyja, Maria; Lis, Tomasz; Gubernat, Maciej; Ziąbka, Magdalena; Błażewicz, Marta

2018-05-01

Adsorption or immobilization of proteins on synthetic surfaces is a key issue in the context of the biocompatibility of implant materials, especially those intended for the needs of cardiac surgery but also for the construction of biosensors or nanomaterials used as drug carriers. The subject of research was the analysis of Raman spectra of two types of fibrous carbon nanomaterials, of great potential for biomedical applications, incubated with human serum albumin (HSA). The first nanomaterial has been created on the layer of MWCNTs deposited by electrophoretic method (EPD) and then covered by thin film of pyrolytic carbon introduced by chemical vapor deposition process (CVD). The second material was formed from carbonized nanofibers prepared via electrospinning (ESCNFs) of polyacrylonitrile (PAN) precursor and then covered with pyrolytic carbon (CVD). The G-band blue-shift towards the position of about 1600 cm-1, observed for both studied surfaces, clearly indicates the albumin (HSA) adhesion to the surface. The G and G' (2D) peak shift was employed to assess the stress build up on the carbon nanomaterials. The surface nano- and micro-topography as well as the method of ordering the carbon nanomaterial has a significant influence on the mode of surface-protein interaction.

Laminated and Two-Dimensional Carbon-Supported Microwave Absorbers Derived from MXenes.

PubMed

Han, Meikang; Yin, Xiaowei; Li, Xinliang; Anasori, Babak; Zhang, Litong; Cheng, Laifei; Gogotsi, Yury

2017-06-14

Microwave absorbers with layered structures that can provide abundant interfaces are highly desirable for enhancing electromagnetic absorbing capability and decreasing the thickness. The atomically thin layers of two-dimensional (2D) transition-metal carbides (MXenes) make them a convenient precursor for synthesis of other 2D and layered structures. Here, laminated carbon/TiO 2 hybrid materials composed of well-aligned 2D carbon sheets with embedded TiO 2 nanoparticles were synthesized and showed excellent microwave absorption. Disordered 2D carbon layers with an unusual structure were obtained by annealing multilayer Ti 3 C 2 MXene in a CO 2 atmosphere. The minimum reflection coefficient of laminated carbon/TiO 2 composites reaches -36 dB, and the effective absorption bandwidth ranges from 3.6 to 18 GHz with the tunable thickness from 1.7 to 5 mm. The effective absorption bandwidth covers the whole Ku band (12.4-18 GHz) when the thickness of carbon/TiO 2 /paraffin composite is 1.7 mm. This study is expected to pave the way to the synthesis of carbon-supported absorbing materials using a large family of 2D carbides.

Confined-plume chemical deposition: rapid synthesis of crystalline coatings of known hard or superhard materials on inorganic or organic supports by resonant IR decomposition of molecular precursors.

PubMed

Ivanov, Borislav L; Wellons, Matthew S; Lukehart, Charles M

2009-08-26

A one-step process for preparing microcrystalline coatings of known superhard, very hard, or ultraincompressible ceramic compositions on either inorganic or organic supports is reported. Midinfrared pulsed-laser irradiation of preceramic chemical precursors layered between IR-transmissive hard/soft supports under temporal and spatial confinement at a laser wavelength resonant with a precursor vibrational band gives one-step deposition of crystalline ceramic coatings without incurring noticeable collateral thermal damage to the support material. Reaction plume formation at the precursor/laser beam interface initiates confined-plume, chemical deposition (CPCD) of crystalline ceramic product. Continuous ceramic coatings are produced by rastering the laser beam over a sample specimen. CPCD processing of the Re-B single-source precursor, (B(3)H(8))Re(CO)(4), the dual-source mixtures, Ru(3)(CO)(12)/B(10)H(14) or W(CO)(6)/B(10)H(14), and the boron/carbon single-source precursor, o-B(10)C(2)H(12), confined between Si wafer or NaCl plates gives microcrystalline deposits of ReB(2), RuB(2), WB(4), or B(4)C, respectively. CPCD processing of Kevlar fabric wetted by (B(3)H(8))Re(CO)(4) produces an oriented, microcrystalline coating of ReB(2) on the Kevlar fabric without incurring noticeable thermal damage of the polymer support. Similarly, microcrystalline coatings of ReB(2) can be formed on IR-transmissive IR2, Teflon, or Ultralene polymer films.

Utilization of Mineral Wools as Alkali-Activated Material Precursor

PubMed Central

Yliniemi, Juho; Kinnunen, Paivo; Karinkanta, Pasi; Illikainen, Mirja

2016-01-01

Mineral wools are the most common insulation materials in buildings worldwide. However, mineral wool waste is often considered unrecyclable because of its fibrous nature and low density. In this paper, rock wool (RW) and glass wool (GW) were studied as alkali-activated material precursors without any additional co-binders. Both mineral wools were pulverized by a vibratory disc mill in order to remove the fibrous nature of the material. The pulverized mineral wools were then alkali-activated with a sodium aluminate solution. Compressive strengths of up to 30.0 MPa and 48.7 MPa were measured for RW and GW, respectively, with high flexural strengths measured for both (20.1 MPa for RW and 13.2 MPa for GW). The resulting alkali-activated matrix was a composite-type in which partly-dissolved fibers were dispersed. In addition to the amorphous material, sodium aluminate silicate hydroxide hydrate and magnesium aluminum hydroxide carbonate phases were identified in the alkali-activated RW samples. The only crystalline phase in the GW samples was sodium aluminum silicate. The results of this study show that mineral wool is a very promising raw material for alkali activation. PMID:28773435

Living hybrid materials capable of energy conversion and CO2 assimilation.

PubMed

Meunier, Christophe F; Rooke, Joanna C; Léonard, Alexandre; Xie, Hao; Su, Bao-Lian

2010-06-14

This paper reviews our work on the fabrication of photobiochemical hybrid materials via immobilisation of photosynthetically active entities within silica materials, summarising the viability and productivity of these active entities post encapsulation and evaluating their efficiency as the principal component of a photobioreactor. Immobilisation of thylakoids extracted from spinach leaves as well as whole cells such as A. thaliana, Synechococcus and C. caldarium was carried out in situ using sol-gel methods. In particular, a comprehensive overview is given of the efforts to find the most biocompatible inorganic precursors that can extend the lifetime of the organisms upon encapsulation. The effect of matrix-cell interactions on cell lifetime and the photosynthetic efficiency of the resultant materials are discussed. Precursors based on alkoxides, commonly used in "Chimie Douce" to form porous silica gel, release by-products which are often cytotoxic. However by controlling the formation of gels from aqueous silica precursors and silica nanoparticles acting as "cements" one can significantly enhance the life span of the entrapped organelles and cells. Adapted characteristic techniques have shown survival times of up to 5 months with the photosynthetic production of oxygen recorded as much as 17 weeks post immobilisation. These results constitute a significant advance towards the final goal, long-lasting semi-artificial photobioreactors that can advantageously exploit solar radiation to convert polluting carbon dioxide into useful biofuels, sugars or medical metabolites.

Template-free synthesis of renewable macroporous carbon via yeast cells for high-performance supercapacitor electrode materials.

PubMed

Sun, Hongmei; He, Wenhui; Zong, Chenghua; Lu, Lehui

2013-03-01

The urgent need for sustainable development has forced material scientists to explore novel materials for next-generation energy storage devices through a green and facile strategy. In this context, yeast, which is a large group of single cell fungi widely distributed in nature environments, will be an ideal candidate for developing effective electrode materials with fascinating structures for high-performance supercapacitors. With this in mind, herein, we present the first example of creating three-dimensional (3D) interpenetrating macroporous carbon materials via a template-free method, using the green, renewable, and widespread yeast cells as the precursors. Remarkably, when the as-prepared materials are used as the electrode materials for supercapacitors, they exhibit outstanding performance with high specific capacitance of 330 F g(-1) at a current density of 1 A g(-1), and good stability, even after 1000 charge/discharge cycles. The approach developed in this work provides a new view of making full use of sustainable resources endowed by nature, opening the avenue to designing and producing robust materials with great promising applications in high-performance energy-storage devices.

Solid-phase materials for chelating metal ions and methods of making and using same

DOEpatents

Harrup, Mason K.; Wey, John E.; Peterson, Eric S.

2003-06-10

A solid material for recovering metal ions from aqueous streams, and methods of making and using the solid material, are disclosed. The solid material is made by covalently bonding a chelating agent to a silica-based solid, or in-situ condensing ceramic precursors along with the chelating agent to accomplish the covalent bonding. The chelating agent preferably comprises a oxime type chelating head, preferably a salicylaldoxime-type molecule, with an organic tail covalently bonded to the head. The hydrocarbon tail includes a carbon-carbon double bond, which is instrumental in the step of covalently bonding the tail to the silica-based solid or the in-situ condensation. The invented solid material may be contacted directly with aqueous streams containing metal ions, and is selective to ions such as copper (II) even in the presence of such ions as iron (III) and other materials that are present in earthen materials. The solid material with high selectivity to copper may be used to recover copper from mining and plating industry streams, to replace the costly and toxic solvent extraction steps of conventional copper processing.

The structure and properties of the carbon non-wovens modified with bioactive nanoceramics for medical applications.

PubMed

Fraczek-Szczypta, A; Rabiej, S; Szparaga, G; Pabjanczyk-Wlazlo, E; Krol, P; Brzezinska, M; Blazewicz, S; Bogun, M

2015-06-01

The paper presents the results of the manufacture of carbon fibers (CF) from polyacrylonitrile fiber precursor containing bioactive ceramic nanoparticles. In order to modify the precursor fibers two types of bio-glasses and wollastonite in the form of nanoparticles were used. The processing variables of the thermal conversion of polyacrylonitrile (PAN) precursor fibers into carbon fibers were determined using the FTIR method. The carbonization process of oxidized PAN fibers was carried out up to 1000°C. The carbon fibers were characterized by a low ordered crystalline structure. The bioactivity tests of carbon fibers modified with a ceramic nanocomponent carried out in the artificial serum (SBF) revealed the apatite precipitation on the fibers' surfaces. Copyright © 2015 Elsevier B.V. All rights reserved.

Method for fabricating light weight carbon-bonded carbon fiber composites

DOEpatents

Wrenn, Jr., George E.; Abbatiello, Leonard A.; Lewis, Jr., John

1989-01-01

Ultralight carbon-bonded carbon fiber composites of densities in the range of about 0.04 to 0.10 grams per cubic centimeter are fabricated by forming an aqueous slurry of carbonaceous fibers which include carbonized fibers and 0-50 weight percent fugitive fibers and a particulate thermosetting resin precursor. The slurry is brought into contact with a perforated mandrel and the water is drained from the slurry through the perforations at a controlled flow rate of about 0.03 to 0.30 liters per minutes per square inch of mandrel surface. The deposited billet of fibers and resin precursor is heated to cure the resin precursor to bind the fibers together, removed from the mandrel, and then the resin and fugitive fibers, if any, are carbonized.

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.

Refractory Oxidative-Resistant Ceramic Carbon Insulation

NASA Technical Reports Server (NTRS)

Leiser, Daniel B. (Inventor); Hsu, Ming-Ta S. (Inventor); Chen, Timothy S. (Inventor)

2001-01-01

High-temperature, lightweight, ceramic carbon insulation is prepared by coating or impregnating a porous carbon substrate with a siloxane gel derived from the reaction of an organodialkoxy silane and an organotrialkoxy silane in an acid or base medium in the presence of the carbon substrate. The siloxane gel is subsequently dried on the carbon substrate to form a ceramic carbon precursor. The carbon precursor is pyrolyzed, in an inert atmosphere, to form the ceramic insulation containing carbon, silicon, and oxygen. The carbon insulation is characterized as a porous, fibrous, carbon ceramic tile which is particularly useful as lightweight tiles for spacecraft.

Biomass derived nitrogen-doped hierarchical porous carbon sheets for supercapacitors with high performance.

PubMed

Wang, Cunjing; Wu, Dapeng; Wang, Hongju; Gao, Zhiyong; Xu, Fang; Jiang, Kai

2018-08-01

A facile potassium chloride salt-locking technique combined with hydrothermal treatment on precursors was explored to prepare nitrogen-doped hierarchical porous carbon sheets in air from biomass. Benefiting from the effective synthesis strategy, the as-obtained carbon possesses a unique nitrogen-doped thin carbon sheet structure with abundant hierarchical pores and large specific surface areas of 1459 m 2  g -1 . The doped nitrogen in carbon framework has a positive effect on the electrochemical properties of the electrode material, the thin carbon sheet structure benefits for fast ion transfer, the abundant meso-pores provide convenient channels for rapid charge transportation, large specific surface area and lots of micro-pores guarantee sufficient ion-storage sites. Therefore, applied for supercapacitors, the carbon electrode material exhibits an outstanding specific capacitance of 451 F g -1 at 0.5 A g -1 in a three-electrode system. Moreover, the assembled symmetric supercapacitor based on two identical carbon electrodes also displays high specific capacitance of 309 F g -1 at 0.5 A g -1 , excellent rate capacity and remarkable cycling stability with 99.3% of the initial capacitance retention after 10,000 cycles at 5 A -1 . The synthesis strategy avoids expensive inert gas protection and the use of corrosive KOH and toxic ZnCl 2 activated reagents, representing a promising green route to design advanced carbon electrode materials from biomass for high-capacity supercapacitors. Copyright © 2018. Published by Elsevier Inc.

Laboratory Experiments on the Low-temperature Formation of Carbonaceous Grains in the ISM

NASA Astrophysics Data System (ADS)

Fulvio, Daniele; Góbi, Sándor; Jäger, Cornelia; Kereszturi, Ákos; Henning, Thomas

2017-11-01

The life cycle of cosmic dust grains is far from being understood and the origin and evolution of interstellar medium (ISM) grains is still under debate. In the ISM, the cosmic dust destruction rate is faster than the production rate by stellar sources. However, observations of ISM refractory matter suggest that to maintain a steady amount of cosmic grains, some supplementary production mechanism takes place. In this context, we aimed to study possible reformation mechanisms of cosmic grains taking place at low temperature directly in the ISM. The low-temperature condensation of carbonaceous materials has been investigated in experiments mimicking the ISM conditions. Gas-phase carbonaceous precursors created by laser ablation of graphite were forced to accrete on cold substrates (T ≈ 10 K) representing surviving dust grains. The growing and evolution of the condensing carbonaceous precursors have been monitored by MIR and UV spectroscopy under a number of experimental scenarios. For the first time, the possibility to form ISM carbonaceous grains in situ is demonstrated. The condensation process is governed by carbon chains that first condense into small carbon clusters and finally into more stable carbonaceous materials, of which structural characteristics are comparable to the material formed in gas-phase condensation experiments at very high temperature. We also show that the so-formed fullerene-like carbonaceous material is transformed into a more ordered material under VUV processing. The cold condensation mechanisms discussed here can give fundamental clues to fully understand the balance between the timescale for dust injection, destruction, and reformation in the ISM.

Air-tolerant Fabrication and Enhanced Thermoelectric Performance of n-Type Single-walled Carbon Nanotubes Encapsulating 1,1'-Bis(diphenylphosphino)ferrocene.

PubMed

Nonoguchi, Yoshiyuki; Iihara, Yu; Ohashi, Kenji; Murayama, Tomoko; Kawai, Tsuyoshi

2016-09-06

The thermally-triggered n-type doping of single-walled carbon nanotubes is demonstrated using 1,1'-bis(diphenylphosphino)ferrocene, a novel n-type dopant. Through a simple thermal vacuum process, the phosphine compounds are moderately encapsulated inside single-walled carbon nanotubes. The encapsulation into SWNTs is carefully characterized using Raman/X-ray spectroscopy and transmission electron microscopy. This easy-to-handle doping with air-stable precursors for n-type SWNTs enables the large-scale fabrication of thermoelectric materials showing an excellent power factor exceeding approximately 240 μW mK(-2) . © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Boosting ORR Catalytic Activity by Integrating Pyridine-N Dopants, a High Degree of Graphitization, and Hierarchical Pores into a MOF-Derived N-Doped Carbon in a Tandem Synthesis.

PubMed

Liu, Dandan; Li, Liangjun; Xu, Huanfei; Dai, Pengcheng; Wang, Ying; Gu, Xin; Yan, Liting; Zhao, Guoming; Zhao, Xuebo

2018-05-18

N-doped carbon materials represent promising metal-free electrocatalysts for the oxygen reduction reaction (ORR), the cathode reaction in fuel cells, metal-air batteries, and so on. A challenge for optimizing the ORR catalytic activities of these electrocatalysts is to tune their local structures and chemical compositions in a rational and controlled way that can achieve the synergistic function of each factor. Herein, we report a tandem synthetic strategy that integrates multiple contributing factors into an N-doped carbon. With an N-containing MOF (ZIF-8) as the precursor, carbonization at higher temperatures leads to a higher degree of graphitization. Subsequent NH 3 etching of this highly graphitic carbon enabled the introduction of a higher content of pyridine-N sites and higher porosity. By optimizing these three factors, the resultant carbon materials displayed ORR activity that was far superior to that of carbon derived from a one-step pyrolysis. The onset potential of 0.955 V versus a reversible hydrogen electrode (RHE) and the half-wave potential of 0.835 V versus RHE are among the top ranks of metal-free ORR catalysts and are comparable to commercial Pt/C (20 wt %) catalysts. Kinetic studies revealed lower H 2 O 2 yields, higher electron-transfer numbers, and lower Tafel slopes for these carbon materials compared with that derived from a one-step carbonization. These findings verify the effectiveness of this tandem synthetic strategy to enhance the ORR activity of N-doped carbon materials. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Magneto-carbonization method for production of carbon fiber, and high performance carbon fibers made thereby

DOEpatents

Naskar, Amit K.; Ozcan, Soydan; Eberle, Claude C.; Abdallah, Mohamed Gabr; Mackiewicz, Ludtka Gail; Ludtka, Gerard Michael; Paulauskas, Felix Leonard; Rivard, John Daniel Kennedy

2017-08-08

Method for the preparation of carbon fiber from fiber precursor, wherein the fiber precursor is subjected to a magnetic field of at least 3 Tesla during a carbonization process. The carbonization process is generally conducted at a temperature of at least 400.degree. C. and less than 2200.degree. C., wherein, in particular embodiments, the carbonization process includes a low temperature carbonization step conducted at a temperature of at least or above 400.degree. C. or 500.degree. C. and less than or up to 1000.degree. C., 1100.degree. C., or 1200.degree. C., followed by a high temperature carbonization step conducted at a temperature of at least or above 1200.degree. C. In particular embodiments, particularly in the case of a polyacrylonitrile (PAN) fiber precursor, the resulting carbon fiber may possess a minimum tensile strength of at least 600 ksi, a tensile modulus of at least 30 Msi, and an ultimate elongation of at least 1.5%.

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.

Structural and adsorptive properties of activated carbons prepared by carbonization and activation of resins.

PubMed

Leboda, R; Skubiszewska-Zieba, J; Tomaszewski, W; Gun'ko, V M

2003-07-15

Four activated carbons (S1-S4) possessing different structural characteristics were prepared by carbonization of commercial resins (used for ion exchange) and subsequent activation. Their textural parameters were determined on the basis of nitrogen adsorption-desorption at 77.4 K, analyzed by applying several local and overall adsorption isotherm equations. The nature of carbon surface functionalities was analyzed by FTIR spectroscopy. The GC and solid-phase extraction (SPE) techniques were applied to study the influence of the texture of carbonaceous materials on their adsorptive properties. The adsorption efficiency of synthesized carbons with respect to alkylhalides used as probe compounds in the GC measurements varied over a range from 28% (C(2)H(3)Cl(3)/S2) to 85% (CHBr(3)/S1) depending on the type of adsorbates and adsorbents. The concentrating efficiency of these carbons in SPE of explosive materials changed over a larger range from 12% (trinitroglycerin/S4) and 13% (trinitrotoluene/S2) up to 100% (octogen/S1). Active carbon prepared using Zerolite 225x8 as a precursor demonstrated better results than other carbons in two types of adsorption with average values of the efficiency of 75.4% for explosives and 60.8% for alkylhalides.

Photoconductivity of Activated Carbon Fibers

DOE R&D Accomplishments Database

Kuriyama, K.; Dresselhaus, M. S.

1990-08-01

The photoconductivity is measured on a high-surface-area disordered carbon material, namely activated carbon fibers, to investigate their electronic properties. Measurements of decay time, recombination kinetics and temperature dependence of the photoconductivity generally reflect the electronic properties of a material. The material studied in this paper is a highly disordered carbon derived from a phenolic precursor, having a huge specific surface area of 1000--2000m{sup 2}/g. Our preliminary thermopower measurements suggest that this carbon material is a p-type semiconductor with an amorphous-like microstructure. The intrinsic electrical conductivity, on the order of 20S/cm at room temperature, increases with increasing temperature in the range 30--290K. In contrast with the intrinsic conductivity, the photoconductivity in vacuum decreases with increasing temperature. The recombination kinetics changes from a monomolecular process at room temperature to a biomolecular process at low temperatures. The observed decay time of the photoconductivity is {approx equal}0.3sec. The magnitude of the photoconductive signal was reduced by a factor of ten when the sample was exposed to air. The intrinsic carrier density and the activation energy for conduction are estimated to be {approx equal}10{sup 21}/cm{sup 3} and {approx equal}20meV, respectively. The majority of the induced photocarriers and of the intrinsic carriers are trapped, resulting in the long decay time of the photoconductivity and the positive temperature dependence of the conductivity.

Carbon-Nanodot Solar Cells from Renewable Precursors.

PubMed

Marinovic, Adam; Kiat, Lim S; Dunn, Steve; Titirici, Maria-Magdalena; Briscoe, Joe

2017-03-09

It has recently been shown that waste biomass can be converted into a wide range of functional materials, including those with desirable optical and electronic properties, offering the opportunity to find new uses for these renewable resources. Photovoltaics is one area in which finding the combination of abundant, low-cost and non-toxic materials with the necessary functionality can be challenging. In this paper the performance of carbon nanodots derived from a wide range of biomaterials obtained from different biomass sources as sensitisers for TiO 2 -based nanostructured solar cells was compared; polysaccharides (chitosan and chitin), monosaccharide (d-glucose), amino acids (l-arginine and l-cysteine) and raw lobster shells were used to produce carbon nanodots through hydrothermal carbonisation. The highest solar power conversion efficiency (PCE) of 0.36 % was obtained by using l-arginine carbon nanodots as sensitisers, whereas lobster shells, as a model source of chitin from actual food waste, showed a PCE of 0.22 %. By comparing this wide range of materials, the performance of the solar cells was correlated with the materials characteristics by carefully investigating the structural and optical properties of each family of carbon nanodots, and it was shown that the combination of amine and carboxylic acid functionalisation is particularly beneficial for the solar-cell performance. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

I. Synthesis, characterization, and base catalysis of novel zeolite supported super-basic materials II. Oxidative dehydrogenation of ethane over reduced heteropolyanion catalysts

NASA Astrophysics Data System (ADS)

Galownia, Jonathan M.

This thesis is composed of two separate and unrelated projects. The first part of this thesis outlines an investigation into the synthesis and characterization of a novel zeolite supported super-base capable of carbon-carbon olefin addition to alkyl aromatics. A zeolite supported basic material capable of such reactions would benefit many fine chemical syntheses, as well as vastly improve the economics associated with production of the high performance thermoplastic polyester polyethylene naphthalate. The thermal decomposition of alkali---metal azides impregnated in zeolite X is investigated as a novel route to the synthesis of a zeolite supported super-base. Impregnation of the alkali---metal azide precursor is shown to result in azide species occluded within the pores of the zeolite support by using high speed, solid-state 23Na MAS and 2D MQMAS NMR, FTIR, and TGA characterization methods. Addition of alkali---metal azides to the zeolite results in redistribution of the extra-lattice cations in the zeolite framework. Thermal decomposition of impregnated azide species produces further cation redistribution, but no neutral metallic clusters are detected by high speed, solid-state 23Na MAS NMR following thermal activation of the materials. Instead, it is possible that inactive ionic clusters are formed. The thermally activated materials do not promote base catalysis for the isomerization of 1-butene, the ethylation of toluene and o-xylene, and the alkenylation of o-xylene with 1,3-butadiene to produce 5-ortho-tolyl-pent-2-ene (5-OTP). The lack of catalytic activity in the materials is attributed to failure of the materials to form neutral metallic clusters during thermal treatment, possibly due to preferential formation of NMR silent ionic clusters. The formation of neutral metallic clusters is found to be insensitive to synthesis technique and activation procedure. It is concluded that the impregnation of alkali---metal azides in zeolite X does not provide a reliable precursor for the formation of zeolite supported super-basic materials. The second part of this thesis describes the oxidative dehydrogenation of ethane over partially reduced heteropolyanions. Niobium and pyridine exchanged salts of phosphomolybdic (NbPMo12Pyr) and phosphovanadomolybdic (NbPMo11VPyr) acids are investigated as catalyst precursors to prepare materials for catalyzing the oxidative dehydrogenation of ethane to ethylene and acetic acid at atmospheric pressure. The effects of feed composition, steam flow, temperature, and precursor composition on catalytic activity and selectivity are presented for both ethane and ethylene oxidation. Production of ethylene and acetic acid from ethane using the catalytic materials exceeds that reported in the literature for Mo-V-Nb-Ox systems under atmospheric or elevated pressure. Production of acetic acid from ethylene is also greater than that observed for Mo-V-Nb-Ox systems. Addition of vanadium reduces catalytic activity and selectivity to both ethylene and acetic acid while niobium is essential for the formation of acetic acid from ethane. Other metals such as antimony, iron, and gallium do not provide the same beneficial effect as niobium. Molybdenum in close proximity to niobium is the active site for ethane activation while niobium is directly involved in the transformation of ethylene to acetic acid. A balance of niobium and protonated pyridine is required to produce an active catalyst. Water is found to aid in desorption of acetic acid, thereby limiting deep oxidation to carbon oxides. A reaction scheme is proposed for the production of acetic acid from ethane over the catalytic materials.

Effect of oxygen and hydrogen on microstructure of pyrolytic carbon deposited from thermal decomposition of methane and ethanol

NASA Astrophysics Data System (ADS)

Ren, Biyun; Zhang, Shouyang; He, LiQun; Gu, Shengyue

2018-05-01

Chemical vapor infiltration (CVI) is the most extensive industrial preparation of carbon/carbon (C/C) composites. Precursor affects the CVI process considerably. In the present study, using carbon fiber bundles as preforms, methane and ethanol as precursors, the C/C composites were densified by decomposition of various gases in CVI. The thickness and texture of deposited pyrolytic carbon (PyC) were characterized by polarized light microscopy (PLM). The microstructure of PyC was analyzed by Raman spectroscopy. The morphologies of PyC were characterized by scanning electron microscopy (SEM). The composition of PyC was detected by X-ray photoelectron spectroscopy (XPS). Adding hydrogen in methane precursor resulted in a sharp decrease in the deposition rate and texture of PyC. Mixture of methane and ethanol as the precursor improved the deposition rate and texture remarkably. Besides, O element in ethanol was not remained as a constitution of PyC, and it was removed before the formation of PyC.

Metalorganic Chemical Vapor Deposition of Ruthenium-Doped Diamond like Carbon Films

NASA Technical Reports Server (NTRS)

Sunkara, M. K.; Ueno, M.; Lian, G.; Dickey, E. C.

2001-01-01

We investigated metalorganic precursor deposition using a Microwave Electron Cyclotron Resonance (ECR) plasma for depositing metal-doped diamondlike carbon films. Specifically, the deposition of ruthenium doped diamondlike carbon films was investigated using the decomposition of a novel ruthenium precursor, Bis(ethylcyclopentadienyl)-ruthenium (Ru(C5H4C2H5)2). The ruthenium precursor was introduced close to the substrate stage. The substrate was independently biased using an applied RF power. Films were characterized using Fourier Transform Infrared Spectroscopy (FTIR), Transmission Electron Microscopy (TEM) and Four Point Probe. The conductivity of the films deposited using ruthenium precursor showed strong dependency on the deposition parameters such as pressure. Ruthenium doped sample showed the presence of diamond crystallites with an average size of approx. 3 nm while un-doped diamondlike carbon sample showed the presence of diamond crystallites with an average size of 11 nm. TEM results showed that ruthenium was atomically dispersed within the amorphous carbon network in the films.

Facile Control of the Porous Structure of Larch-Derived Mesoporous Carbons via Self-Assembly for Supercapacitors

PubMed Central

Zhao, Xin; Li, Wei; Chen, Honglei; Wang, Shoujuan; Kong, Fangong; Liu, Shouxin

2017-01-01

Mesoporous carbons have been successfully synthesized via self-assembly using larch-based resins as precursors and triblock copolymers as soft templates. The porous structure of mesoporous carbons can be tailored by adjusting the ratio of hydrophilic/hydrophobic (EO/PO) units owing to interfacial curvature. Interestingly, the porous structures show a distinct change from vortex-like to worm-like pores, to stripe-like pores, and to ordered two-dimensional hexagonal pores as the ratio of hydrophilic/hydrophobic units increases, indicating the significant effect of EO/PO ratio on the porous structure. The mesoporous carbons as supercapacitor electrodes exhibit superior electrochemical capacitive performance and a high degree of reversibility after 2000 cycles for supercapacitors due to the well-defined mesoporosity of the carbon materials. Meanwhile, the superior carbon has a high specific capacitance of 107 F·g−1 in 6 M KOH at a current density of 10 A·g−1. PMID:29156641

Facile Control of the Porous Structure of Larch-Derived Mesoporous Carbons via Self-Assembly for Supercapacitors.

PubMed

Zhao, Xin; Li, Wei; Chen, Honglei; Wang, Shoujuan; Kong, Fangong; Liu, Shouxin

2017-11-20

Mesoporous carbons have been successfully synthesized via self-assembly using larch-based resins as precursors and triblock copolymers as soft templates. The porous structure of mesoporous carbons can be tailored by adjusting the ratio of hydrophilic/hydrophobic (EO/PO) units owing to interfacial curvature. Interestingly, the porous structures show a distinct change from vortex-like to worm-like pores, to stripe-like pores, and to ordered two-dimensional hexagonal pores as the ratio of hydrophilic/hydrophobic units increases, indicating the significant effect of EO/PO ratio on the porous structure. The mesoporous carbons as supercapacitor electrodes exhibit superior electrochemical capacitive performance and a high degree of reversibility after 2000 cycles for supercapacitors due to the well-defined mesoporosity of the carbon materials. Meanwhile, the superior carbon has a high specific capacitance of 107 F·g -1 in 6 M KOH at a current density of 10 A·g -1 .

Selective growth of palladium and titanium dioxide nanostructures inside carbon nanotube membranes

PubMed Central

2012-01-01

Hybrid nanostructured arrays based on carbon nanotubes (CNT) and palladium or titanium dioxide materials have been synthesized using self-supported and silicon-supported anodized aluminum oxide (AAO) as nanoporous template. It is well demonstrated that carbon nanotubes can be grown using these membranes and hydrocarbon precursors that decompose at temperatures closer to 600°C without the use of a metal catalyst. In this process, carbonic fragments condensate to form stacked graphitic sheets, which adopt the shape of the pores, yielding from these moulds' multi-walled carbon nanotubes. After this process, the ends of the tubes remain open and accessible to other substances, whereas the outer walls are protected by the alumina. Taking advantage of this fact, we have performed the synthesis of palladium and titanium dioxide nanostructures selectively inside carbon nanotubes using these CNT-AAO membranes as nanoreactors. PMID:22731888

Stable prenucleation mineral clusters are liquid-like ionic polymers

PubMed Central

Demichelis, Raffaella; Raiteri, Paolo; Gale, Julian D.; Quigley, David; Gebauer, Denis

2011-01-01

Calcium carbonate is an abundant substance that can be created in several mineral forms by the reaction of dissolved carbon dioxide in water with calcium ions. Through biomineralization, organisms can harness and control this process to form various functional materials that can act as anything from shells through to lenses. The early stages of calcium carbonate formation have recently attracted attention as stable prenucleation clusters have been observed, contrary to classical models. Here we show, using computer simulations combined with the analysis of experimental data, that these mineral clusters are made of an ionic polymer, composed of alternating calcium and carbonate ions, with a dynamic topology consisting of chains, branches and rings. The existence of a disordered, flexible and strongly hydrated precursor provides a basis for explaining the formation of other liquid-like amorphous states of calcium carbonate, in addition to the non-classical behaviour during growth of amorphous calcium carbonate. PMID:22186886

Wood-Derived Ultrathin Carbon Nanofiber Aerogels.

PubMed

Li, Si-Cheng; Hu, Bi-Cheng; Ding, Yan-Wei; Liang, Hai-Wei; Li, Chao; Yu, Zi-You; Wu, Zhen-Yu; Chen, Wen-Shuai; Yu, Shu-Hong

2018-06-11

Carbon aerogels with 3D networks of interconnected nanometer-sized particles exhibit fascinating physical properties and show great application potential. Efficient and sustainable methods are required to produce high-performance carbon aerogels on a large scale to boost their practical applications. An economical and sustainable method is now developed for the synthesis of ultrathin carbon nanofiber (CNF) aerogels from the wood-based nanofibrillated cellulose (NFC) aerogels via a catalytic pyrolysis process, which guarantees high carbon residual and well maintenance of the nanofibrous morphology during thermal decomposition of the NFC aerogels. The wood-derived CNF aerogels exhibit excellent electrical conductivity, a large surface area, and potential as a binder-free electrode material for supercapacitors. The results suggest great promise in developing new families of carbon aerogels based on the controlled pyrolysis of economical and sustainable nanostructured precursors. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Using Converter Dust to Produce Low Cost Cementitious Composites by in situ Carbon Nanotube and Nanofiber Synthesis

PubMed Central

Ludvig, Péter; Calixto, José M.; Ladeira, Luiz O.; Gaspar, Ivan C.P.

2011-01-01

Carbon nanotubes (CNTs) and nanofibers (CNFs) were synthesized on clinker and silica fume particles in order to create a low cost cementitious nanostructured material. The synthesis was carried out by an in situ chemical vapor deposition (CVD) process using converter dust, an industrial byproduct, as iron precursor. The use of these materials reduces the cost, with the objective of application in large-scale nanostructured cement production. The resulting products were analyzed by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA) and were found to be polydisperse in size and to have defective microstructure. Some enhancement in the mechanical behavior of cement mortars was observed due to the addition of these nano-size materials. The contribution of these CNTs/CNFs to the mechanical strength of mortar specimens is similar to that of high quality CNTs incorporated in mortars by physical mixture. PMID:28880007

Metal-Organic Framework-Templated Porous Carbon for Highly Efficient Catalysis: The Critical Role of Pyrrolic Nitrogen Species.

PubMed

Huang, Gang; Yang, Li; Ma, Xiao; Jiang, Jun; Yu, Shu-Hong; Jiang, Hai-Long

2016-03-01

Metal-free catalysts are of great importance and alternative candidates to conventional metal-based catalysts for many reactions. Herein, several types of metal-organic frameworks have been exploited as templates/precursors to afford porous carbon materials with various nitrogen dopant forms and contents, degrees of graphitization, porosities, and surface areas. Amongst these materials, the PCN-224-templated porous carbon material optimized by pyrolysis at 700 °C (denoted as PCN-224-700) is composed of amorphous carbon coated with well-defined graphene layers, offering a high surface area, hierarchical pores, and high nitrogen content (mainly, pyrrolic nitrogen species). Remarkably, as a metal-free catalyst, PCN-224-700 exhibits a low activation energy and superior activity to most metallic catalysts in the catalytic reduction of 4-nitrophenol to 4-aminophenol. Theoretical investigations suggest that the content and type of the nitrogen dopant play crucial roles in determining the catalytic performance and that the pyrrolic nitrogen species makes the dominant contribution to this activity, which explains the excellent efficiency of the PCN-224-700 catalyst well. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Highly Siderophile Elements and Osmium Isotope Systematics in Ureilites: Are the Carbonaceous Veins Primary Components?

NASA Technical Reports Server (NTRS)

Rankenburg, K.; Brandon, A. D.; Humayun, M.

2005-01-01

Ureilites are an enigmatic group of primitive carbon-bearing achondrites of ultramafic composition. The majority of the 143 ureilite meteorites consist primarily of olivine and pyroxene (and occasionally chromite) [1]. They are coarse-grained, slowly cooled, and depleted in incompatible lithophile elements. Minor amounts of dark interstitial material consisting of carbon, metal, sulfides, and fine-grained silicates occur primarily along silicate grain boundaries, but also intrude the silicates along fractures and cleavage planes. Variable degrees of impact shock features have also been imparted on ureilites. The prevailing two origins proposed for these rocks are either as melting residues of carbonaceous chondritic material [2], [3], or alternatively, derivation as mineral cumulates from such melts [4], [5], [6]. It has recently been proposed that ureilites are the residues of a smelting event, i.e. residues of a partial melting event under highly reducing conditions, where a solid Fe-bearing phase reacts with a melt and carbon to form Fe metal and carbon monoxide [7]. Rapid, localized extraction and loss of the basaltic component into space resulting from high eruption velocities could preserve unequilibrated oxygen isotopes and produce the observed olivine-pyroxene residues via 25-30% partial melting of chondritic-like precursor material.

Process for coating an object with silicon carbide

NASA Technical Reports Server (NTRS)

Levin, Harry (Inventor)

1989-01-01

A process for coating a carbon or graphite object with silicon carbide by contacting it with silicon liquid and vapor over various lengths of contact time. In the process, a stream of silicon-containing precursor material in gaseous phase below the decomposition temperature of said gas and a co-reactant, carrier or diluent gas such as hydrogen is passed through a hole within a high emissivity, thin, insulating septum into a reaction chamber above the melting point of silicon. The thin septum has one face below the decomposition temperature of the gas and an opposite face exposed to the reaction chamber. The precursor gas is decomposed directly to silicon in the reaction chamber. A stream of any decomposition gas and any unreacted precursor gas from said reaction chamber is removed. The object within the reaction chamber is then contacted with silicon, and recovered after it has been coated with silicon carbide.

TiO2-coated mesoporous carbon: conventional vs. microwave-annealing process.

PubMed

Coromelci-Pastravanu, Cristina; Ignat, Maria; Popovici, Evelini; Harabagiu, Valeria

2014-08-15

The study of coating mesoporous carbon materials with titanium oxide nanoparticles is now becoming a promising and challenging area of research. To optimize the use of carbon materials in various applications, it is necessary to attach functional groups or other nanostructures to their surface. The combination of the distinctive properties of mesoporous carbon materials and titanium oxide is expected to be applied in field emission displays, nanoelectronic devices, novel catalysts, and polymer or ceramic reinforcement. But, their synthesis is still largely based on conventional techniques, such as wet impregnation followed by chemical reduction of the metal nanoparticle precursors, which takes time and money. The thermal heating based techniques are time consuming and often lack control of particle size and morphology. Hence, since there is a growing interest in microwave technology, an alternative way of power input into chemical reactions through dielectric heating is the use of microwaves. This work is focused on the advantages of microwave-assisted synthesis of TiO2-coated mesoporous carbon over conventional thermal heating method. The reviewed studies showed that the microwave-assisted synthesis of such composites allows processes to be completed within a shorter reaction time allowing the nanoparticles formation with superior properties than that obtained by conventional method. Copyright © 2014 Elsevier B.V. All rights reserved.

Method for fabricating light weight carbon-bonded carbon fiber composites

DOEpatents

Wrenn, G.E. Jr.; Abbatiello, L.A.; Lewis, J. Jr.

1987-06-17

The invention is directed to the fabrication of ultralight carbon- bonded carbon fiber composites of densities in the range of about 0. 04 to 0.10 grams per cubic centimeter. The composites are fabricated by forming an aqueous slurry of carbonaceous fibers which include carbonized fibers and 0-50 weight percent fugitive fibers and a particulate thermosetting resin precursor. The slurry is brought into contact with a perforated mandrel and the water is drained from the slurry through the perforations at a controlled flow rate of about 0. 03 to 0.30 liters per minutes per square inch of a mandrel surface. The deposited billet of fibers and resin precursor is heated to cure the resin precursor to bind the fibers together, removed from the mandrel, and then the resin and fugitive fibers, if any, are carbonized.

Amine-pillared Nanosheet Adsorbents for CO2 Capture Applications

NASA Astrophysics Data System (ADS)

Jiang, Hui

Amine-functionalized solid adsorbents have gained attention within the last decade for their application in carbon dioxide capture, due to their many advantages such as low energy cost for regeneration, tunable structure, elimination of corrosion problems, and additional advantages. However, one of the challenges facing this technology is to accomplish both high CO 2 capture capacity along with high CO2 diffusion rates concurrently. Current amine-based solid sorbents such as porous materials similar to SBA-15 have large pores diffusion entering molecules; however, the pores become clogged upon amine inclusion. To meet this challenge, our group's solution involves the creation of a new type of material which we are calling-amino-pillared nanosheet (APN) adsorbents which are generated from layered nanosheet precursors. These materials are being proposed because of their unique lamellar structure which exhibits ability to be modified by organic or inorganic pillars through consecutive swelling and pillaring steps to form large mesoporous interlayer spaces. After the expansion of the layer space through swelling and pillaring, the large pore space can be functionalized with amine groups. This selective functionalization is possible by the choice of amine group introduced. Our choice, large amine molecules, do not access the micropore within each layer; however, either physically or chemically immobilized onto the surface of the mesoporous interlayer space between each layer. The final goal of the research is to investigate the ability to prepare APN adsorbents from a model nanoporous layered materials including nanosheets precursor material MCM-22(P) and nanoporous layered silicate material AMH-3. MCM-22(P) contains 2-dimensional porous channels, 6 membered rings (MB) openings perpendicular to the layers and 10 MB channels in the plane of the layers. However, the transport limiting openings (6 MB) to the layers is smaller than CO2 gas molecules. In contrast, AMH-3 has 3D microporous layers with 8 MB openings in the plane of the layers, as well as perpendicular to the layers, which are larger than CO2 molecules. Based on the structure differences between nanosheets precursor material MCM-22(P) and nanoporous layered silicate material AMH-3, the latter might be more suitable for CO 2 capturer application as an APN candidate material. However, none of the assumptions above have been approved experimentally. In this study, the influence of the amine loading on adsorption capacity and kinetics of adsorption for the mixed porosity material pillared MCM-22 (P) (also called MCM-36) is studied systematically, in order to determine a potential route to achieve a final material with both high amine loading and high adsorption capacity. We first synthesized MCM-22(P), followed by swelling and pillaring to create MCM-36. Polymeric amines such as polyethylenimine (PEI) are used as an organic component of the supported amine adsorbents, with varying polymer loadings within the adsorbents used. The kinetics and diffusion properties of carbon dioxide capture on a MCM-36 pillared material impregnated with amine containing Polyethylenimine polymers has been investigated. It was determined that the introduction of amine polymer cannot be used to improve the capture capacity of the support over that of the bare material, due to the fact that with the addition of a high loading of amine polymer the large pore diffusion channels become impossible for carbon dioxide molecules to diffuse through. This sets an upper limit to the capture capacity of polymer impregnated MCM-36 for carbon dioxide which does not surpass that for the initial bare material, and greatly reduces the utility of using this sort of amine-solid adsorbent for carbon capture plans in the future.

Electrical, thermal and electrochemical properties of disordered carbon prepared from palygorskite and cane molasses

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

Alvarez, Edelio Danguillecourt, E-mail: edelioalvarez42@gmail.com; Laffita, Yodalgis Mosqueda, E-mail: yodalgis@imre.uh.cu; Montoro, Luciano Andrey, E-mail: landrey.montoro@gmail.com

We have synthesized and electrochemically tested a carbon sample that was suitable as anode for lithium secondary battery. The synthesis was based on the use of the palygorskite clay as template and sugar cane molasses as carbon source. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, Brunauer–Emmett–Teller (BET) measurements and High Resolution Transmission Electron Microscope (HRTEM) analysis showed that the nanometric carbon material has a highly disordered graphene-like wrinkled structure and large specific surface area (467 m{sup 2} g{sup −1}). The compositional characterization revealed a 14% of heteroatoms-containing groups (O, H, N, S) doping the as-prepared carbon. Thermophysicalmore » measurements revealed the good thermal stability and an acceptable thermal diffusivity (9·10{sup −7} m{sup 2} s{sup −1}) and conductivity (1.1 W m{sup −1} K{sup −1}) of this carbon. The electrical properties showed an electronic conductivity of hole-like carriers of approximately one S/cm in a 173–293 K range. The testing of this material as anodes in a secondary lithium battery displayed a high specific capacity and excellent performance in terms of number of cycles. A high reversible capacity of 356 mA h g{sup −1} was reached. - Graphical abstract: TEM image and electrochemistry behavior of a new graphene oxide-like carbon. - Highlights: • A high disordered graphene oxide-like conducting carbon is reported. • The synthesis was based on palygorskite and sugar cane molasses as precursors. • The disordered conducting carbon is composed of doped- graphene heterogeneous domains. • This material combines a large specific surface area and high electric conductivity. • The thermophysical and electrochemical properties of this material reveal adequate behavior.« less

Fabrication of hierarchical porous N-doping carbon membrane by using ;confined nanospace deposition; method for supercapacitor

NASA Astrophysics Data System (ADS)

Wang, Guoxu; Liu, Meng; Du, Juan; Liu, Lei; Yu, Yifeng; Sha, Jitong; Chen, Aibing

2018-03-01

The membrane carbon materials with hierarchical porous architecture are attractive because they can provide more channels for ion transport and shorten the ions transport path. Herein, we develop a facile way based on "confined nanospace deposition" to fabricate N-dopi-ng three dimensional hierarchical porous membrane carbon material (N-THPMC) via coating the nickel nitrate, silicate oligomers and triblock copolymer P123 on the branches of commercial polyamide membrane (PAM). During high temperature treatment, the mesoporous silica layer and Ni species serve as a "confined nanospace" and catalyst respectively, which are indispensable elements for formation of carbon framework, and the gas-phase carbon precursors which derive from the decomposition of PAM are deposited into the "confined nanospace" forming carbon framework. The N-THPMC with hierarchical macro/meso/microporous structure, N-doping (2.9%) and large specific surface area (994m2 g-1) well inherits the membrane morphology and hierarchical porous structure of PAM. The N-THPMC as electrode without binder exhibits a specific capacitance of 252 F g-1 at the current density of 1 A g-1 in 6 M KOH electrolyte and excellent cycling stability of 92.7% even after 5000 cycles.

Synthesis of porous carbon/silica nanostructured microfiber with ultrahigh surface area

NASA Astrophysics Data System (ADS)

Zhou, Dan; Dong, Yan; Cui, Liru; Lin, Huiming; Qu, Fengyu

2014-12-01

Carbon/silica-nanostructured microfibers were synthesized via electrospinning method using phenol-formaldehyde resin and tetraethyl orthosilicate as carbon and silica precursor with triblock copolymer Pluronic P123 as soft template. The prepared samples show uniform microfiber structure with 1 μm in diameter and dozens of microns in length. Additionally, the mesopores in the material is about 2-6 nm. When the silica component was removed by HF, the porous carbon microfibers (PCMFs) were obtained. In addition, after the carbon/silica composites were calcined in air, the porous silica microfibers (PSiMFs) were obtained, revealing the converse porous nanostructure as PCMFs. It is a simple way to prepare PCMFs and PSiMFs with silica and carbon as the template to each other. Additionally, PCMFs possess an ultrahigh specific surface area (2,092 m2 g-1) and large pore volume. The electrochemical performance of the prepared PCMF material was investigated in 6.0 M KOH electrolyte. The PCMF electrode exhibits a high specific capacitance (252 F g-1 at 0.5 A g-1). Then, superior cycling stability (97 % retention after 4,000 cycles) mainly is due to its unique nanostructure.

Fracture in Phenolic Impregnated Carbon Ablator

NASA Technical Reports Server (NTRS)

Agrawal, Parul; Chavez-Garcia, Jose F.

2011-01-01

The thermal protection materials used for spacecraft heat shields are subjected to various thermal-mechanical loads during an atmospheric entry which can threaten the structural integrity of the system. This paper discusses the development of a novel technique to understand the failure mechanisms inside thermal protection materials. The focus of research is Phenolic Impregnated Carbon Ablator (PICA). It has successfully flown on the Stardust spacecraft and is the TPS material chosen for the Mars Science Laboratory (MSL) and Dragon spacecraft. Although PICA has good thermal properties, structurally, it is a weak material. In order to thoroughly understand failure in PICA, fracture tests were performed on FiberForm* (precursor of PICA), virgin and charred PICA materials. Several samples of these materials were tested to investigate failure mechanisms at a microstructural scale. Stress-strain data were obtained simultaneously to estimate the fracture toughness. It was found that cracks initiated and grew in the FiberForm when a critical stress limit was reached such that the carbon fibers separated from the binder. However, both for virgin and charred PICA, crack initiation and growth occurred in the matrix (phenolic) phase. Both virgin and charred PICA showed greater strength values compared to FiberForm coupons, confirming that the presence of the porous matrix helps in absorbing the fracture energy.

Synthesis, Characterization, and Electrochemical Behavior of LiMnxFe(1−x)PO4 Composites Obtained from Phenylphosphonate-Based Organic-Inorganic Hybrids

PubMed Central

Dell’Era, Alessandro; Pasquali, Mauro; Bauer, Elvira Maria; Lupi, Carla

2017-01-01

The synthesis of organic-inorganic hybrid compounds based on phenylphosphonate and their use as precursors to form LiMnxFe(1−x)PO4 composites containing carbonaceous substances with sub-micrometric morphology are presented. The experimental procedure includes the preliminary synthesis of Fe2+ and/or Mn2+ phenylphosphonates with the general formula Fe(1−x)Mnx[(C6H5PO3)(H2O)] (with 0 < x < 1), which are then mixed at different molar ratios with lithium carbonate. In this way the carbon, obtained from in situ partial oxidation of the precursor organic part, coats the LiMnxFe(1−x)PO4 particles. After a structural and morphological characterization, the electrochemical behavior of lithium iron manganese phosphates has been compared to the one of pristine LiFePO4 and LiMnPO4, in order to evaluate the doping influence on the material. PMID:29301206

Heatshield material selection for advanced ballistic reentry vehicles. [rayon fiber cloth impregnated with phenolic resin

NASA Technical Reports Server (NTRS)

Legendre, P. J.; Holtz, T.; Sikra, J. C.

1980-01-01

The Performance of staple rayon fiber and AVTEX continuous rayon fiber was evaluated as precursor materials for heatshields. The materials studied were referenced to the IRC FM5055A heatshield materials flown during the past decade. Three different arc jet facilities were used to simulate portions of the reentry environment. The IRC FM5055A and the AVTEX FM5055G, both continuous rayon fiber woven materials having the phenolic impregnant filled with carbon particles were compared. The AVTEX continuous fiber, unfilled material FM5822A was also examined to a limited extent. Test results show that the AVTEX FM5055G material provided a close substitute for the IRC FM5055A material both in terms of thermal protection and roll torque performance.

In-Situ Crafting of ZnFe₂O₄ Nanoparticles Impregnated within Continuous Carbon Network as Advanced Anode Materials.

PubMed

Jiang, Beibei; Han, Cuiping; Li, Bo; He, Yanjie; Lin, Zhiqun

2016-02-23

The ability to create a synergistic effect of nanostructure engineering and its hybridization with conductive carbonaceous material is highly desirable for attaining high-performance lithium ion batteries (LIBs). Herein, we judiciously crafted ZnFe2O4/carbon nanocomposites composed of ZnFe2O4 nanoparticles with an average size of 16 ± 5 nm encapsulated within the continuous carbon network as anode materials for LIBs. Such intriguing nanocomposites were yielded in situ via the pyrolysis-induced carbonization of polystyrene@poly(acrylic acid) (PS@PAA) core@shell nanospheres in conjunction with the formation of ZnFe2O4 nanoparticles through the thermal decomposition of ZnFe2O4 precursors incorporated within the PS@PAA nanospheres. By systematically varying the ZnFe2O4 content in the ZnFe2O4/carbon nanocomposites, the nanocomposite containing 79.3 wt % ZnFe2O4 was found to exhibit an excellent rate performance with high capacities of 1238, 1198, 1136, 1052, 926, and 521 mAh g(-1) at specific currents of 100, 200, 500, 1000, 2000, and 5000 mA g(-1), respectively. Moreover, cycling performance of the ZnFe2O4/carbon nanocomposite with 79.3 wt % ZnFe2O4 at specific currents of 200 mA g(-1) delivered an outstanding prolonged cycling stability for several hundred cycles.

Synthesis of lithium nickel cobalt manganese oxide cathode materials by infrared induction heating

NASA Astrophysics Data System (ADS)

Hsieh, Chien-Te; Chen, Yu-Fu; Pai, Chun-Ting; Mo, Chung-Yu

2014-12-01

This study adopts an in-situ infrared (IR) sintering incorporated with carbonization technique to synthesize carbon-coated LiNi1/3Co1/3Mn1/3O2 (LNCM) cathode materials for Li-ion batteries. Compared with electric resistance heating, the in-situ IR sintering is capable of rapidly producing highly-crystalline LNCM powders at 900 °C within a short period, i.e., 3 h in this case. Glucose additive is employed to serve a carbon precursor, which is carbonized and coated over the surface of LNCM crystals during the IR sintering process. The electrochemical performance of LNCM cathodes is well examined by charge-discharge cycling at 0.1-5C. An appropriate carbon coating is capable of raising discharge capacity (i.e., 181.5 mAh g-1 at 0.1C), rate capability (i.e., 75.0 mAh g-1 at 5C), and cycling stability (i.e., capacity retention: 94.2% at 1C after 50 cycles) of LNCM cathodes. This enhanced performance can be ascribed to the carbon coating onto the external surface of LNCM powders, creating an outer circuit of charge-transfer pathway and preventing cathode corrosion from direct contact to the electrolyte. Accordingly, the in-situ IR sintering technique offers a potential feasibility for synthesizing cathode materials commercially in large scale.

Composite materials formed with anchored nanostructures

DOEpatents

Seals, Roland D; Menchhofer, Paul A; Howe, Jane Y; Wang, Wei

2015-03-10

A method of forming nano-structure composite materials that have a binder material and a nanostructure fiber material is described. A precursor material may be formed using a mixture of at least one metal powder and anchored nanostructure materials. The metal powder mixture may be (a) Ni powder and (b) NiAl powder. The anchored nanostructure materials may comprise (i) NiAl powder as a support material and (ii) carbon nanotubes attached to nanoparticles adjacent to a surface of the support material. The process of forming nano-structure composite materials typically involves sintering the mixture under vacuum in a die. When Ni and NiAl are used in the metal powder mixture Ni.sub.3Al may form as the binder material after sintering. The mixture is sintered until it consolidates to form the nano-structure composite material.

Ceramic silicon-boron-carbon fibers from organic silicon-boron-polymers

NASA Technical Reports Server (NTRS)

Riccitiello, Salvatore R. (Inventor); Hsu, Ming-Ta S. (Inventor); Chen, Timothy S. (Inventor)

1993-01-01

Novel high strength ceramic fibers derived from boron, silicon, and carbon organic precursor polymers are discussed. The ceramic fibers are thermally stable up to and beyond 1200 C in air. The method of preparation of the boron-silicon-carbon fibers from a low oxygen content organosilicon boron precursor polymer of the general formula Si(R2)BR(sup 1) includes melt-spinning, crosslinking, and pyrolysis. Specifically, the crosslinked (or cured) precursor organic polymer fibers do not melt or deform during pyrolysis to form the silicon-boron-carbon ceramic fiber. These novel silicon-boron-carbon ceramic fibers are useful in high temperature applications because they retain tensile and other properties up to 1200 C, from 1200 to 1300 C, and in some cases higher than 1300 C.

Gas-solid carbonation as a current alternative origin for carbonates in Martian regolith

NASA Astrophysics Data System (ADS)

Garenne, A.; Montes-Hernandez, G.; Beck, P.; Schmitt, B.; Brissaud, O.

2011-12-01

Carbonates are abundant sedimentary minerals at the surface and sub-surface of Earth and they have been proposed as tracers of liquid water in extraterrestrial environments (e.g. at Mars surface). Its formation mechanism is since generally associated with aqueous alteration processes. Recently, carbonates minerals have been discovered on Mars surface by different orbital or rovers missions. In particular, the phoenix mission has measured from 1 to 5% of calcium carbonate (calcite type). These occurrences have been reported in area were the relative humidity is significantly high (Boynton et al., 2009). The small concentration of carbonates suggests an alternative process than carbonation in aqueous conditions. Such an observation might rather point toward a possible formation mechanism by dust-gas reaction under current Martian conditions. For this reason, in the present study, we designed an experimental setup consisting of an infrared microscope coupled to a cryogenic reaction cell (IR-CryoCell setup) in order to investigate the gas-solid carbonation of three different mineral precursors for carbonates (Ca and Mg hydroxides, and a hydrated Ca silicate formed from Ca2SiO4) at low temperature (from -10 to 25°C) and at reduced CO2 pressure (from 100 to 1000 mbar). These mineral materials are crucial precursors to form respective Ca and Mg carbonates in humid environments (0 < relative humidity < 100%) at dust-CO2 or dust-water ice-CO2 interfaces. The results have revealed a significant and fast carbonation process for Ca hydroxide and hydrated Ca silicate. Conversely, slight carbonation process was observed for Mg hydroxide. These results suggest that gas-solid carbonation process or carbonate formation at the dust-water ice-CO2 interfaces could be a currently active Mars surface process. We note that the carbonation process at low temperature (<0°C) described in the present study could also have important implications on the dust-water ice-CO2 interactions in cold terrestrial environments (e.g. Antarctic).

Facile synthesis of ultrahigh-surface-area hollow carbon nanospheres for enhanced adsorption and energy storage

PubMed Central

Xu, Fei; Tang, Zhiwei; Huang, Siqi; Chen, Luyi; Liang, Yeru; Mai, Weicong; Zhong, Hui; Fu, Ruowen; Wu, Dingcai

2015-01-01

Exceptionally large surface area and well-defined nanostructure are both critical in the field of nanoporous carbons for challenging energy and environmental issues. The pursuit of ultrahigh surface area while maintaining definite nanostructure remains a formidable challenge because extensive creation of pores will undoubtedly give rise to the damage of nanostructures, especially below 100 nm. Here we report that high surface area of up to 3,022 m2 g−1 can be achieved for hollow carbon nanospheres with an outer diameter of 69 nm by a simple carbonization procedure with carefully selected carbon precursors and carbonization conditions. The tailor-made pore structure of hollow carbon nanospheres enables target-oriented applications, as exemplified by their enhanced adsorption capability towards organic vapours, and electrochemical performances as electrodes for supercapacitors and sulphur host materials for lithium–sulphur batteries. The facile approach may open the doors for preparation of highly porous carbons with desired nanostructure for numerous applications. PMID:26072734

Electrospinning of calcium carbonate fibers and their conversion to nanocrystalline hydroxyapatite.

PubMed

Holopainen, Jani; Santala, Eero; Heikkilä, Mikko; Ritala, Mikko

2014-12-01

Calcium carbonate (CaCO3) fibers were prepared by electrospinning followed by annealing. Solutions consisting of calcium nitrate tetrahydrate (Ca(NO3)2·4H2O) and polyvinylpyrrolidone (PVP) dissolved in ethanol or 2-methoxyethanol were used for the fiber preparation. By varying the precursor concentrations in the electrospinning solutions CaCO3 fibers with average diameters from 140 to 290 nm were obtained. After calcination the fibers were identified as calcite by X-ray diffraction (XRD). The calcination process was studied in detail with high temperature X-ray diffraction (HTXRD) and thermogravimetric analysis (TGA). The initially weak fiber-to-substrate adhesion was improved by adding a strengthening CaCO3 layer by spin or dip coating Ca(NO3)2/PVP precursor solution on the CaCO3 fibers followed by annealing of the gel formed inside the fiber layer. The CaCO3 fibers were converted to nanocrystalline hydroxyapatite (HA) fibers by treatment in a dilute phosphate solution. The resulting hydroxyapatite had a plate-like crystal structure with resemblance to bone mineral. The calcium carbonate and hydroxyapatite fibers are interesting materials for bone scaffolds and bioactive coatings. Copyright © 2014 Elsevier B.V. All rights reserved.

Manganese Dioxide Supported on Porous Biomorphic Carbons as Hybrid Materials for Energy Storage Devices.

PubMed

Gutierrez-Pardo, Antonio; Lacroix, Bertrand; Martinez-Fernandez, Julian; Ramirez-Rico, Joaquin

2016-11-16

A facile and low-cost method has been employed to fabricate MnO 2 /C hybrid materials for use as binder-free electrodes for supercapacitor applications. Biocarbon monoliths were obtained through pyrolysis of beech wood, replicating the microstructure of the cellulosic precursor, and serve as 3D porous and conductive scaffolds for the direct growth of MnO 2 nanosheets by a solution method. Evaluation of the experimental results indicates that a homogeneous and uniform composite material made of a carbon matrix exhibiting ordered hierarchical porosity and MnO 2 nanosheets with a layered nanocrystalline structure is obtained. The tuning of the MnO 2 content and crystallite size via the concentration of KMnO 4 used as impregnation solution allows to obtain composites that exhibit enhanced electrochemical behavior, achieving a capacitance of 592 F g -1 in electrodes containing 3 wt % MnO 2 with an excellent cyclic stability. The electrode materials were characterized before and after electrochemical testing.

Atomically dispersed metal sites in MOF-based materials for electrocatalytic and photocatalytic energy conversion.

PubMed

Liang, Zibin; Qu, Chong; Xia, Dingguo; Zou, Ruqiang; Xu, Qiang

2018-02-19

Metal sites play an essential role for both electrocatalytic and photocatalytic energy conversion applications. The highly ordered arrangements of the organic linkers and metal nodes and the well-defined pore structures of metal-organic frameworks (MOFs) make them ideal substrates to support atomically dispersed metal sites (ADMSs) located in their metal nodes, linkers, and pores. Besides, porous carbon materials doped with ADMSs can be derived from these ADMS-incorporated MOF precursors through controlled treatments. These ADMSs incorporated in pristine MOFs and MOF-derived carbon materials possess unique merits over the molecular or the bulk metal-based catalysts, bridging the gap between homogeneous and heterogeneous catalysts for energy conversion applications. In this review, recent progress and perspective of design and incorporation of ADMSs in pristine MOFs and MOF-derived materials for energy conversion applications are highlighted, which will hopefully promote further developments of advanced MOF-based catalysts in foreseeable future. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Thermochemical Stability and Friction Properties of Soft Organosilica Networks for Solid Lubrication.

PubMed

Gonzalez Rodriguez, Pablo; Dral, A Petra; van den Nieuwenhuijzen, Karin J H; Lette, Walter; Schipper, Dik J; Ten Elshof, Johan E

2018-01-24

In view of their possible application as high temperature solid lubricants, the tribological and thermochemical properties of several organosilica networks were investigated over a range of temperatures between 25 and 580 °C. Organosilica networks, obtained from monomers with terminal and bridging organic groups, were synthesized by a sol-gel process. The influence of carbon content, crosslink density, rotational freedom of incorporated hydrocarbon groups, and network connectivity on the high temperature friction properties of the polymer was studied for condensed materials from silicon alkoxide precursors with terminating organic groups, i.e., methyltrimethoxysilane, propyltrimethoxysilane, diisopropyldimethoxysilane, cyclohexyltrimethoxysilane, phenyltrimethoxysilane and 4-biphenylyltriethoxysilane networks, as well as precursors with organic bridging groups between Si centers, i.e., 1,4-bis(triethoxysilyl)benzene and 4,4'-bis(triethoxysilyl)-1,1'-biphenyl. Pin-on-disc measurements were performed using all selected solid lubricants. It was found that materials obtained from phenyltrimethoxysilane and cyclohexyltrimethoxysilane precursors showed softening above 120 °C and performed best in terms of friction reduction, reaching friction coefficients as low as 0.01. This value is lower than that of graphite films (0.050 ± 0.005), a common bench mark for solid lubricants.

Thermochemical Stability and Friction Properties of Soft Organosilica Networks for Solid Lubrication

PubMed Central

Gonzalez Rodriguez, Pablo; van den Nieuwenhuijzen, Karin J. H.; Lette, Walter; Schipper, Dik J.

2018-01-01

In view of their possible application as high temperature solid lubricants, the tribological and thermochemical properties of several organosilica networks were investigated over a range of temperatures between 25 and 580 °C. Organosilica networks, obtained from monomers with terminal and bridging organic groups, were synthesized by a sol-gel process. The influence of carbon content, crosslink density, rotational freedom of incorporated hydrocarbon groups, and network connectivity on the high temperature friction properties of the polymer was studied for condensed materials from silicon alkoxide precursors with terminating organic groups, i.e., methyltrimethoxysilane, propyltrimethoxysilane, diisopropyldimethoxysilane, cyclohexyltrimethoxysilane, phenyltrimethoxysilane and 4-biphenylyltriethoxysilane networks, as well as precursors with organic bridging groups between Si centers, i.e., 1,4-bis(triethoxysilyl)benzene and 4,4′-bis(triethoxysilyl)-1,1′-biphenyl. Pin-on-disc measurements were performed using all selected solid lubricants. It was found that materials obtained from phenyltrimethoxysilane and cyclohexyltrimethoxysilane precursors showed softening above 120 °C and performed best in terms of friction reduction, reaching friction coefficients as low as 0.01. This value is lower than that of graphite films (0.050 ± 0.005), a common bench mark for solid lubricants. PMID:29364164

Efficient nitrogen incorporation in GaAs using novel metal organic As-N precursor di-tertiary-butyl-arsano-amine (DTBAA)

NASA Astrophysics Data System (ADS)

Sterzer, E.; Beyer, A.; Duschek, L.; Nattermann, L.; Ringler, B.; Leube, B.; Stegmüller, A.; Tonner, R.; von Hänisch, C.; Stolz, W.; Volz, K.

2016-04-01

III/V semiconductors containing small amounts of nitrogen (N; dilute nitrides) are discussed in the context of different solar cell and laser applications. The efficiency of these devices is negatively affected by carbon (C) incorporation, which comes either from the direct C-N bond in the N precursor unsymmetrical 1,1-dimethylhydrazine (UDMHy) used conventionally or from the alkyl groups of the conventional precursors for gallium (Ga), indium and arsenic (As) containing carbon. This C is incorporated together with the N due to the strength of the C-N bond. A further important issue in dilute nitride growth is the very low N incorporation efficiency in the crystal from UDMHy, which can be as little as 1% of the N supplied in the gas phase. Therefore, new metal organic chemicals have to be synthesized and their growth characteristics and suitability for dilute nitride growth have to be explored. This work presents the chemical di-tertiary-butyl-arsano-amine (DTBAA), which was synthesized, purified and tested as an N precursor for metal organic vapor phase epitaxy (MOVPE). Computational investigations show β-hydrogen and isobutane elimination to be the main reaction channel in the gas phase with high reaction barriers and absence of small fragments containing C as products. The loss of N via N2, as in UDMHy, can be excluded for unimolecular reactions of DTBAA. The Ga(NAs)/GaAs heterostructures were grown by MOVPE as initial test material and a systematic N incorporation study is presented in this paper. It is shown that high quality Ga(NAs) can be grown using DTBAA. The N incorporation was confirmed by high resolution X-ray diffraction and photoluminescence studies. All samples grown exhibit as grown room temperature photoluminescence and smooth surface morphologies. Furthermore, DTBAA shows extremely high N incorporation efficiency, which makes this molecule a very promising candidate for further research into dilute nitride material growth.

Graphitization in Carbon MEMS and Carbon NEMS

NASA Astrophysics Data System (ADS)

Sharma, Swati

Carbon MEMS (CMEMS) and Carbon NEMS (CNEMS) are an emerging class of miniaturized devices. Due to the numerous advantages such as scalable manufacturing processes, inexpensive and readily available precursor polymer materials, tunable surface properties and biocompatibility, carbon has become a preferred material for a wide variety of future sensing applications. Single suspended carbon nanowires (CNWs) integrated on CMEMS structures fabricated by electrospinning of SU8 photoresist on photolithographially patterned SU8 followed by pyrolysis are utilized for understanding the graphitization process in micro and nano carbon materials. These monolithic CNW-CMEMS structures enable the fabrication of very high aspect ratio CNWs of predefined length. The CNWs thus fabricated display core---shell structures having a graphitic shell with a glassy carbon core. The electrical conductivity of these CNWs is increased by about 100% compared to glassy carbon as a result of enhanced graphitization. We explore various tunable fabrication and pyrolysis parameters to improve graphitization in the resulting CNWs. We also suggest gas-sensing application of the thus fabricated single suspended CNW-CMEMS devices by using the CNW as a nano-hotplate for local chemical vapor deposition. In this thesis we also report on results from an optimization study of SU8 photoresist derived carbon electrodes. These electrodes were applied to the simultaneous detection of traces of Cd(II) and Pb(II) through anodic stripping voltammetry and detection limits as low as 0.7 and 0.8 microgL-1 were achieved. To further improve upon the electrochemical behavior of the carbon electrodes we elucidate a modified pyrolysis technique featuring an ultra-fast temperature ramp for obtaining bubbled porous carbon from lithographically patterned SU8. We conclude this dissertation by suggesting the possible future works on enhancing graphitization as well as on electrochemical applications

Glutamine: Precursor or nitrogen donor for citrulline synthesis?

USDA-ARS?s Scientific Manuscript database

Although glutamine is considered the main precursor for citrulline synthesis, the current literature does not differentiate between the contribution of glutamine carbon skeleton, versus nonspecific nitrogen (i.e., ammonia) and carbon derived from glutamine oxidation. To elucidate the role of glutami...

The application of pulse modulated plasma to the plasma enhanced chemical vapor deposition of dielectric materials

NASA Astrophysics Data System (ADS)

Qi, Yu

This dissertation work applied the pulse modulated plasma to the plasma enhanced chemical vapor deposition (PECVD) of two types of dielectric materials: SiO2-like coatings and Teflon-like coatings. SiO2-like coatings were firstly implemented with continuous plasma. It was proven that three different precursors: hexamethyldisiloxane (HMDSO), 1, 3, 5, 7-tetramethylcyclotetrasiloxane (TMCTS) and octamethylcyclotetrasiloxane (OMCTS) can be used to generate hard, clear and high density SiO2 deposition with coupled high growth rate and low processing temperature via PECVD. Under similar conditions, HMDSO has the lowest growth rate, lowest hardness and highest carbon content; TMCTS has the highest growth rate and hardness, and lowest carbon content; and OMCTS has moderate rates of these deposition qualities, but the best corrosion resistance. Substrate bias seems to have no effect on any deposition quality. High chamber pressure can significantly lower the carbon content in the thin films but does not affect any other qualities; the O2/precursor ratio is the most influential factor among all variables considered in this experiment. The deposition hardness and O:Si ratio always increase with this ratio while the carbon content always decreases. However, different precursors require different optimal ratios to achieve the highest growth rate. Pulse modulation was introduced into PECVD of SiO2-like coatings and OMCTS was selected as the precursor. It was demonstrated that pulse frequency, duty ratio and peak power have significant effects on deposition qualities. The proper combination of the pulse parameters and other traditional plasma parameters can significantly lower the processing temperature while retaining or even improving other deposition qualities, such as growth rate, corrosion resistance and elemental composition. Hardness is the only sacrifice of the lower time-average power caused by pulsing. Therefore, pulse modulation can effectively expand the possible range of combinations of desired deposition qualities. Finally, the pulsed plasma was used to implement PECVD of teflon-like coatings. An important discovery in this application is that in addition to pulse period, on-time and on-time peak power, the power level during the off-time is an important factor. The density of CF2 is a function of all these pulse parameters. The best result obtained is up to 67.2% CF2 and a 1.87:1 of F:C ratio when the off-time power level is ˜100--130 W the frequency is several Hz, the on-time peak power is ˜1000 W and the duty ratio is ˜7--10%.

Synthesis and Performance of Tungsten Disulfide/Carbon (WS2/C) Composite as Anode Material

NASA Astrophysics Data System (ADS)

Yuan, Zhengyong; Jiang, Qiang; Feng, Chuanqi; Chen, Xiao; Guo, Zaiping

2018-01-01

The precursors of an amorphous WS2/C composite were synthesized by a simple hydrothermal method using Na2WO4·2H2O and CH3CSNH2 as raw materials, polyethylene glycol as dispersant, and glucose as the carbon source. The as-synthesized precursors were further annealed at a low temperature in flowing argon to obtain the final materials (WS2/C composite). The structure and morphology of the WS2/C composite were characterized by x-ray diffraction, x-ray photoelectron spectroscopy, and scanning electron microscopy. The electrochemical properties were tested by galvanostatic charge/discharge testing and alternating current (AC) impedance measurements. The results show that the as-prepared amorphous WS2/C composite features both high specific capacity and good cycling performance at room temperature within the potential window from 3.0 V to 0.01 V (versus Li+/Li) at current density of 100 mAg-1. The achieved initial discharge capacity was 1080 mAhg-1, and 786 mAhg-1 was retained after 170 cycles. Furthermore, the amorphous WS2/C composite exhibited a lower charge/discharge plateau than bare WS2, which is more beneficial for use as an anode. The cyclic voltammetry and AC impedance testing further confirmed the change in the plateau and the decrease in the charge transfer resistance in the WS2/C composite. The chemical formation process and the electrochemical mechanism of the WS2/C composite are also presented. The amorphous WS2/C composite can be used as a new anode material for future applications.

Solar-Driven Hydrogen Peroxide Production Using Polymer-Supported Carbon Dots as Heterogeneous Catalyst

NASA Astrophysics Data System (ADS)

Gogoi, Satyabrat; Karak, Niranjan

2017-10-01

Safe, sustainable, and green production of hydrogen peroxide is an exciting proposition due to the role of hydrogen peroxide as a green oxidant and energy carrier for fuel cells. The current work reports the development of carbon dot-impregnated waterborne hyperbranched polyurethane as a heterogeneous photo-catalyst for solar-driven production of hydrogen peroxide. The results reveal that the carbon dots possess a suitable band-gap of 2.98 eV, which facilitates effective splitting of both water and ethanol under solar irradiation. Inclusion of the carbon dots within the eco-friendly polymeric material ensures their catalytic activity and also provides a facile route for easy catalyst separation, especially from a solubilizing medium. The overall process was performed in accordance with the principles of green chemistry using bio-based precursors and aqueous medium. This work highlights the potential of carbon dots as an effective photo-catalyst.

Mesoporous cellular-structured carbons derived from glucose-fructose syrup and their adsorption properties towards acetaminophen

NASA Astrophysics Data System (ADS)

Tzvetkov, George; Spassov, Tony; Kaneva, Nina; Tsyntsarski, Boyko

Here, a series of cellular-structured and predominantly mesoporous carbons were prepared via carbonization of glucose-fructose syrup (GFS) with sulfuric acid and subsequent calcination between 400∘C and 700∘C. Comparative results on the microstructure, chemical and textural properties of the newly produced carbons are presented. Furthermore, their adsorption performance for removal of acetaminophen from water was tested and it was found that the carbon calcined at 700∘C has a maximum adsorption capacity (98.7mgṡg-1) among all samples due to its suitable textural properties (BET surface area of 418m2ṡg-1 and total pore volume of 0.2cm3ṡg-1). This study demonstrates the potential use of GFS as a precursor in the preparation of carbonaceous materials for removal of biologically-active micropollutants from water.

Three-dimensional polypyrrole-derived carbon nanotube framework for dye adsorption and electrochemical supercapacitor

NASA Astrophysics Data System (ADS)

Xin, Shengchang; Yang, Na; Gao, Fei; Zhao, Jing; Li, Liang; Teng, Chao

2017-08-01

Three-dimensional carbon nanotube frameworks have been prepared via pyrolysis of polypyrrole nanotube aerogels that are synthesized by the simultaneous self-degraded template synthesis and hydrogel assembly followed by freeze-drying. The microstructure and composition of the materials are investigated by thermal gravimetric analysis, Raman spectrum, X-ray photoelectron spectroscopy, transmission electron microscopy, and specific surface analyzer. The results confirm the formation of three-dimensional carbon nanotube frameworks with low density, high mechanical properties, and high specific surface area. Compared with PPy aerogel precursor, the as-prepared three-dimensional carbon nanotube frameworks exhibit outstanding adsorption capacity towards organic dyes. Moreover, electrochemical tests show that the products possess high specific capacitance, good rate capability and excellent cycling performance with no capacitance loss over 1000 cycles. These characteristics collectively indicate the potential of three-dimensional polypyrrole-derived carbon nanotube framework as a promising macroscopic device for the applications in environmental and energy storages.

Synthesis of Olive-Like Nitrogen-Doped Carbon with Embedded Ge Nanoparticles for Ultrahigh Stable Lithium Battery Anodes.

PubMed

Ma, Xiaomei; Zhou, Yongning; Chen, Min; Wu, Limin

2017-05-01

The development of environment-friendly and high-performance carbon materials for energy applications has remained a great challenge. Here, a novel and facile method for synthesis of olive-like nitrogen-doped carbon embedded with germanium (Ge) nanoparticles using widespread and nontoxic dopamine as carbon and nitrogen precursors is demonstrated, especially by understanding the tendency of pure GeO 2 nanoparticles forming ellipsoidal aggregation, and the chelating reaction of the catechol structure in dopamine with metal ions. The as-synthesized Ge/N-C composites show an olive-like porous carbon structure with a loading weight of as high as 68.5% Ge nanoparticles. A lithium ion battery using Ge/N-C as the anode shows 1042 mAh g -1 charge capacity after 2000 cycles (125 d) charge/discharge at C/2 (1C = 1600 mA g -1 ) with a capacity maintaining efficiency of 99.6%, significantly exceeding those of the previously reported Ge/C-based anode materials. This prominent cyclic charge/discharge performance of the Ge/N-C anode is attributed to the well-dispersed Ge nanoparticles in graphitic N-doped carbon matrix, which facilitates high rates (0.5-15 C) of charge/discharge and increases the anode structure integrity. The synthesis strategy presented here may be a very promising approach to prepare a series of active nanoparticle-carbon hybrid materials with nitrogen doping for more and important applications. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Fabrication of nanostructured metal oxide films with supercritical carbon dioxide: Processing and applications

NASA Astrophysics Data System (ADS)

You, Eunyoung

Nanostructured metal oxide films have many applications in catalysis, microelectronics, microfluidics, photovoltaics and other fields. Since the performance of a device depends greatly on the structure of the material, the development of methodologies that enable prescriptive control of morphology are of great interest. The focus of this work is to control the structure and properties of the nanostructured metal oxide films using novel synthetic schemes in supercritical fluids and to use those films as key building components in alternative energy applications. A supercritical fluid is a substance at a temperature and pressure above its critical point. It typically exhibits gas-like transport properties and liquid-like densities. Supercritical fluid deposition (SFD) utilizes these properties of supercritical CO2 (scCO2) to deposit chemically pure metal, oxides and alloys of metal films. SFD is a chemical vapor deposition (CVD)-like process in the sense that it uses similar metal organic precursors and deposits films at elevated temperatures. Instead of vaporizing or subliming the precursors, they are dissolved in supercritical fluids. SFD has typically shown to exhibit higher precursor concentrations, lower deposition temperatures, conformal deposition of films on high aspect ratio features as compared to CVD. In2 O3, ZnO and SnO2 are attractive materials because they are used in transparent conductors. SFD of these materials were studied and In2 O3 deposition kinetics using tris(2,2,6,6-tetramethyl-3,5-heptanedionato) In (III) as precursor were determined. Growth rate dependence on the deposition temperature and the precursor concentrations were studied and the physicochemical and optical properties of In2 O3 films were characterized. Metal oxide nanochannels that can potentially be used for microfluidics have been fabricated by sequentially performing nanoimprint lithography (NIL) and SFD. NIL was used to pattern photoresist grating on substrates and SFD of TiO2 was performed thereafter. Subsequent calcination of the samples at high temperature of 400 °C revealed TiO2 nanochannels. H2-assisted-codeposition of Pt and cerium oxide using SFD was performed on porous carbon substrates for their use as anodes for direct methanol fuel cells. X-ray photoelectron analysis revealed that Pt was deposited as a pure metal and Ce was deposited as an oxide. Electrochemical analysis of a full cell revealed that an anode prepared with SFD exhibited better performance than that prepared with conventional brush-painting method. The second process that was developed is a direct spray-on technique to rapidly deposit crystalline nanoscale dendritic TiO2 onto a solid surface. This technique employs atomization of precursor solutions in supercritical fluids combined with the plasma thermal spraying. A solution of metal oxide precursor in scCO2 was expanded across a nozzle into the plasma jet where it is converted to metal oxide. We have investigated TiO2 as our model system using titanium tetra isopropoxide (Ttip) as a precursor. The film structure depends on key process variables including precursor concentration, precursor solution flow rate and plasma gun to substrate distance. The high surface area of the deposited films is attractive for applications in photovoltaics and we have fabricated dye-sensitized solar cells using these films.

Characterization of activated carbons from oil-palm shell by CO2 activation with no holding carbonization temperature.

PubMed

Herawan, S G; Hadi, M S; Ayob, Md R; Putra, A

2013-01-01

Activated carbons can be produced from different precursors, including coals of different ranks, and lignocellulosic materials, by physical or chemical activation processes. The objective of this paper is to characterize oil-palm shells, as a biomass byproduct from palm-oil mills which were converted into activated carbons by nitrogen pyrolysis followed by CO2 activation. The effects of no holding peak pyrolysis temperature on the physical characteristics of the activated carbons are studied. The BET surface area of the activated carbon is investigated using N2 adsorption at 77 K with selected temperatures of 500, 600, and 700°C. These pyrolysis conditions for preparing the activated carbons are found to yield higher BET surface area at a pyrolysis temperature of 700°C compared to selected commercial activated carbon. The activated carbons thus result in well-developed porosities and predominantly microporosities. By using this activation method, significant improvement can be obtained in the surface characteristics of the activated carbons. Thus this study shows that the preparation time can be shortened while better results of activated carbon can be produced.

Magnéli phases Ti{sub 4}O{sub 7} and Ti{sub 8}O{sub 15} and their carbon nanocomposites via the thermal decomposition-precursor route

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

Conze, S., E-mail: susan.conze@ikts.fraunhofer.de; Veremchuk, I.; Reibold, M.

2015-09-15

A new synthetic approach for producing nano-powders of the Magnéli phases Ti{sub 4}O{sub 7}, Ti{sub 8}O{sub 15} and their carbon nanocomposites by thermal decomposition-precursor route is proposed. The formation mechanism of the single-phase carbon nanocomposites (Ti{sub 4}O{sub 7}/C and Ti{sub 8}O{sub 15}/C) from metal–organic precursors is studied using FT-IR, elemental analysis, TG, STA-MS and others. The synthesis parameters and conditions were optimized to prepare the target oxides with the desired microstructure and physical properties. The electrical and transport properties of Ti{sub 4}O{sub 7}/C and Ti{sub 8}O{sub 15}/C are investigated. These nano-materials are n-type semiconductors with relatively low thermal conductivity inmore » contrast to the bulk species. The nanostructured carbon nanocomposites of Magnéli phases achieve a low thermal conductivity close to 1 W/m K at RT. The maximum ZT{sub 570} {sub °C} values are 0.04 for Ti{sub 4}O{sub 7}/C powder nanocomposite and 0.01 for Ti{sub 8}O{sub 15}/C bulk nanocomposite. - Graphical abstract: From the precursor to the produced titanium oxide pellet and its microstructure (SEM, TEM micrographs) as well as results of phase and thermoelectric analyses. - Highlights: • Magnéli phases Ti{sub 4}O{sub 7}/Ti{sub 8}O{sub 15} via thermal decomposition-precursor route is proposed. • The formation mechanism of the nanocomposites Ti{sub 4}O{sub 7}/C and Ti{sub 8}O{sub 15}/C are investigated. • Microstructure of Ti{sub 4}O{sub 7}/C and Ti{sub 8}O{sub 15}/C are examined. • The electrical and transport properties of Ti{sub 4}O{sub 7}/C and Ti{sub 8}O{sub 15}/C are investigated. • The maximum figure of mertit ZT{sub 570} {sub °C} of Ti{sub 4}O{sub 7}/C and Ti{sub 8}O{sub 15}/C are 0.01 and 0.04.« less

Prognostic investigation of galvanic corrosion precursors in aircraft structures and their detection strategy

NASA Astrophysics Data System (ADS)

James, Robin; Kim, Tae Hee; Narayanan, Ram M.

2017-04-01

Aluminum alloys have been the dominant materials for aerospace construction in the past fifty years due to their light weight, forming and alloying, and relative low cost in comparison to titanium and composites. However, in recent years, carbon fiber reinforced polymers (CFRPs) and honeycomb materials have been used in aircrafts in the quest to attain lower weight, high temperature resistance, and better fuel efficiency. When these two materials are coupled together, the structural strength of the aircraft is unparalleled, but this comes at a price, namely galvanic corrosion. Previous experimental results have shown that when CFRP composite materials are joined with high strength aluminum alloys (AA7075-T6 or AA2024-T3), galvanic corrosion occurs at the material interfaces, and the aluminum is in greater danger of corroding, particularly since carbon and aluminum are on the opposite ends of the galvanic series. In this paper, we explore the occurrence of the recognizable precursors of galvanic corrosion when CFRP plate is coupled to an aluminum alloy using SS-304 bolts and exposed to environmental degradation, which creates significant concerns for aircraft structural reliability. The galvanic corrosion software package, BEASY, is used to simulate the growth of corrosion in the designed specimen after which a microwave non-destructive testing (NDT) technique is explored to detect corrosion defects that appear at the interface of this galvanic couple. This paper also explores a loaded waveguide technique to determine the dielectric constant of the final corrosion product at the Q-band millimeter-wave frequency range (33-50 GHz), as this can be an invaluable asset in developing early detection strategies.

(GaIn)(NAs) growth using di-tertiary-butyl-arsano-amine (DTBAA)

NASA Astrophysics Data System (ADS)

Sterzer, E.; Ringler, B.; Nattermann, L.; Beyer, A.; von Hänisch, C.; Stolz, W.; Volz, K.

2017-06-01

III/V semiconductors containing small amounts of Nitrogen (N) are very interesting for a variety of optoelectronic applications. Unfortunately, the conventionally used N precursor 1,1-dimethylhydrazine (UDMHy) has an extremely low N incorporation efficiency in GaAs when grown using metal organic vapor phase epitaxy. Alloying Ga(NAs) with Indium (In) even leads to an exponential reduction of N incorporation. The huge amount of UDMHy in turn changes drastically the growth conditions. Furthermore, the application of this material is still hampered by the large carbon incorporation, most probably originating from the metal organic precursors. Hence, novel precursors for dilute nitride growth are needed. This paper will show (GaIn)(NAs) growth studies with the novel precursor di-tertiary-butyl-arsano-amine in combination with tri-ethyl-gallium and tri-methyl-indium. We show an extremely high N incorporation efficiency in the In containing (GaIn)(NAs). The (GaIn)(NAs) samples investigated in this study have been examined using high resolution X-Ray diffraction, room temperature photoluminescence and atomic force microscope measurements as well as secondary ion mass spectrometry.

Electrochemical characteristics of discrete, uniform, and monodispersed hollow mesoporous carbon spheres in double-layered supercapacitors.

PubMed

Chen, Xuecheng; Kierzek, Krzysztof; Wenelska, Karolina; Cendrowski, Krzystof; Gong, Jiang; Wen, Xin; Tang, Tao; Chu, Paul K; Mijowska, Ewa

2013-11-01

Core-shell-structured mesoporous silica spheres were prepared by using n-octadecyltrimethoxysilane (C18TMS) as the surfactant. Hollow mesoporous carbon spheres with controllable diameters were fabricated from core-shell-structured mesoporous silica sphere templates by chemical vapor deposition (CVD). By controlling the thickness of the silica shell, hollow carbon spheres (HCSs) with different diameters can be obtained. The use of ethylene as the carbon precursor in the CVD process produces the materials in a single step without the need to remove the surfactant. The mechanism of formation and the role played by the surfactant, C18TMS, are investigated. The materials have large potential in double-layer supercapacitors, and their electrochemical properties were determined. HCSs with thicker mesoporous shells possess a larger surface area, which in turn increases their electrochemical capacitance. The samples prepared at a lower temperature also exhibit increased capacitance as a result of the Brunauer-Emmett-Teller (BET) area and larger pore size. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

TRIHALOMETHANE PRECURSOR REMOVAL BY THE MAGNESIUM CARBONATE PROCESS

EPA Science Inventory

A project was conducted to determine and improve the ability of the magnesium carbonate process to remove trihalomethane (THM) precursors in treated drinking water. The project was conducted at a drinking water treatment plant in Melbourne, FL, which had been developed and instal...

Theoretical and experimental studies on silica-coated carbon spheres composites

NASA Astrophysics Data System (ADS)

Guo, Xingmei; Liu, Haixing; Shen, Yinghua; Niu, Mei; Yang, Yongzhen; Liu, Xuguang

2013-10-01

In order to prepare carbon-based photonic crystals, first of all, theoretical modeling calculation was used to predict the bandgap characteristics of silica-coated carbon spheres. Then, silica-coated carbon spheres composites were synthesized using tetraethyl orthosilicate as precursor of silica by a sol-gel method combined with Stöber method. Effect of reaction conditions on surface coating of carbon spheres with silica, including the pH, the amount of precursor and reaction time, was emphasized. The morphology and structure of the composites and the effect coating of carbon spheres with silica were characterized by field-emission scanning electron microscopy, high resolution transmission electron microscopy and Fourier-transform infrared spectrometry. The coating ratio of silica was investigated by thermogravimetry. The results show that pH value played an important role in coating reaction, the dosage of the precursor and reaction time had significant effect on coating layer thickness, that is, coating ratio. Carbon spheres coated with silica had good dispersibility and dispersion stability in water and ethanol, which is preconditions of reactivity of carbon spheres in liquid phase and lays the basis for the application of carbon spheres.

Metal/ceramic composites via infiltration of an interconnected wood-derived ceramic

NASA Astrophysics Data System (ADS)

Wilkes, Thomas E.

The use of composites is increasing as they afford scientists and engineers the ability to combine the advantageous properties of each constituent phase, e.g. metal ductility and ceramic stiffness. With respect to materials design, biomimetics is garnering increasing attention due to the complex, yet efficient, natural microstructures. One such biomimetic, or in this case 'bio-derived,' curiosity is wood-derived ceramic, which is made by either replicating or converting wood into a ceramic. The resulting porous and anisotropic material retains the precursor microstructure. The wide variety of precursors can yield materials with a range of pore sizes and distribution of pores. The purpose of this work was to study the processing, microstructure, and properties of aluminum/silicon carbide composites. The composites were made by infiltrating molten aluminum into porous wood-derived SIC, which was produced by the reactive melt-infiltration of silicon into pyrolyzed wood. The composite microstructure consisted of interconnected SiC surrounding Al-alloy 'fibers.' The strength, modulus, and toughness were measured in both longitudinal and transverse orientations. The Al → SiC load transfer was investigated with high-energy X-ray diffraction in combination with in-situ compressive loading. The properties in flexure were found to decrease with increasing temperature. Despite the complex microstructure, predictions of the composite flexural modulus and longitudinal fracture toughness were obtained using simple models: Halpin-Tsai bounds and the Ashby et al. model of the effect of ductile particle-reinforcements on the toughness of brittle materials (Ashby et al. 1989), respectively. In addition, the Al/SiC research inspired the investigation of carbon-reinforced copper composites. The goal was to explore the feasibility of making a high-thermal conductivity composite by infiltrating copper into wood-derived carbon. Results indicated that Cu/C composites could be made with pressurized infiltration, but the predicted thermal conductivity was low due to the amorphous wood-derived carbon.

Method of preparing thermal insulation for high temperature microwave sintering operations

DOEpatents

Holcombe, C.E.; Dykes, N.L.; Morrow, M.S.

1996-07-16

Superior microwave transparent thermal insulations for high temperature microwave sintering operations were prepared. One embodiment of the thermal insulation comprises granules of boron nitride coated with a very thin layer of glassy carbon made by preparing a glassy carbon precursor and blending it with boron nitride powder to form a mixture. The blended mixture is granulated to form a grit which is dried and heated to form the granules of boron nitride coated with a glassy carbon. Alternatively, grains of glassy carbon are coated with boron nitride by blending a mixture of a slurry comprising boron nitride, boric acid binder, and methyl alcohol with glassy carbon grains to form a blended mixture. The blended mixture is dried to form grains of glassy carbon coated with boron nitride. In addition, a physical mixture of boron nitride powder and glassy carbon grains has also been shown to be an excellent thermal insulation material for microwave processing and sintering. 1 fig.

Thermal insulation for high temperature microwave sintering operations and method thereof

DOEpatents

Holcombe, C.E.; Dykes, N.L.; Morrow, M.S.

1995-09-12

Superior microwave transparent thermal insulations for high temperature microwave sintering operations were prepared. One embodiment of the thermal insulation comprises granules of boron nitride coated with a very thin layer of glassy carbon made by preparing a glassy carbon precursor and blending it with boron nitride powder to form a mixture. The blended mixture is granulated to form a grit which is dried and heated to form the granules of boron nitride coated with a glassy carbon. Alternatively, grains of glassy carbon are coated with boron nitride by blending a mixture of a slurry comprising boron nitride, boric acid binder, and methyl alcohol with glassy carbon grains to form a blended mixture. The blended mixture is dried to form grains of glassy carbon coated with boron nitride. In addition, a physical mixture of boron nitride powder and glassy carbon grains has also been shown to be an excellent thermal insulation material for microwave processing and sintering. 1 fig.

Low-Temperature Fluorination of Soft-Templated Mesoporous Carbons for a High-Power Lithium/Carbon Fluoride Battery

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

Fulvio, Pasquale F.; Brown, Suree S.; Adcock, Jamie

Soft-templated mesoporous carbons and activated mesoporous carbons were fluorinated using elemental fluorine between room temperature and 235 °C. The mesoporous carbons were prepared via self-assembly synthesis of phloroglucinol–formaldehyde as a carbon precursor in the presence of triblock ethylene oxide–propylene oxide–ethylene oxide copolymer BASF Pluronic F127 as the template. The F/C ratios ranged from ~0.15 to 0.75 according to gravimetric, energy dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy analysis. Materials have mesopore diameters up to 11 nm and specific surface areas as high as 850 m² g⁻¹ after fluorination as calculated from nitrogen adsorption isotherms at -196 °C. Furthermore, the materialsmore » exhibit higher discharge potentials and energy and power densities as well as faster reaction kinetics under high current densities than commercial carbon fluorides with similar fluorine contents when tested as cathodes for Li/CF x batteries.« less

Nanopatterned carbon films with engineered morphology by direct carbonization of UV-stabilized block copolymer films.

PubMed

Wang, Yong; Liu, Jinquan; Christiansen, Silke; Kim, Dong Ha; Gösele, Ulrich; Steinhart, Martin

2008-11-01

Nanopatterned thin carbon films were prepared by direct and expeditious carbonization of the block copolymer polystyrene- block-poly(2-vinylpyridine) (PS- b-P2VP) without the necessity of slow heating to the process temperature and of addition of further carbon precursors. Carbonaceous films having an ordered "dots-on-film" surface topology were obtained from reverse micelle monolayers. The regular nanoporous morphology of PS- b-P2VP films obtained by subjecting reverse micelle monolayers to swelling-induced surface reconstruction could likewise be transferred to carbon films thus characterized by ordered nanopit arrays. Stabilization of PS- b-P2VP by UV irradiation and the concurrent carbonization of both blocks were key to the conservation of the film topography. The approach reported here may enable the realization of a broad range of nanoscaled architectures for carbonaceous materials using a block copolymer ideally suited as a template because of the pronounced repulsion between its blocks and its capability to form highly ordered microdomain structures.

All-benzene carbon nanocages: size-selective synthesis, photophysical properties, and crystal structure.

PubMed

Matsui, Katsuma; Segawa, Yasutomo; Itami, Kenichiro

2014-11-19

The design and synthesis of a series of carbon nanocages consisting solely of benzene rings are described. Carbon nanocages are appealing molecules not only because they represent junction unit structures of branched carbon nanotubes, but also because of their potential utilities as unique optoelectronic π-conjugated materials and guest-encapsulating hosts. Three sizes of strained, conjugated [n.n.n]carbon nanocages (1, n = 4; 2, n = 5; 3, n = 6) were synthesized with perfect size-selectivity. Cyclohexane-containing units and 1,3,5-trisubstituted benzene-containing units were assembled to yield the minimally strained bicyclic precursors, which were successfully converted into the corresponding carbon nanocages via acid-mediated aromatization. X-ray crystallography of 1 confirmed the cage-shaped structure with an approximately spherical void inside the cage molecule. The present studies revealed the unique properties of carbon nanocages, including strain energies, size-dependent absorption and fluorescence, as well as unique size-dependency for the electronic features of 1-3.

Modeling of the HiPco process for carbon nanotube production. I. Chemical kinetics

NASA Technical Reports Server (NTRS)

Dateo, Christopher E.; Gokcen, Tahir; Meyyappan, M.

2002-01-01

A chemical kinetic model is developed to help understand and optimize the production of single-walled carbon nanotubes via the high-pressure carbon monoxide (HiPco) process, which employs iron pentacarbonyl as the catalyst precursor and carbon monoxide as the carbon feedstock. The model separates the HiPco process into three steps, precursor decomposition, catalyst growth and evaporation, and carbon nanotube production resulting from the catalyst-enhanced disproportionation of carbon monoxide, known as the Boudouard reaction: 2 CO(g)-->C(s) + CO2(g). The resulting detailed model contains 971 species and 1948 chemical reactions. A second model with a reduced reaction set containing 14 species and 22 chemical reactions is developed on the basis of the detailed model and reproduces the chemistry of the major species. Results showing the parametric dependence of temperature, total pressure, and initial precursor partial pressures are presented, with comparison between the two models. The reduced model is more amenable to coupled reacting flow-field simulations, presented in the following article.

Controllable synthesis of mesoporous carbon nanospheres and Fe-N/carbon nanospheres as efficient oxygen reduction electrocatalysts

NASA Astrophysics Data System (ADS)

Wei, Jing; Liang, Yan; Zhang, Xinyi; Simon, George P.; Zhao, Dongyuan; Zhang, Jin; Jiang, Sanping; Wang, Huanting

2015-03-01

The synthesis of mesoporous carbon nanospheres (MCNs), especially with diameters below 200 nm remains a great challenge due to weak interactions between the carbon precursors and soft templates, as well as the uncontrollable cross-linking rate of carbon precursors. Herein, we demonstrate a simple acid-assisted, hydrothermal synthesis approach to synthesizing such uniform MCNs with well controlled diameters ranging from 20 to 150 nm under highly acidic conditions (2 M HCl). Both the carbon precursor and the template are partly protonated under such conditions and show additional Coulombic interactions with chloride ions (acts as mediators). This kind of enhanced interaction is similar to that of the ``I+X-S+'' mechanism in the synthesis of mesoporous metal oxide, which can effectively retard the cross-linking rate of resol molecules and avoid macroscopic phase separation during the hydrothermal synthesis. Due to their uniform spherical morphology, small diameter, and high surface areas, MCNs can be modified with Fe and N species via impregnation of cheap precursors (ferric nitrate and dicyandiamide), which are further converted into nonprecious electrocatalysts for oxygen reduction reactions. The resulting Fe-N/MCNs exhibit high catalytic activities, long-term stability and improved methanol tolerance under alkaline conditions, which can be potentially used in direct methanol fuel cells and metal-air batteries.The synthesis of mesoporous carbon nanospheres (MCNs), especially with diameters below 200 nm remains a great challenge due to weak interactions between the carbon precursors and soft templates, as well as the uncontrollable cross-linking rate of carbon precursors. Herein, we demonstrate a simple acid-assisted, hydrothermal synthesis approach to synthesizing such uniform MCNs with well controlled diameters ranging from 20 to 150 nm under highly acidic conditions (2 M HCl). Both the carbon precursor and the template are partly protonated under such conditions and show additional Coulombic interactions with chloride ions (acts as mediators). This kind of enhanced interaction is similar to that of the ``I+X-S+'' mechanism in the synthesis of mesoporous metal oxide, which can effectively retard the cross-linking rate of resol molecules and avoid macroscopic phase separation during the hydrothermal synthesis. Due to their uniform spherical morphology, small diameter, and high surface areas, MCNs can be modified with Fe and N species via impregnation of cheap precursors (ferric nitrate and dicyandiamide), which are further converted into nonprecious electrocatalysts for oxygen reduction reactions. The resulting Fe-N/MCNs exhibit high catalytic activities, long-term stability and improved methanol tolerance under alkaline conditions, which can be potentially used in direct methanol fuel cells and metal-air batteries. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr00331h

Detection of carbonaceous material in naga bhasma.

PubMed

Singh, S K; Rai, S B

2012-03-01

Traditional medicines have maintained their popularity in all regions of the developing world and are being adopted increasingly by people worldwide. Indian traditional system of medicine Ayurveda make use of unique metallic-herbal preparations (called Bhasma) which involves different processing steps including repeated steps of calcination of metal in the presence of natural precursor (herbal juices, decoctions, and powders, etc). It has been recently established that Bhasma contains nano/sub-micron size particles and different nutrient elements. However, the role and the end product of the raw materials, especially the herbal parts, used during the synthesis of the drug (Bhasma) is one of the important but unanswered problems in such medicinal preparations. Present work on Naga Bhasma is an attempt to understand the role of natural precursors in detail. Our results on infrared, Raman and X-ray photoelectron spectroscopy along with thermal measurements identify the presence of carbonaceous material (hydrogenated amorphous carbon) in the drug along with other compounds. In addition, this work also suggests the science and mechanism behind such complex preparations which could help in standardization of such medicines.

Highly nitrogen-doped carbon capsules: scalable preparation and high-performance applications in fuel cells and lithium ion batteries.

PubMed

Hu, Chuangang; Xiao, Ying; Zhao, Yang; Chen, Nan; Zhang, Zhipan; Cao, Minhua; Qu, Liangti

2013-04-07

Highly nitrogen-doped carbon capsules (hN-CCs) have been successfully prepared by using inexpensive melamine and glyoxal as precursors via solvothermal reaction and carbonization. With a great promise for large scale production, the hN-CCs, having large surface area and high-level nitrogen content (N/C atomic ration of ca. 13%), possess superior crossover resistance, selective activity and catalytic stability towards oxygen reduction reaction for fuel cells in alkaline medium. As a new anode material in lithium-ion battery, hN-CCs also exhibit excellent cycle performance and high rate capacity with a reversible capacity of as high as 1046 mA h g(-1) at a current density of 50 mA g(-1) after 50 cycles. These features make the hN-CCs developed in this study promising as suitable substitutes for the expensive noble metal catalysts in the next generation alkaline fuel cells, and as advanced electrode materials in lithium-ion batteries.

Isotope-Labeled Composition B for Tracing Detonation Signatures

NASA Astrophysics Data System (ADS)

Manner, Virginia; Podlesak, David; Huber, Rachel; Amato, Ronald; Giambra, Anna; Bowden, Patrick; Hartline, Ernest; Dattelbaum, Dana

2017-06-01

To better understand how solid carbon forms and evolves during detonation, we have prepared Composition B with 13 C and 15 N-labeled 1,3,5-trinitro-1,3,5-triazacyclohexane (RDX) and 2,4,6-trinitrotoluene (TNT) in order to trace the formation of soot from the carbon and nitrogen atoms in these explosives. Isotope-labeling of explosives has been performed in the recent past for a variety of reasons, including environmental remediation and reaction mechanism studies. Because it is expensive and time consuming to prepare these materials, and our detection equipment only requires trace amounts of isotopes, we have prepared fully-labeled materials and substituted them into unlabeled RDX and TNT at less than the 1% level. We will discuss the preparation and full characterization of this labeled Composition B, the detonation tests performed, along with the results of the post-detonation soot analysis. Various detonation models predict differing amounts and forms of carbon and nitrogen; these isotopically-labeled precursors have allowed these models to be tested.

Recent Development of Nanomaterial-Doped Conductive Polymers

NASA Astrophysics Data System (ADS)

Asyraf, Mohammad; Anwar, Mahmood; Sheng, Law Ming; Danquah, Michael K.

2017-12-01

Conductive polymers (CPs) have received significant research attention in material engineering for applications in microelectronics, micro-scale sensors, electromagnetic shielding, and micro actuators. Numerous research efforts have been focused on enhancing the conductivity of CPs by doping. Various conductive materials, such as metal nanoparticles and carbon-based nanoparticles, and structures, such as silver nanoparticles and graphene nanosheets, have been converted into polypyrrole and polypyrrole compounds as the precursors to developing hybrids, conjugates, or crystal nodes within the matrix to enhance the various structural properties, particularly the electrical conductivity. This article reviews nanomaterial doping of conductive polymers alongside technological advancements in the development and application of nanomaterial-doped polymeric systems. Emphasis is given to conductive nanomaterials such as nano-silver particles and carbon-based nanoparticles, graphene nano-sheets, fullerene, and carbon nanotubes (CNT) as dopants for polypyrrole-based CPs. The nature of induced electrical properties including electromagnetic absorption, electrical capacitance, and conductivities of polypyrrole systems is also discussed. The prospects and challenges associated with the development and application of CPs are also presented.

Sol-Gel Chemistry for Carbon Dots.

PubMed

Malfatti, Luca; Innocenzi, Plinio

2018-03-14

Carbon dots are an emerging class of carbon-based nanostructures produced by low-cost raw materials which exhibit a widely-tunable photoluminescence and a high quantum yield. The potential of these nanomaterials as a substitute of semiconductor quantum dots in optoelectronics and biomedicine is very high, however they need a customized chemistry to be integrated in host-guest systems or functionalized in core-shell structures. This review is focused on recent advances of the sol-gel chemistry applied to the C-dots technology. The surface modification, the fine tailoring of the chemical composition and the embedding into a complex nanostructured material are the main targets of combining sol-gel processing with C-dots chemistry. In addition, the synergistic effect of the sol-gel precursor combined with the C-dots contribute to modify the intrinsic chemo-physical properties of the dots, empowering the emission efficiency or enabling the tuning of the photoluminescence over a wide range of the visible spectrum. © 2018 The Chemical Society of Japan & Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Supercritical fluid attachment of palladium nanoparticles on aligned carbon nanotubes.

PubMed

Ye, Xiang-Rong; Lin, Yuehe; Wai, Chien M; Talbot, Jan B; Jin, Sungho

2005-06-01

Nanocomposite materials consisting of Pd nanoparticles deposited on aligned multi-walled carbon nanotubes have been fabricated through hydrogen reduction of palladium-beta-diketone precursor in supercritical carbon dioxide. The supercritical fluid processing allowed deposition of high-density Pd nanoparticles (approximately 5-10 nm) on both as-grown (unfunctionalized) and functionalized (using HNO3 oxidation) nanotubes. However, the wet processing for functionalization results in pre-agglomerated, bundle-shaped nanotubes, thus significantly reducing the effective surface area for Pd particle deposition, although the bundling provides more secure, lock-in-place positioning of nanotubes and Pd catalyst particles. The nanotube bundling is substantially mitigated by Pd nanoparticle deposition on the unfunctionalized and geometrically separated nanotubes, which provides much higher catalyst surface area. Such nanocomposite materials utilizing geometrically secured and aligned nanotubes can be useful for providing much enhanced catalytic activities to chemical and electrochemical reactions (e.g., fuel cell reactions), and eliminate the need for tedious catalyst recovery process after the reaction is completed.

Focused-electron-beam-induced processing (FEBIP) for emerging applications in carbon nanoelectronics

NASA Astrophysics Data System (ADS)

Fedorov, Andrei G.; Kim, Songkil; Henry, Mathias; Kulkarni, Dhaval; Tsukruk, Vladimir V.

2014-12-01

Focused-electron-beam-induced processing (FEBIP), a resist-free additive nanomanufacturing technique, is an actively researched method for "direct-write" processing of a wide range of structural and functional nanomaterials, with high degree of spatial and time-domain control. This article attempts to critically assess the FEBIP capabilities and unique value proposition in the context of processing of electronics materials, with a particular emphasis on emerging carbon (i.e., based on graphene and carbon nanotubes) devices and interconnect structures. One of the major hurdles in advancing the carbon-based electronic materials and device fabrication is a disjoint nature of various processing steps involved in making a functional device from the precursor graphene/CNT materials. Not only this multi-step sequence severely limits the throughput and increases the cost, but also dramatically reduces the processing reproducibility and negatively impacts the quality because of possible between-the-step contamination, especially for impurity-susceptible materials such as graphene. The FEBIP provides a unique opportunity to address many challenges of carbon nanoelectronics, especially when it is employed as part of an integrated processing environment based on multiple "beams" of energetic particles, including electrons, photons, and molecules. This avenue is promising from the applications' prospective, as such a multi-functional (electron/photon/molecule beam) enables one to define shapes (patterning), form structures (deposition/etching), and modify (cleaning/doping/annealing) properties with locally resolved control on nanoscale using the same tool without ever changing the processing environment. It thus will have a direct positive impact on enhancing functionality, improving quality and reducing fabrication costs for electronic devices, based on both conventional CMOS and emerging carbon (CNT/graphene) materials.

High capacitance of coarse-grained carbide derived carbon electrodes

DOE PAGES

Dyatkin, Boris; Gogotsi, Oleksiy; Malinovskiy, Bohdan; ...

2016-01-01

Here, we report exceptional electrochemical properties of supercapacitor electrodes composed of large, granular carbide-derived carbon (CDC) particles. We synthesized 70–250 μm sized particles with high surface area and a narrow pore size distribution, using a titanium carbide (TiC) precursor. Electrochemical cycling of these coarse-grained powders defied conventional wisdom that a small particle size is strictly required for supercapacitor electrodes and allowed high charge storage densities, rapid transport, and good rate handling ability. Moreover, the material showcased capacitance above 100 F g -1 at sweep rates as high as 250 mV s -1 in organic electrolyte. 250–1000 micron thick dense CDCmore » films with up to 80 mg cm -2 loading showed superior areal capacitances. The material significantly outperformed its activated carbon counterpart in organic electrolytes and ionic liquids. Furthermore, large internal/external surface ratio of coarse-grained carbons allowed the resulting electrodes to maintain high electrochemical stability up to 3.1 V in ionic liquid electrolyte. In addition to presenting novel insights into the electrosorption process, these coarse-grained carbons offer a pathway to low-cost, high-performance implementation of supercapacitors in automotive and grid-storage applications.« less

High capacitance of coarse-grained carbide derived carbon electrodes

NASA Astrophysics Data System (ADS)

Dyatkin, Boris; Gogotsi, Oleksiy; Malinovskiy, Bohdan; Zozulya, Yuliya; Simon, Patrice; Gogotsi, Yury

2016-02-01

We report exceptional electrochemical properties of supercapacitor electrodes composed of large, granular carbide-derived carbon (CDC) particles. Using a titanium carbide (TiC) precursor, we synthesized 70-250 μm sized particles with high surface area and a narrow pore size distribution. Electrochemical cycling of these coarse-grained powders defied conventional wisdom that a small particle size is strictly required for supercapacitor electrodes and allowed high charge storage densities, rapid transport, and good rate handling ability. The material showcased capacitance above 100 F g-1 at sweep rates as high as 250 mV s-1 in organic electrolyte. 250-1000 micron thick dense CDC films with up to 80 mg cm-2 loading showed superior areal capacitances. The material significantly outperformed its activated carbon counterpart in organic electrolytes and ionic liquids. Furthermore, large internal/external surface ratio of coarse-grained carbons allowed the resulting electrodes to maintain high electrochemical stability up to 3.1 V in ionic liquid electrolyte. In addition to presenting novel insights into the electrosorption process, these coarse-grained carbons offer a pathway to low-cost, high-performance implementation of supercapacitors in automotive and grid-storage applications.

Biomass-based palm shell activated carbon and palm shell carbon molecular sieve as gas separation adsorbents.

PubMed

Sethupathi, Sumathi; Bashir, Mohammed Jk; Akbar, Zinatizadeh Ali; Mohamed, Abdul Rahman

2015-04-01

Lignocellulosic biomass has been widely recognised as a potential low-cost source for the production of high added value materials and proved to be a good precursor for the production of activated carbons. One of such valuable biomasses used for the production of activated carbons is palm shell. Palm shell (endocarp) is an abundant by-product produced from the palm oil industries throughout tropical countries. Palm shell activated carbon and palm shell carbon molecular sieve has been widely applied in various environmental pollution control technologies, mainly owing to its high adsorption performance, well-developed porosity and low cost, leading to potential applications in gas-phase separation using adsorption processes. This mini-review represents a comprehensive overview of the palm shell activated carbon and palm shell carbon molecular sieve preparation method, physicochemical properties and feasibility of palm shell activated carbon and palm shell carbon molecular sieve in gas separation processes. Some of the limitations are outlined and suggestions for future improvements are pointed out. © The Author(s) 2015.

Synthesizing and characterization of titanium diboride for composite bipolar plates in PEM fuel cell

NASA Astrophysics Data System (ADS)

Duddukuri, Ramesh

This research deals with the synthesis and characterization of titanium diboride (TiB2) from novel carbon coated precursors. This work provides information on using different boron sources and their effect on the resulting powders of TiB2. The process has two steps in which the oxide powders were first coated with carbon by cracking of a hydrocarbon gas, propylene (C3H6) and then, mixed with boron carbide and boric acid powders in a stoichiometric ratio. These precursors were treated at temperatures in the range of 1200--1400° C for 2 h in flowing Argon atmosphere to synthesize TiB2. The process utilizes a carbothermic reduction reaction of novel carbon coated precursor that has potential of producing high-quality powders (sub-micrometer and high purity). Single phase TiB2 powders produced, were compared with commercially available titanium diboride using X-ray diffraction and Transmission electron microscopy obtained from boron carbide and boric acid containing carbon coated precursor.

Block copolymer directed one-pot simple synthesis of L10-phase FePt nanoparticles inside ordered mesoporous aluminosilicate/carbon composites.

PubMed

Kang, Eunae; Jung, Hyunok; Park, Je-Geun; Kwon, Seungchul; Shim, Jongmin; Sai, Hiroaki; Wiesner, Ulich; Kim, Jin Kon; Lee, Jinwoo

2011-02-22

A "one-pot" synthetic method was developed to produce L1(0)-phase FePt nanoparticles in ordered mesostructured aluminosilicate/carbon composites using polyisoprene-block-poly(ethylene oxide) (PI-b-PEO) as a structure-directing agent. PI-b-PEO block copolymers with aluminosilicate sols are self-assembled with a hydrophobic iron precursor (dimethylaminomethyl-ferrocene) and a hydrophobic platinum precursor (dimethyl(1,5-cyclooctadiene)platinum(II)) to obtain mesostructured composites. The as-synthesized material was heat-treated to 800 °C under an Ar/H(2) mixture (5% v/v), resulting in the formation of fct FePt nanocrystals encapsulated in ordered mesopores. By changing the quantities of the Fe and Pt precursors in the composite materials, the average particle size of the resulting fct FePt, estimated using the Debye-Scherer equation with X-ray diffraction patterns, can be easily controlled to be 2.6-10.4 nm. Using this simple synthetic method, we can extend the size of directly synthesized fct FePt up to ∼10 nm, which cannot be achieved directly in the colloidal synthetic method. All fct FePt nanoparticles show hysteresis behavior at room temperature, which indicates that ferromagnetic particles are obtained inside mesostructued channels. Well-isolated, ∼10 nm fct FePt have a coercivity of 1100 Oe at 300 K. This coercivity value is higher than values of fct FePt nanoparticles synthesized through the tedious hard template method by employing SBA-15 as a host material. The coercivity value for FePt-1 (2.6 nm) at 5 K is as high as 11 900 Oe, which is one of the largest values reported for FePt nanoparticles, or any other magnetic nanoparticles. The fct FePt nanoparticles also showed exchange-bias behavior.

Quantitative atomic-scale structure characterization of ordered mesoporous carbon materials by solid state NMR

DOE PAGES

Wang, Zhuoran; Opembe, Naftali; Kobayashi, Takeshi; ...

2018-02-03

In this study, solid-state (SS)NMR techniques were applied to characterize the atomic-scale structures of ordered mesoporous carbon (OMC) materials prepared using Pluronic F127 as template with resorcinol and formaldehyde as polymerizing precursors. A rigorous quantitative analysis was developed using a combination of 13C SSNMR spectra acquired with direct polarization and cross polarization on natural abundant and selectively 13C-enriched series of samples pyrolyzed at various temperatures. These experiments identified and counted the key functional groups present in the OMCs at various stages of preparation and thermal treatment. Lastly, the chemical evolution of molecular networks, the average sizes of aromatic clusters andmore » the extended molecular structures of OMCs were then inferred by coupling this information with the elemental analysis results.« less

Quantitative atomic-scale structure characterization of ordered mesoporous carbon materials by solid state NMR

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

Wang, Zhuoran; Opembe, Naftali; Kobayashi, Takeshi

In this study, solid-state (SS)NMR techniques were applied to characterize the atomic-scale structures of ordered mesoporous carbon (OMC) materials prepared using Pluronic F127 as template with resorcinol and formaldehyde as polymerizing precursors. A rigorous quantitative analysis was developed using a combination of 13C SSNMR spectra acquired with direct polarization and cross polarization on natural abundant and selectively 13C-enriched series of samples pyrolyzed at various temperatures. These experiments identified and counted the key functional groups present in the OMCs at various stages of preparation and thermal treatment. Lastly, the chemical evolution of molecular networks, the average sizes of aromatic clusters andmore » the extended molecular structures of OMCs were then inferred by coupling this information with the elemental analysis results.« less

Monodisperse Mesoporous Carbon Nanoparticles from Polymer/Silica Self-Aggregates and Their Electrocatalytic Activities.

PubMed

Huang, Xiaoxi; Zhou, Li-Jing; Voiry, Damien; Chhowalla, Manish; Zou, Xiaoxin; Asefa, Tewodros

2016-07-27

In our quest to make various chemical processes sustainable, the development of facile synthetic routes and inexpensive catalysts can play a central role. Herein we report the synthesis of monodisperse, polyaniline (PANI)-derived mesoporous carbon nanoparticles (PAMCs) that can serve as efficient metal-free electrocatalysts for the hydrogen peroxide reduction reaction (HPRR) as well as the oxygen reduction reaction (ORR) in fuel cells. The materials are synthesized by polymerization of aniline with the aid of (NH4)2S2O8 as oxidant and colloidal silica nanoparticles as templates, then carbonization of the resulting PANI/silica composite material at different high temperatures, and finally removal of the silica templates from the carbonized products. The PAMC materials that are synthesized under optimized synthetic conditions possess monodisperse mesoporous carbon nanoparticles with an average size of 128 ± 12 nm and an average pore size of ca. 12 nm. Compared with Co3O4, a commonly used electrocatalyst for HPRR, these materials show much better catalytic activity for this reaction. In addition, unlike Co3O4, the PAMCs remain relatively stable during the reaction, under both basic and acidic conditions. The nanoparticles also show good electrocatalytic activity toward ORR. Based on the experimental results, PAMCs' excellent electrocatalytic activity is attributed partly to their heteroatom dopants and/or intrinsic defect sites created by vacancies in their structures and partly to their high porosity and surface area. The reported synthetic method is equally applicable to other polymeric precursors (e.g., polypyrrole (PPY)), which also produces monodisperse, mesoporous carbon nanoparticles in the same way. The resulting materials are potentially useful not only for electrocatalysis of HPRR and ORR in fuel cells but also for other applications where high surface area, small sized, nanostructured carbon materials are generally useful for (e.g., adsorption, supercapacitors, etc.).

Synthesis of mesoporous carbon nanoparticles with large and tunable pore sizes

NASA Astrophysics Data System (ADS)

Liu, Chao; Yu, Meihua; Li, Yang; Li, Jiansheng; Wang, Jing; Yu, Chengzhong; Wang, Lianjun

2015-07-01

Mesoporous carbon nanoparticles (MCNs) with large and adjustable pores have been synthesized by using poly(ethylene oxide)-b-polystyrene (PEO-b-PS) as a template and resorcinol-formaldehyde (RF) as a carbon precursor. The resulting MCNs possess small diameters (100-126 nm) and high BET surface areas (up to 646 m2 g-1). By using home-designed block copolymers, the pore size of MCNs can be tuned in the range of 13-32 nm. Importantly, the pore size of 32 nm is the largest among the MCNs prepared by the soft-templating route. The formation mechanism and structure evolution of MCNs were studied by TEM and DLS measurements, based on which a soft-templating/sphere packing mechanism was proposed. Because of the large pores and small particle sizes, the resulting MCNs were excellent nano-carriers to deliver biomolecules into cancer cells. MCNs were further demonstrated with negligible toxicity. It is anticipated that this carbon material with large pores and small particle sizes may have excellent potential in drug/gene delivery.Mesoporous carbon nanoparticles (MCNs) with large and adjustable pores have been synthesized by using poly(ethylene oxide)-b-polystyrene (PEO-b-PS) as a template and resorcinol-formaldehyde (RF) as a carbon precursor. The resulting MCNs possess small diameters (100-126 nm) and high BET surface areas (up to 646 m2 g-1). By using home-designed block copolymers, the pore size of MCNs can be tuned in the range of 13-32 nm. Importantly, the pore size of 32 nm is the largest among the MCNs prepared by the soft-templating route. The formation mechanism and structure evolution of MCNs were studied by TEM and DLS measurements, based on which a soft-templating/sphere packing mechanism was proposed. Because of the large pores and small particle sizes, the resulting MCNs were excellent nano-carriers to deliver biomolecules into cancer cells. MCNs were further demonstrated with negligible toxicity. It is anticipated that this carbon material with large pores and small particle sizes may have excellent potential in drug/gene delivery. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr02389k

The production of glow precursors by oxidative erosion of spacecraft surfaces

NASA Technical Reports Server (NTRS)

Gregory, J. C.; Peters, P. N.

1985-01-01

Erosion rates of organic materials are measured during a recent flight of the shuttle (STS-8). Several forms of carbon and a variety of thermosetting and thermoplastic polymers are exposed to the ram beam of atomic oxygen. Arrhenius energies of about 1000 to 2000 cal/mole were measured from the rate dependencies on temperature. If some simple assumptions are made about the chemical nature of the desorbed species, the data can be used to estimate production rates at surfaces in orbit under different conditions of temperature, oxygen atom flux, and material surface conditions.

Methionine as a Precursor of Ethylene—Commentary

USDA-ARS?s Scientific Manuscript database

Lieberman et al. showed in a 1966 publication of Plant Physiology that methionine is a precursor of ethylene. It was the first paper that showed ethylene carbons are derived from carbons 3 and 4 of methionine. This paper catalyzed remarkable interest among plant biologists to elucidate the biosynth...

Process for producing metal compounds from graphite oxide

NASA Technical Reports Server (NTRS)

Hung, Ching-Cheh (Inventor)

2000-01-01

A process for providing elemental metals or metal oxides distributed on a carbon substrate or self-supported utilizing graphite oxide as a precursor. The graphite oxide is exposed to one or more metal chlorides to form an intermediary product comprising carbon, metal, chloride, and oxygen This intermediary product can be flier processed by direct exposure to carbonate solutions to form a second intermediary product comprising carbon, metal carbonate, and oxygen. Either intermediary product may be further processed: a) in air to produce metal oxide; b) in an inert environment to produce metal oxide on carbon substrate; c) in a reducing environment to produce elemental metal distributed on carbon substrate. The product generally takes the shape of the carbon precursor.

Process for Producing Metal Compounds from Graphite Oxide

NASA Technical Reports Server (NTRS)

Hung, Ching-Cheh (Inventor)

2000-01-01

A process for providing elemental metals or metal oxides distributed on a carbon substrate or self-supported utilizing graphite oxide as a precursor. The graphite oxide is exposed to one or more metal chlorides to form an intermediary product comprising carbon. metal. chloride. and oxygen This intermediary product can be flier processed by direct exposure to carbonate solutions to form a second intermediary product comprising carbon. metal carbonate. and oxygen. Either intermediary product may be further processed: a) in air to produce metal oxide: b) in an inert environment to produce metal oxide on carbon substrate: c) in a reducing environment. to produce elemental metal distributed on carbon substrate. The product generally takes the shape of the carbon precursor.

Bifunctional catalyst of graphite-encapsulated iron compound nanoparticle for magnetic carbon nanotubes growth by chemical vapor deposition

NASA Astrophysics Data System (ADS)

Saraswati, Teguh Endah; Prasiwi, Oktaviana Dewi Indah; Masykur, Abu; Anwar, Miftahul

2017-01-01

The carbon nanotube has widely taken great attractive in carbon nanomaterial research and application. One of its preparation methods is catalytic chemical vapor deposition (CCVD) using catalyst i.e. iron, nickel, etc. Generally, except the catalyst, carbon source gasses as the precursor are still required. Here, we report the use of the bifunctional material of Fe3O4/C which has an incorporated core/shell structures of carbon-encapsulated iron compound nanoparticles. The bifunctional catalyst was prepared by submerged arc discharge that simply performed using carbon and carbon/iron oxide electrodes in ethanol 50%. The prepared material was then used as a catalyst in thermal chemical vapor deposition at 800°C flown with ethanol vapor as the primer carbon source in a low-pressure condition. This catalyst might play a dual role as a catalyst and secondary carbon source for growing carbon nanotubes at the time. The synthesized products were characterized by transmission electron microscopy (TEM) and X-ray diffraction (XRD) analysis. The successful formation of carbon nanotubes was assigned by the shifted X-ray diffracted peak of carbon C(002), the iron oxides of Fe3O4 and γ-Fe2O3, and the other peaks which were highly considered to the other carbon allotropes with sp2 hybridization structures. The other assignment was studied by electron microscopy which successfully observed the presence of single-wall carbon nanotubes. In addition, the as-prepared carbon nanotubes have a magnetic property which was induced by the remaining of metal catalyst inside the CNT.

Recovery of silica from electronic waste for the synthesis of cubic MCM-48 and its application in preparing ordered mesoporous carbon molecular sieves using a green approach

NASA Astrophysics Data System (ADS)

Liou, Tzong-Horng

2012-07-01

The electronics industry is one of the world's fastest growing manufacturing industries. However, e-waste has become a serious pollution problem. This study reports the recovery of e-waste for preparing valuable MCM-48 and ordered mesoporous carbon for the first time. Specifically, this study adopts an alkali-extracted method to obtain sodium silicate precursors from electronic packaging resin ash. The influence of synthesis variables such as gelation pH, neutral/cationic surfactant ratio, hydrothermal treatment temperature, and calcination temperature on the mesophase of MCM-48 materials is investigated. Experimental results confirm that well-ordered cubic MCM-48 materials were synthesized in strongly acidic and strongly basic media. The resulting mesoporous silica had a high surface area of 1,317 m2/g, mean pore size of about 3.0 nm, and a high purity of 99.87 wt%. Ordered mesoporous carbon with high surface area (1,715 m2/g) and uniform pore size of CMK-1 type was successfully prepared by impregnating MCM-48 template using the resin waste. The carbon structure was sensitive to the sulfuric acid concentration and carbonization temperature. Converting e-waste into MCM-48 materials not only eliminates the disposal problem of e-waste, but also transforms industrial waste into a useful nanomaterial.

New catalysts for coal liquefaction and new nanocrystalline catalysts synthesis methods

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

Linehan, J.C.; Matson, D.W.; Darab, J.G.

1994-09-01

The use of coal as a source of transportation fuel is currently economically unfavorable due to an abundant world petroleum supply and the relatively high cost of coal liquefaction. Consequently, a reduction in the cost of coal liquefaction, for example by using less and/or less costly catalysts or lower liquefaction temperatures, must be accomplished if coal is to play an significant role as a source of liquid feedstock for the petrochemical industry. The authors and others have investigated the applicability of using inexpensive iron-based catalysts in place of more costly and environmentally hazardous metal catalysts for direct coal liquefaction. Iron-basedmore » catalysts can be effective in liquefying coal and in promoting carbon-carbon bond cleavage in model compounds. The authors have been involved in an ongoing effort to develop and optimize iron-based powders for use in coal liquefaction and related petrochemical applications. Research efforts in this area have been directed at three general areas. The authors have explored ways to optimize the effectiveness of catalyst precursor species through use of nanocrystalline materials and/or finely divided powders. In this effort, the authors have developed two new nanophase material production techniques, Modified Reverse Micelle (MRM) and the Rapid Thermal Decomposition of precursors in Solution (RTDS). A second effort has been aimed at optimizing the effectiveness of catalysts by variations in other factors. To this, the authors have investigated the effect that the crystalline phase has on the capacity of iron-based oxide and oxyhydroxide powders to be effectively converted to an active catalyst phase under liquefaction conditions. And finally, the authors have developed methods to produce active catalyst precursor powders in quantities sufficient for pilot-scale testing. Major results in these three areas are summarized.« less

High performance all-solid-state symmetric supercapacitor based on porous carbon made from a metal-organic framework compound

NASA Astrophysics Data System (ADS)

Yu, Feng; Wang, Teng; Wen, Zubiao; Wang, Hongxia

2017-10-01

In this work, we demonstrate the synthesis of porous carbon material with high specific surface area by using metal-organic framework (MOF) as precursor. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) have confirmed that the material was amorphous and consisted of nanoparticles (5-6 nm) and hierarchical distribution of pores. The characterization of the material by N2 adsorption/desorption isotherm measurement have shown that the material had a high specific surface area reaching to 2618.7 m2 g-1 and abundant porosity with pore size less than 10 nm. The investigation of the electrochemical properties of the material has shown the porous carbon electrode possessed excellent rate performance with high specific capacitances of 150.8 F g-1 at a current density of 5 A g-1, and 133.6 F g-1 at a current density of 50 A g-1, respectively. An all-solid-state symmetric supercapacitor assembled using the as-prepared porous carbon as electrodes and Na2SO4/PVA gel as an electrolyte delivered a high power density of 13 516.4 W kg-1 with an energy density of 8.26 Wh kg-1. A high energy density of 17.37 Wh kg-1 was obtained at discharge current density of 1 A g-1. In addition, the device exhibited superior cycling performance with 94.8% retention rate after 10 000 cycles at a current density of 10 A g-1.

Natural sisal fibers derived hierarchical porous activated carbon as capacitive material in lithium ion capacitor

NASA Astrophysics Data System (ADS)

Yang, Zhewei; Guo, Huajun; Li, Xinhai; Wang, Zhixing; Yan, Zhiliang; Wang, Yansen

2016-10-01

Lithium-ion capacitor (LIC) is a novel advanced electrochemical energy storage (EES) system bridging gap between lithium ion battery (LIB) and electrochemical capacitor (ECC). In this work, we report that sisal fiber activated carbon (SFAC) was synthesized by hydrothermal treatment followed by KOH activation and served as capacitive material in LIC for the first time. Different particle structure, morphology, specific surface area and heteroatoms affected the electrochemical performance of as-prepared materials and corresponding LICs. When the mass ratio of KOH to char precursor was 2, hierarchical porous structured SFAC-2 was prepared and exhibited moderate specific capacitance (103 F g-1 at 0.1 A g-1), superior rate capability and cyclic stability (88% capacity retention after 5000 cycles at 1 A g-1). The corresponding assembled LIC (LIC-SC2) with optimal comprehensive electrochemical performance, displayed the energy density of 83 Wh kg-1, the power density of 5718 W kg-1 and superior cyclic stability (92% energy density retention after 1000 cycles at 0.5 A g-1). It is worthwhile that the source for activated carbon is a natural and renewable one and the synthesis method is eco-friendly, which facilitate that hierarchical porous activated carbon has potential applications in the field of LIC and other energy storage systems.

Highly porous activated carbons from resource-recovered Leucaena leucocephala wood as capacitive deionization electrodes.

PubMed

Hou, Chia-Hung; Liu, Nei-Ling; Hsi, Hsing-Cheng

2015-12-01

Highly porous activated carbons were resource-recovered from Leucaena leucocephala (Lam.) de Wit. wood through combined chemical and physical activation (i.e., KOH etching followed by CO2 activation). This invasive species, which has severely damaged the ecological economics of Taiwan, was used as the precursor for producing high-quality carbonaceous electrodes for capacitive deionization (CDI). Carbonization and activation conditions strongly influenced the structure of chars and activated carbons. The total surface area and pore volume of activated carbons increased with increasing KOH/char ratio and activation time. Overgasification induced a substantial amount of mesopores in the activated carbons. In addition, the electrochemical properties and CDI electrosorptive performance of the activated carbons were evaluated; cyclic voltammetry and galvanostatic charge/discharge measurements revealed a typical capacitive behavior and electrical double layer formation, confirming ion electrosorption in the porous structure. The activated-carbon electrode, which possessed high surface area and both mesopores and micropores, exhibited improved capacitor characteristics and high electrosorptive performance. Highly porous activated carbons derived from waste L. leucocephala were demonstrated to be suitable CDI electrode materials. Copyright © 2015 Elsevier Ltd. All rights reserved.

Highly Enhanced Raman Scattering on Carbonized Polymer Films.

PubMed

Yoon, Jong-Chul; Hwang, Jongha; Thiyagarajan, Pradheep; Ruoff, Rodney S; Jang, Ji-Hyun

2017-06-28

We have discovered a carbonized polymer film to be a reliable and durable carbon-based substrate for carbon enhanced Raman scattering (CERS). Commercially available SU8 was spin coated and carbonized (c-SU8) to yield a film optimized to have a favorable Fermi level position for efficient charge transfer, which results in a significant Raman scattering enhancement under mild measurement conditions. A highly sensitive CERS (detection limit of 10 -8 M) that was uniform over a large area was achieved on a patterned c-SU8 film and the Raman signal intensity has remained constant for 2 years. This approach works not only for the CMOS-compatible c-SU8 film but for any carbonized film with the correct composition and Fermi level, as demonstrated with carbonized-PVA (poly(vinyl alcohol)) and carbonized-PVP (polyvinylpyrollidone) films. Our study certainly expands the rather narrow range of Raman-active material platforms to include robust carbon-based films readily obtained from polymer precursors. As it uses broadly applicable and cheap polymers, it could offer great advantages in the development of practical devices for chemical/bio analysis and sensors.

Carbon nanosheets-based supercapacitors: Design of dual redox additives of 1, 4-dihydroxyanthraquinone and hydroquinone for improved performance

NASA Astrophysics Data System (ADS)

Xu, Dong; Sun, Xiao Na; Hu, Wei; Chen, Xiang Ying

2017-07-01

Using thiocarbanilide and Mg(OH)2 powders as carbon precursor and template, respectively, novel 2D carbon nanosheets with large area have been produced. Next, based on the cooperative effect, 1, 4-dihydroxyanthraquinone (DQ) and hydroquinone (HQ) regarded as efficient dual redox additives have been incorporated into the electrode carbon material and H2SO4 electrolyte, respectively, to largely elevate the capacitive performance of supercapacitors. More importantly, the cooperative effect results from the redox processes of DQ and HQ consecutively occurring in the electrode carbon material and aqueous H2SO4 electrolyte, respectively. Besides, the molar ratio of DQ and HQ exerts a crucial role in the determination of the electrochemical behaviors and eventually the optimum condition is the mass ratio of 1:1 concerning the DQ and porous carbon within solid electrode while retaining the HQ concentration as 20 mmol L-1 in 1 mol L-1 H2SO4 electrolyte. As a result, the maximum specific capacitance is achieved of 239 F g-1 at 3 A g-1, and furthermore the maximum energy density up to 21.1 Wh kg-1 is almost 3.5 times larger than that of the one without introducing any redox additive.

Production of Cinnamic and p-Hydroxycinnamic Acids in Engineered Microbes.

PubMed

Vargas-Tah, Alejandra; Gosset, Guillermo

2015-01-01

The aromatic compounds cinnamic and p-hydroxycinnamic acids (pHCAs) are phenylpropanoids having applications as precursors for the synthesis of thermoplastics, flavoring, cosmetic, and health products. These two aromatic acids can be obtained by chemical synthesis or extraction from plant tissues. However, both manufacturing processes have shortcomings, such as the generation of toxic subproducts or a low concentration in plant material. Alternative production methods are being developed to enable the biotechnological production of cinnamic and (pHCAs) by genetically engineering various microbial hosts, including Escherichia coli, Saccharomyces cerevisiae, Pseudomonas putida, and Streptomyces lividans. The natural capacity to synthesize these aromatic acids is not existent in these microbial species. Therefore, genetic modification have been performed that include the heterologous expression of genes encoding phenylalanine ammonia-lyase and tyrosine ammonia-lyase activities, which catalyze the conversion of l-phenylalanine (l-Phe) and l-tyrosine (l-Tyr) to cinnamic acid and (pHCA), respectively. Additional host modifications include the metabolic engineering to increase carbon flow from central metabolism to the l-Phe or l-Tyr biosynthetic pathways. These strategies include the expression of feedback insensitive mutant versions of enzymes from the aromatic pathways, as well as genetic modifications to central carbon metabolism to increase biosynthetic availability of precursors phosphoenolpyruvate and erythrose-4-phosphate. These efforts have been complemented with strain optimization for the utilization of raw material, including various simple carbon sources, as well as sugar polymers and sugar mixtures derived from plant biomass. A systems biology approach to production strains characterization has been limited so far and should yield important data for future strain improvement.

Production of Cinnamic and p-Hydroxycinnamic Acids in Engineered Microbes

PubMed Central

Vargas-Tah, Alejandra; Gosset, Guillermo

2015-01-01

The aromatic compounds cinnamic and p-hydroxycinnamic acids (pHCAs) are phenylpropanoids having applications as precursors for the synthesis of thermoplastics, flavoring, cosmetic, and health products. These two aromatic acids can be obtained by chemical synthesis or extraction from plant tissues. However, both manufacturing processes have shortcomings, such as the generation of toxic subproducts or a low concentration in plant material. Alternative production methods are being developed to enable the biotechnological production of cinnamic and (pHCAs) by genetically engineering various microbial hosts, including Escherichia coli, Saccharomyces cerevisiae, Pseudomonas putida, and Streptomyces lividans. The natural capacity to synthesize these aromatic acids is not existent in these microbial species. Therefore, genetic modification have been performed that include the heterologous expression of genes encoding phenylalanine ammonia-lyase and tyrosine ammonia-lyase activities, which catalyze the conversion of l-phenylalanine (l-Phe) and l-tyrosine (l-Tyr) to cinnamic acid and (pHCA), respectively. Additional host modifications include the metabolic engineering to increase carbon flow from central metabolism to the l-Phe or l-Tyr biosynthetic pathways. These strategies include the expression of feedback insensitive mutant versions of enzymes from the aromatic pathways, as well as genetic modifications to central carbon metabolism to increase biosynthetic availability of precursors phosphoenolpyruvate and erythrose-4-phosphate. These efforts have been complemented with strain optimization for the utilization of raw material, including various simple carbon sources, as well as sugar polymers and sugar mixtures derived from plant biomass. A systems biology approach to production strains characterization has been limited so far and should yield important data for future strain improvement. PMID:26347861

Supercapacitor Electrode Materials from Highly Porous Carbon Nanofibers with Tailored Pore Distributions

NASA Astrophysics Data System (ADS)

Chathurika Abeykoon, Nimali

Environmental and human health risks associated with the traditional methods of energy production (e.g., oil and gas) and intermittency and uncertainty of renewable sources (e.g., solar and wind) have led to exploring effective and alternative energy sources to meet the growing energy demands. Electricity based on energy storage devices are the most promising solutions for realization of these objectives. Among the energy storage devices, electrochemical double layer capacitors (EDLCs) or supercapacitors have become an attractive research interest due to their outstanding performance, especially high power densities, long cycle life and rapid charge and discharge times, which enables them to utilize in many applications including consumer electronics and transportation, where high power is needed. However, low energy density of supercapacitors is a major obstacle to compete with the commercially existing high energy density energy storage device such as batteries. The fabrication of advanced electrodes materials with very high surface area from novel precursors and utilization of electrolytes with higher operating voltages are essential to enhance energy density of supercapacitors. In this work, carbon nanofibers (CNFs) from different polymer precursors with new fabrication techniques are explored to develop highly porous carbon with tailored pore distributions to match with employed ionic liquid electrolytes (which possess high working voltages), to realize high energy storage capability. Novel electrode materials derived from electrospun immiscible polymer blends and synthesized copolymers and terpolymers were described. Pore distributions of CNFs were tailored by varying the composition of polymers in immiscible blends or varying the monomer ratios of copolymer or terpolymers. Chapter 1 gives the detailed introduction of supercapacitors including history and storage principle of EDLCs, fabrication of carbon nanofiber based electrodes and electrolytes employed for EDLCs. It also explains the necessity and the advantages of tailored high surface area nanofibers as an electrode materials for supercapacitors. Chapter 2 describes the preparation of high surface area carbon nanofibers using polymer blends containing PAN and PMMA and introduces an effective and simple strategy to improve the surface area of CNFs by using a sacrificial polymer, PMMA. Chapter 3 describes blending of high fractional free volume polymer, 6FDA-DAM: DABA (3:2) into PBI to increase surface area and by using the higher etch rate of 6FDA-DAM: DABA in the blend to optimize pore distribution of CNFs. Chapter 4 introduces a novel approach to increase surface area of CNFs without any physical or chemical activation by using an in situ porogen containing copolymer P(AN-co-IA). The concept developed here avoids unnecessary and complex extra activation steps when fabricating carbon nanofibers which leads to lower char yield and uncontrollable pore sizes. Chapter 5 describes enhancement of surface area by using terpolymer P(AN-VIM-IA) to develop a new precursor. This approach is further advantageous since terpolymer can combine superior electrochemical properties of homopolymer, PAN and P(AN- co-IA) and P(AN-co-VIM). Chapter 6 describes the use of commercially available small molecule compatibilizer 2-MI to tailor pore architecture of carbon fiber derived from the immiscible blend of PBI/6FDD to match with the ion sizes of ionic liquid electrolytes thereby increasing the surface area of the CNFs that is accessible to electrolytes.

Novel fabrication of silicon carbide based ceramics for nuclear applications

NASA Astrophysics Data System (ADS)

Singh, Abhishek Kumar

Advances in nuclear reactor technology and the use of gas-cooled fast reactors require the development of new materials that can operate at the higher temperatures expected in these systems. These materials include refractory alloys based on Nb, Zr, Ta, Mo, W, and Re; ceramics and composites such as SiC--SiCf; carbon--carbon composites; and advanced coatings. Besides the ability to handle higher expected temperatures, effective heat transfer between reactor components is necessary for improved efficiency. Improving thermal conductivity of the fuel can lower the center-line temperature and, thereby, enhance power production capabilities and reduce the risk of premature fuel pellet failure. Crystalline silicon carbide has superior characteristics as a structural material from the viewpoint of its thermal and mechanical properties, thermal shock resistance, chemical stability, and low radioactivation. Therefore, there have been many efforts to develop SiC based composites in various forms for use in advanced energy systems. In recent years, with the development of high yield preceramic precursors, the polymer infiltration and pyrolysis (PIP) method has aroused interest for the fabrication of ceramic based materials, for various applications ranging from disc brakes to nuclear reactor fuels. The pyrolysis of preceramic polymers allow new types of ceramic materials to be processed at relatively low temperatures. The raw materials are element-organic polymers whose composition and architecture can be tailored and varied. The primary focus of this study is to use a pyrolysis based process to fabricate a host of novel silicon carbide-metal carbide or oxide composites, and to synthesize new materials based on mixed-metal silicocarbides that cannot be processed using conventional techniques. Allylhydridopolycarbosilane (AHPCS), which is an organometal polymer, was used as the precursor for silicon carbide. Inert gas pyrolysis of AHPCS produces near-stoichiometric amorphous silicon carbide (a-SiC) at 900--1150 °C. Results indicated that this processing technique can be effectively used to fabricate various silicon carbide composites with UC or UO2 as the nuclear component.

Controllable synthesis of mesoporous carbon nanospheres and Fe-N/carbon nanospheres as efficient oxygen reduction electrocatalysts.

PubMed

Wei, Jing; Liang, Yan; Zhang, Xinyi; Simon, George P; Zhao, Dongyuan; Zhang, Jin; Jiang, Sanping; Wang, Huanting

2015-04-14

The synthesis of mesoporous carbon nanospheres (MCNs), especially with diameters below 200 nm remains a great challenge due to weak interactions between the carbon precursors and soft templates, as well as the uncontrollable cross-linking rate of carbon precursors. Herein, we demonstrate a simple acid-assisted, hydrothermal synthesis approach to synthesizing such uniform MCNs with well controlled diameters ranging from 20 to 150 nm under highly acidic conditions (2 M HCl). Both the carbon precursor and the template are partly protonated under such conditions and show additional Coulombic interactions with chloride ions (acts as mediators). This kind of enhanced interaction is similar to that of the "I(+)X(-)S(+)" mechanism in the synthesis of mesoporous metal oxide, which can effectively retard the cross-linking rate of resol molecules and avoid macroscopic phase separation during the hydrothermal synthesis. Due to their uniform spherical morphology, small diameter, and high surface areas, MCNs can be modified with Fe and N species via impregnation of cheap precursors (ferric nitrate and dicyandiamide), which are further converted into nonprecious electrocatalysts for oxygen reduction reactions. The resulting Fe-N/MCNs exhibit high catalytic activities, long-term stability and improved methanol tolerance under alkaline conditions, which can be potentially used in direct methanol fuel cells and metal-air batteries.

Low-surface-area hard carbon anode for Na-ion batteries via graphene oxide as a dehydration agent

DOE PAGES

Luo, Wei; Bommier, Clement; Jian, Zelang; ...

2015-02-04

Na-ion batteries are emerging as one of the most promising energy storage technologies, particularly for grid-level applications. Among anode candidate materials, hard carbon is very attractive due to its high capacity and low cost. However, hard carbon anodes often suffer a low first-cycle Coulombic efficiency and fast capacity fading. In this study, we discover that doping graphene oxide into sucrose, the precursor for hard carbon, can effectively reduce the specific surface area of hard carbon to as low as 5.4 m²/g. We further reveal that such doping can effectively prevent foaming during caramelization of sucrose and extend the pyrolysis burn-offmore » of sucrose caramel over a wider temperature range. Thus, the obtained low-surface-area hard carbon greatly improves the first-cycle Coulombic efficiency from 74% to 83% and delivers a very stable cyclic life with 95% of capacity retention after 200 cycles.« less

Adsorption of methyl orange using activated carbon prepared from lignin by ZnCl2 treatment

NASA Astrophysics Data System (ADS)

Mahmoudi, K.; Hamdi, N.; Kriaa, A.; Srasra, E.

2012-08-01

Lignocellulosic materials are good and cheap precursors for the production of activated carbon. In this study, activated carbons were prepared from the lignin at different temperatures (200 to 500°C) by ZnCl2. The effects influencing the surface area of the resulting activated carbon are activation temperature, activation time and impregnation ratio. The optimum condition, are found an impregnation ratio of 2, an activation temperature of 450°C, and an activation time of 2 h. The results showed that the surface area and micropores volume of activated carbon at the experimental conditions are achieved to 587 and 0.23 cm3 g-1, respectively. The adsorption behavior of methyl orange dye from aqueous solution onto activated lignin was investigated as a function of equilibrium time, pH and concentration. The Langmuir and Freundlich adsorption models were applied to describe the equilibrium isotherms. A maximum adsorption capacity of 300 mg g-1 of methyl orange by activated carbon was achieved.

Low-Surface-Area Hard Carbon Anode for Na-Ion Batteries via Graphene Oxide as a Dehydration Agent

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

Luo, W; Bommier, C; Jian, ZL

2015-02-04

Na-ion batteries are emerging as one of the most promising energy storage technologies, particularly for grid-level applications. Among anode candidate materials, hard carbon is very attractive due to its high capacity and low cost. However, hard carbon anodes often suffer a low first-cycle Coulombic efficiency and fast capacity fading. In this study, we discover that doping graphene oxide into sucrose, the precursor for hard carbon, can effectively reduce the specific surface area of hard carbon to as low as 5.4 m(2)/g. We further reveal that such doping can effectively prevent foaming during caramelization of sucrose and extend the pyrolysis burnoffmore » of sucrose caramel over a wider temperature range. The obtained low-surface-area hard carbon greatly improves the first-cycle Coulombic efficiency from 74% to 83% and delivers a very stable cyclic life with 95% of capacity retention after 200 cycles.« less

Frontalin pheromone biosynthesis in the mountain pine beetle, Dendroctonus ponderosae, and the role of isoprenyl diphosphate synthases

PubMed Central

Keeling, Christopher I.; Chiu, Christine C.; Aw, Tidiane; Li, Maria; Henderson, Hannah; Tittiger, Claus; Weng, Hong-Biao; Blomquist, Gary J.; Bohlmann, Joerg

2013-01-01

The mountain pine beetle (Dendroctonus ponderosae Hopkins) is the most destructive pest of western North American pine forests. Adult males produce frontalin, an eight-carbon antiaggregation pheromone, via the mevalonate pathway, as part of several pheromones that initiate and modulate the mass attack of host trees. Frontalin acts as a pheromone, attractant, or kairomone in most Dendroctonus species, other insects, and even elephants. 6-Methylhept-6-en-2-one, a frontalin precursor, is hypothesized to originate from 10-carbon geranyl diphosphate (GPP), 15-carbon farnesyl diphosphate (FPP), or 20-carbon geranylgeranyl diphosphate (GGPP) via a dioxygenase- or cytochrome P450-mediated carbon–carbon bond cleavage. To investigate the role of isoprenyl diphosphate synthases in pheromone biosynthesis, we characterized a bifunctional GPP/FPP synthase and a GGPP synthase in the mountain pine beetle. The ratio of GPP to FPP produced by the GPP/FPP synthase was highly dependent on the ratio of the substrates isopentenyl diphosphate and dimethylallyl diphosphate used in the assay. Transcript levels in various tissues and life stages suggested that GGPP rather than GPP or FPP is used as a precursor to frontalin. Reduction of transcript levels by RNA interference of the isoprenyl diphosphate synthases identified GGPP synthase as having the largest effect on frontalin production, suggesting that frontalin is derived from a 20-carbon isoprenoid precursor rather than from the 10- or 15-carbon precursors. PMID:24167290

Stable-carbon isotope ratios for sourcing the nerve-agent precursor methylphosphonic dichloride and its products

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

Moran, James J.; Fraga, Carlos G.; Nims, Megan K.

The ability to connect a chemical threat agent to a specific batch of a synthetic precursor can provide a fingerprint to contribute to effective forensic investigations. Stable isotope analysis can leverage intrinsic, natural isotopic variability within the molecules of a threat agent to unlock embedded chemical fingerprints in the material. Methylphosphonic dichloride (DC) is a chemical precursor to the nerve agent sarin. It is converted to methylphosphonic difluoride (DF) as part of the sarin synthesis process. We used a suite of commercially available DC stocks to both evaluate the potential for δ13C analysis to be used as a fingerprinting toolmore » in sarin-related investigations and to develop sample preparation techniques (using chemical hydrolysis) that can simplify isotopic analysis of DC and its synthetic products. We demonstrate that natural isotopic variability in DC results in at least three distinct, isotope-resolved clusters within the thirteen stocks we analyzed. Isotopic variability in the carbon feedstock (i.e., methanol) used for DC synthesis is likely inherited by the DC samples we measured. We demonstrate that the hydrolysis of DC and DF to methylphosphonic acid (MPA) can be used as a preparative step for isotopic analysis because the reaction does not impart a measureable isotopic fractionation. MPA is more chemically stable, less toxic, and easier to handle than DC or DF. Further, the hydrolysis method we demonstrated can be applied to a suite of other precursors or to sarin itself, thereby providing a potentially valuable forensic tool.« less

Stable-Carbon Isotope Ratios for Sourcing the Nerve-Agent Precursor Methylphosphonic Dichloride and Its Products

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

Moran, James J.; Fraga, Carlos G.; Nims, Megan K.

The ability to connect a chemical threat agent to a specific batch of a synthetic precursor can provide a fingerprint to contribute to effective forensic investigations. Stable isotope analysis can leverage intrinsic, natural isotopic variability within the molecules of a threat agent to unlock embedded chemical fingerprints in the material. Methylphosphonic dichloride (DC) is a chemical precursor to the nerve agent sarin. DC is converted to methylphosphonic difluoride (DF) as part of the sarin synthesis process. We used a suite of commercially available DC stocks to both evaluate the potential for δ 13C analysis to be used as a fingerprintingmore » tool in sarin-related investigations and to develop sample preparation techniques (using chemical hydrolysis) that can simplify isotopic analysis of DC and its synthetic products. We demonstrate that natural isotopic variability in DC results in at least three distinct, isotope-resolved clusters within the thirteen stocks we analyzed. Isotopic variability in the carbon feedstock (i.e., methanol) used for DC synthesis is likely inherited by the DC samples we measured. Here, we demonstrate that the hydrolysis of DC and DF to methylphosphonic acid (MPA) can be used as a preparative step for isotopic analysis because the reaction does not impart a significant isotopic fractionation. MPA is more chemically stable, less toxic, and easier to handle than DC or DF. Further, the hydrolysis method we demonstrated can be applied to a suite of other precursors or to sarin itself, thereby providing a potentially valuable forensic tool.« less

Stable-Carbon Isotope Ratios for Sourcing the Nerve-Agent Precursor Methylphosphonic Dichloride and Its Products

DOE PAGES

Moran, James J.; Fraga, Carlos G.; Nims, Megan K.

2018-04-01

The ability to connect a chemical threat agent to a specific batch of a synthetic precursor can provide a fingerprint to contribute to effective forensic investigations. Stable isotope analysis can leverage intrinsic, natural isotopic variability within the molecules of a threat agent to unlock embedded chemical fingerprints in the material. Methylphosphonic dichloride (DC) is a chemical precursor to the nerve agent sarin. DC is converted to methylphosphonic difluoride (DF) as part of the sarin synthesis process. We used a suite of commercially available DC stocks to both evaluate the potential for δ 13C analysis to be used as a fingerprintingmore » tool in sarin-related investigations and to develop sample preparation techniques (using chemical hydrolysis) that can simplify isotopic analysis of DC and its synthetic products. We demonstrate that natural isotopic variability in DC results in at least three distinct, isotope-resolved clusters within the thirteen stocks we analyzed. Isotopic variability in the carbon feedstock (i.e., methanol) used for DC synthesis is likely inherited by the DC samples we measured. Here, we demonstrate that the hydrolysis of DC and DF to methylphosphonic acid (MPA) can be used as a preparative step for isotopic analysis because the reaction does not impart a significant isotopic fractionation. MPA is more chemically stable, less toxic, and easier to handle than DC or DF. Further, the hydrolysis method we demonstrated can be applied to a suite of other precursors or to sarin itself, thereby providing a potentially valuable forensic tool.« less

Stable-carbon isotope ratios for sourcing the nerve-agent precursor methylphosphonic dichloride and its products.

PubMed

Moran, James J; Fraga, Carlos G; Nims, Megan K

2018-08-15

The ability to connect a chemical threat agent to a specific batch of a synthetic precursor can provide a fingerprint to contribute to effective forensic investigations. Stable isotope analysis can leverage intrinsic, natural isotopic variability within the molecules of a threat agent to unlock embedded chemical fingerprints in the material. Methylphosphonic dichloride (DC) is a chemical precursor to the nerve agent sarin. DC is converted to methylphosphonic difluoride (DF) as part of the sarin synthesis process. We used a suite of commercially available DC stocks to both evaluate the potential for δ 13 C analysis to be used as a fingerprinting tool in sarin-related investigations and to develop sample preparation techniques (using chemical hydrolysis) that can simplify isotopic analysis of DC and its synthetic products. We demonstrate that natural isotopic variability in DC results in at least three distinct, isotope-resolved clusters within the thirteen stocks we analyzed. Isotopic variability in the carbon feedstock (i.e., methanol) used for DC synthesis is likely inherited by the DC samples we measured. We demonstrate that the hydrolysis of DC and DF to methylphosphonic acid (MPA) can be used as a preparative step for isotopic analysis because the reaction does not impart a significant isotopic fractionation. MPA is more chemically stable, less toxic, and easier to handle than DC or DF. Further, the hydrolysis method we demonstrated can be applied to a suite of other precursors or to sarin itself, thereby providing a potentially valuable forensic tool. Copyright © 2018. Published by Elsevier B.V.

The production of oxidants in Europa's surface.

PubMed

Johnson, R E; Quickenden, T I; Cooper, P D; McKinley, A J; Freeman, C G

2003-01-01

The oxidants produced by radiolysis and photolysis in the icy surface of Europa may be necessary to sustain carbon-based biochemistry in Europa's putative subsurface ocean. Because the subduction of oxidants to the ocean presents considerable thermodynamic challenges, we examine the formation of oxygen and related species in Europa's surface ice with the goal of characterizing the chemical state of the irradiated material. Relevant spectral observations of Europa and the laboratory data on the production of oxygen and related species are first summarized. Since the laboratory data are incomplete, we examine the rate equations for formation of oxygen and its chemical precursors by radiolysis and photolysis. Measurements and simple rate equations are suggested that can be used to characterize the production of oxidants in Europa's surface material and the chemical environment produced by radiolysis. Possible precursor molecules and the role of radical trapping are examined. The possibility of oxygen reactions on grain surfaces in Europa's regolith is discussed, and the earlier estimates of the supply of O(2) to the atmosphere are increased.

Obtaining aluminas from the thermal decomposition of their different precursors: An {sup 27}Al MAS NMR and X-ray powder diffraction studies

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

Chagas, L.H.; De Carvalho, G.S.G.; San Gil, R.A.S.

2014-01-01

Graphical abstract: - Highlights: • We synthesized three precursors of alumina from different methods. • The calcination of the precursors generated several alumina polymorphs. • XRD and NMR were used for structural investigation of the polymorphs. • The synthesis route determines the structural and textural properties of the solids. - Abstract: A commercial sample of Boehmite was used as precursor of alumina polymorphs. For comparison, three other precursors were synthesized from different methods. Particularly, the use of excess of urea promoted a very crystalline form of basic aluminum carbonate. The characteristics of the four precursors were investigated by thermal, vibrationalmore » and X-ray powder diffraction (XRD) analysis. Additionally, the nuclear magnetic resonance, with magic angle spinning ({sup 27}Al MAS NMR), was used to verify the coordination of aluminum cations. Each precursor was calcined at various temperatures generating alumina polymorphs, which were structurally analyzed by XRD and {sup 27}Al MAS NMR. Due to interest in catalysis supports, special attention was given to the γ-Al{sub 2}O{sub 3} phase, which in addition to structural investigation was subjected to textural analysis. The results showed that, from different synthesis procedures and common route of calcination, one can obtain materials with the same composition but with different structural and textural properties, which in turn can significantly influence the performance of a supported catalyst.« less

Gelcasting polymeric precursors for producing net-shaped graphites

DOEpatents

Klett, James W.; Janney, Mark A.

2002-01-01

The present invention discloses a method for molding complex and intricately shaped high density monolithic carbon, carbon-carbon, graphite, and thermoplastic composites using gelcasting technology. The method comprising a polymeric carbon precursor, a solvent, a dispersant, an anti-foaming agent, a monomer system, and an initiator system. The components are combined to form a suspension which is poured into a mold and heat-treated to form a thermoplastic part. The thermoplastic part can then be further densified and heat-treated to produce a high density carbon or graphite composite. The present invention also discloses the products derived from this method.

Porous yolk-shell microspheres as N-doped carbon matrix for motivating the oxygen reduction activity of oxygen evolution oriented materials.

PubMed

Zhou, Jinqiu; Wang, Mengfan; Qian, Tao; Liu, Sisi; Cao, Xuecheng; Yang, Tingzhou; Yang, Ruizhi; Yan, Chenglin

2017-09-08

It is highly challenging to explore high-performance bi-functional oxygen electrode catalysts for their practical application in next-generation energy storage and conversion devices. In this work, we synthesize hierarchical N-doped carbon microspheres with porous yolk-shell structure (NCYS) as a metal-free electrocatalyst toward efficient oxygen reduction through a template-free route. The enhanced oxygen reduction performances in both alkaline and acid media profit well from the porous yolk-shell structure as well as abundant nitrogen functional groups. Furthermore, such yolk-shell microspheres can be used as precursor materials to motivate the oxygen reduction activity of oxygen evolution oriented materials to obtain a desirable bi-functional electrocatalyst. To verify its practical utility, Zn-air battery tests are conducted and exhibit satisfactory performance, indicating that this constructed concept for preparation of bi-functional catalyst will afford a promising strategy for exploring novel metal-air battery electrocatalysts.

Porous yolk-shell microspheres as N-doped carbon matrix for motivating the oxygen reduction activity of oxygen evolution oriented materials

NASA Astrophysics Data System (ADS)

Zhou, Jinqiu; Wang, Mengfan; Qian, Tao; Liu, Sisi; Cao, Xuecheng; Yang, Tingzhou; Yang, Ruizhi; Yan, Chenglin

2017-09-01

It is highly challenging to explore high-performance bi-functional oxygen electrode catalysts for their practical application in next-generation energy storage and conversion devices. In this work, we synthesize hierarchical N-doped carbon microspheres with porous yolk-shell structure (NCYS) as a metal-free electrocatalyst toward efficient oxygen reduction through a template-free route. The enhanced oxygen reduction performances in both alkaline and acid media profit well from the porous yolk-shell structure as well as abundant nitrogen functional groups. Furthermore, such yolk-shell microspheres can be used as precursor materials to motivate the oxygen reduction activity of oxygen evolution oriented materials to obtain a desirable bi-functional electrocatalyst. To verify its practical utility, Zn-air battery tests are conducted and exhibit satisfactory performance, indicating that this constructed concept for preparation of bi-functional catalyst will afford a promising strategy for exploring novel metal-air battery electrocatalysts.

One-pot synthesis of amino acid precursors with insoluble organic matter in planetesimals with aqueous activity.

PubMed

Kebukawa, Yoko; Chan, Queenie H S; Tachibana, Shogo; Kobayashi, Kensei; Zolensky, Michael E

2017-03-01

The exogenous delivery of organic molecules could have played an important role in the emergence of life on the early Earth. Carbonaceous chondrites are known to contain indigenous amino acids as well as various organic compounds and complex macromolecular materials, such as the so-called insoluble organic matter (IOM), but the origins of the organic matter are still subject to debate. We report that the water-soluble amino acid precursors are synthesized from formaldehyde, glycolaldehyde, and ammonia with the presence of liquid water, simultaneously with macromolecular organic solids similar to the chondritic IOM. Amino acid products from hydrothermal experiments after acid hydrolysis include α-, β-, and γ-amino acids up to five carbons, for which relative abundances are similar to those extracted from carbonaceous chondrites. One-pot aqueous processing from simple ubiquitous molecules can thus produce a wide variety of meteoritic organic matter from amino acid precursors to macromolecular IOM in chondrite parent bodies.

Facile synthesis high nitrogen-doped porous carbon nanosheet from pomelo peel and as catalyst support for nitrobenzene hydrogenation

NASA Astrophysics Data System (ADS)

Zuo, Pingping; Duan, Jiaqi; Fan, Huailin; Qu, Shijie; Shen, Wenzhong

2018-03-01

Nitrogen-doping porous carbon-based nanosheets were fabricated from pemole peel and melamine through hydrothermal route and carbonization. The pomelo peel with sponge-like natural structure was employed as carbon source, and melamine was used both as nitrogen precursors and as nanosheet structure directing. The morphology and chemical composition of the obtained porous carbon nanosheet carbon materials were characterized by scanning electron microscopy, thermogravimetric analyzer, Fourier transform infrared spectra, transmission electron microscopy, BET surface area measurement, X-ray photoelectron spectroscopy and X-ray powder diffraction. The result indicated that the nanosheet thickness, nitrogen-doped amount and surface area were determined by the ratio of pomelo peel to melamine and carbonization temperature. The catalytic nitrobenzene hydrogenation was evaluated after Pd was loaded on nitrogen-doping porous carbon-based nanosheet. The results showed Pd@PCN had almost 100% conversion and good cycling performance towards the hydrogenation of nitrobenzene due to the developed pore structure, high nitrogen-doping and well dispersed less Pd particle; it was superior to other nanomaterial supports and demonstrated great potential application.

On-site manufacture of propellant oxygen from lunar resources

NASA Technical Reports Server (NTRS)

Rosenberg, Sanders D.

1992-01-01

The Aerojet Carbothermal Process for the manufacture of oxygen from lunar resources has three essential steps: the reduction of silicate with methane to form carbon monoxide and hydrogen; the reduction of carbon monoxide with hydrogen to form methane and water; and the electrolysis of water to form oxygen and hydrogen. This cyclic process does not depend upon the presence of water or water precursors in the lunar materials; it will produce oxygen from silicates regardless of their precise composition and fine structure. Research on the first step of the process was initiated by determining some of the operating conditions required to reduce igneous rock with carbon and silicon carbide. The initial phase of research on the second step is completed; quantitative conversion of carbon monoxide and hydrogen to methane and water was achieved with a nickel-on-kieselguhr catalyst. The equipment used in and the results obtained from these process studies are reported in detail.

A facile molten-salt route to graphene synthesis.

PubMed

Liu, Xiaofeng; Giordano, Cristina; Antonietti, Markus

2014-01-15

Efficient synthetic routes are continuously pursued for graphene in order to implement its applications in different areas. However, direct conversion of simple monomers to graphene through polymerization in a scalable manner remains a major challenge for chemists. Herein, a molten-salt (MS) route for the synthesis of carbon nanostructures and graphene by controlled carbonization of glucose in molten metal chloride is reported. In this process, carbohydrate undergoes polymerization in the presence of strongly interacting ionic species, which leads to nanoporous carbon with amorphous nature and adjustable pore size. At a low precursor concentration, the process converts the sugar molecules (glucose) to rather pure few-layer graphenes. The MS-derived graphenes are strongly hydrophobic and exhibit remarkable selectivity and capacity for absorption of organics. The methodology described may open up a new avenue towards the synthesis and manipulation of carbon materials in liquid media. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Raman spectra boron doped amorphous carbon thin film deposited by bias assisted-CVD

NASA Astrophysics Data System (ADS)

Ishak, A.; Fadzilah, A. N.; Dayana, K.; Saurdi, I.; Malek, M. F.; Nurbaya, Z.; Shafura, A. K.; Rusop, M.

2018-05-01

Boron doped amorphous carbon thin film carbon was deposited at 200°C-350°C by bias assisted-CVD using palm oil as a precursor material. The structural boron doped amorphous carbon films were discussed by Raman analysis through the evolution of D and G bands. The spectral evolution observed showed the increase of upward shift of D and G peaks as substrate deposition temperatures increased. These structural changes were further correlated with optical gap and the results obtained are discussed and compared. The estimated optical band gap is found to be 1.9 to 2.05 eV and conductivity is to be in the range of 10-5 Scm-1 to 10-4 Scm-1. The decrease of optical band gap is associated to conductivity increased which change the characteristic parameters of Raman spectra including the position of G peak, full width at half maximum of G peak, and ID/IG.

Improvement in Field Electron Emission Performance of Natural-Precursor-Grown Carbon Nanofibers by Thermal Annealing in Argon Atmosphere

NASA Astrophysics Data System (ADS)

Ghosh, Pradip; Zamri, Mohd; Ghosh, Debasish; Soga, Tetsuo; Jimbo, Takashi; Hashimoto, Shinobu; Ohashi, Shuho; Tanemura, Masaki

2011-01-01

Carbon nanofibers (CNFs) were grown on a graphite substrate by the spray pyrolysis of a botanical hydrocarbon, turpentine oil, using ferrocene as the catalyst and sulfur as the promoter. The as-grown CNFs were annealed at 450 °C for 30 min in an air, and then at 1800 °C in an argon atmosphere for 2 h. The annealed CNFs have better degree of crystallinity and reduced number of defects compared with the as-grown CNFs confirmed by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy, and thermogravimetric analysis. The as-grown and annealed CNFs were found to be effective electron emitters with turn-on fields of 3.2 and 2.1 V/µm, respectively. The improvement in field emission (FE) performance can be explained in terms of the higher degree of graphitization of the CNFs after thermal annealing. This improved FE performance of the natural precursor grown CNFs was comparable to the FE performance level attainable for the conventional carbon nanomaterials grown using petroleum products. Thus, it was considered that the use of petroleum products could be avoidable for CNF growth and that CNFs grown using ecofriendly materials are very promising for the application in future field emission displays (FEDs).

Treatment of surfaces with low-energy electrons

NASA Astrophysics Data System (ADS)

Frank, L.; Mikmeková, E.; Lejeune, M.

2017-06-01

Electron-beam-induced deposition of various materials from suitable precursors has represented an established branch of nanotechnology for more than a decade. A specific alternative is carbon deposition on the basis of hydrocarbons as precursors that has been applied to grow various nanostructures including masks for subsequent technological steps. Our area of study was unintentional electron-beam-induced carbon deposition from spontaneously adsorbed hydrocarbon molecules. This process traditionally constitutes a challenge for scanning electron microscopy practice preventing one from performing any true surface studies outside an ultrahigh vacuum and without in-situ cleaning of samples, and also jeopardising other electron-optical devices such as electron beam lithographs. Here we show that when reducing the energy of irradiating electrons sufficiently, the e-beam-induced deposition can be converted to e-beam-induced release causing desorption of hydrocarbons and ultimate cleaning of surfaces in both an ultrahigh and a standard high vacuum. Using series of experiments with graphene samples, we demonstrate fundamental features of e-beam-induced desorption and present results of checks for possible radiation damage using Raman spectroscopy that led to optimisation of the electron energy for damage-free cleaning. The method of preventing carbon contamination described here paves the way for greatly enhanced surface sensitivity of imaging and substantially reduced demands on vacuum systems for nanotechnological applications.

Laser-Induced Graphene by Multiple Lasing: Toward Electronics on Cloth, Paper, and Food.

PubMed

Chyan, Yieu; Ye, Ruquan; Li, Yilun; Singh, Swatantra Pratap; Arnusch, Christopher J; Tour, James M

2018-03-27

A simple and facile method for obtaining patterned graphene under ambient conditions on the surface of diverse materials ranging from renewable precursors such as food, cloth, paper, and cardboard to high-performance polymers like Kevlar or even on natural coal would be highly desirable. Here, we report a method of using multiple pulsed-laser scribing to convert a wide range of substrates into laser-induced graphene (LIG). With the increased versatility of the multiple lase process, highly conductive patterns can be achieved on the surface of a diverse number of substrates in ambient atmosphere. The use of a defocus method results in multiple lases in a single pass of the laser, further simplifying the procedure. This method can be implemented without increasing processing times when compared with laser induction of graphene on polyimide (Kapton) substrates as previously reported. In fact, any carbon precursor that can be converted into amorphous carbon can be converted into graphene using this multiple lase method. This may be a generally applicable technique for forming graphene on diverse substrates in applications such as flexible or even biodegradable and edible electronics.

Enhanced humification by carbonated basic oxygen furnace steel slag--I. Characterization of humic-like acids produced from humic precursors.

PubMed

Qi, Guangxia; Yue, Dongbei; Fukushima, Masami; Fukuchi, Shigeki; Nie, Yongfeng

2012-01-01

Carbonated basic oxygen furnace steel slag (hereinafter referred to as "steel slag") is generated during iron and steel manufacturing and is often classified as waste. The effect of steel slag on humification process was investigated. Catechol, glycine and glucose were used as model humic precursors from degraded biowastes. To verify that humification occurred in the system, humic-like acids (HLAs) were isolated and characterized structurally by elemental analysis, FTIR spectra, solid-state CP-MAS (13)C NMR spectra, and TMAH-Py-GC/MS. Characteristics of the steel slag-HLA were compared with those of HLAs formed in the presence of zeolite and birnessite, and with that of mature compost humic acid. The results showed that steel slag-HLA, like zeolite- and birnessite-HLA, is complex organic material containing prominent aromatic structures. Steel slag substantially accelerated the humification process, which would be highly significant for accelerating the stabilization of biowastes during composting (e.g. municipal solid waste, sewage sludge, and food waste). Copyright © 2011 Elsevier Ltd. All rights reserved.

Salt flux synthesis of single and bimetallic carbide nanowires

NASA Astrophysics Data System (ADS)

Leonard, Brian M.; Waetzig, Gregory R.; Clouser, Dale A.; Schmuecker, Samantha M.; Harris, Daniel P.; Stacy, John M.; Duffee, Kyle D.; Wan, Cheng

2016-07-01

Metal carbide compounds have a broad range of interesting properties and are some of the hardest and highest melting point compounds known. However, their high melting points force very high reaction temperatures and thus limit the formation of high surface area nanomaterials. To avoid the extreme synthesis temperatures commonly associated with these materials, a new salt flux technique has been employed to reduce reaction temperatures and form these materials in the nanometer regime. Additionally, the use of multiwall carbon nanotubes as a reactant further reduces the diffusion distance and provides a template for the final carbide materials. The metal carbide compounds produced through this low temperature salt flux technique maintain the nanowire morphology of the carbon nanotubes but increase in size to ˜15-20 nm diameter due to the incorporation of metal in the carbon lattice. These nano-carbides not only have nanowire like shape but also have much higher surface areas than traditionally prepared metal carbides. Finally, bimetallic carbides with composition control can be produced with this method by simply using two metal precursors in the reaction. This method provides the ability to produce nano sized metal carbide materials with size, morphology, and composition control and will allow for these compounds to be synthesized and studied in a whole new size and temperature regime.

Toughened and corrosion- and wear-resistant composite structures and fabrication methods thereof

DOEpatents

Seals, Roland D; Ripley, Edward B; Hallman, Russell L

2014-04-08

Composite structures having a reinforced material interjoined with a substrate and methods of creating a composite material interjoined with a substrate. In some embodiments the composite structure may be a line or a spot or formed by reinforced material interjoined with the substrate. The methods typically include disposing a precursor material comprising titanium diboride and/or titanium monoboride on at least a portion of the substrate and heating the precursor material and the at least a portion of the substrate in the presence of an oxidation preventative until at least a portion of the precursor material forms reinforced material interjoined with the substrate. The precursor material may be disposed on the substrate as a sheet or a tape or a slurry or a paste. Localized surface heating may be used to heat the precursor material. The reinforced material typically comprises a titanium boron compound, such as titanium monoboride, and preferably comprises .beta.-titanium. The substrate is typically titanium-bearing, iron-bearing, or aluminum-bearing. A welding rod is provided as an embodiment. The welding rod includes a metal electrode and a precursor material is disposed adjacent at least a portion of the metal electrode. A material for use in forming a composite structure is provided. The material typically includes a precursor material that includes one or more materials selected from the following group: titanium diboride and titanium monoboride. The material also typically includes a flux.

Changes in Dissolved Organic Matter Composition and Disinfection Byproduct Precursors in Advanced Drinking Water Treatment Processes.

PubMed

Phungsai, Phanwatt; Kurisu, Futoshi; Kasuga, Ikuro; Furumai, Hiroaki

2018-03-20

Molecular changes in dissolved organic matter (DOM) from treatment processes at two drinking water treatment plants in Japan were investigated using unknown screening analysis by Orbitrap mass spectrometry. DOM formulas with carbon, hydrogen and oxygen (CHO-DOM) were the most abundant class in water samples, and over half of them were commonly found at both plants. Among the treatment processes, ozonation induced the most drastic changes to DOM. Mass peak intensities of less saturated CHO-DOM (positive (oxygen subtracted double bond equivalent per carbon (DBE-O)/C)) decreased by ozonation, while more saturated oxidation byproducts (negative (DBE-O)/C) increased and new oxidation byproducts (OBPs) were detected. By Kendrick mass analysis, ozone reactions preferred less saturated CHO-DOM in the same alkylation families and produced more saturated alkylation families of OBPs. Following ozonation, biological activated carbon filtration effectively removed <300 Da CHO-DOM, including OBPs. Following chlorination, over 50 chlorinated formulas of disinfection byproducts (DBPs) were found in chlorinated water samples where at least half were unknown. Putative precursors of these DBPs were determined based on electrophilic substitutions and addition reactions. Ozonation demonstrated better decomposition of addition reaction-type precursors than electrophilic substitution-type precursors; over half of both precursor types decreased during biological activated carbon filtration.

Advanced Nanofiber-Based Lithium-Ion Battery Cathodes

NASA Astrophysics Data System (ADS)

Toprakci, Ozan

Among various energy storage technologies, rechargeable lithium-ion batteries have been considered as effective solution to the increasing need for high-energy density electrochemical power sources. Rechargeable lithium-ion batteries offer energy densities 2 - 3 times and power densities 5 - 6 times higher than conventional Ni-Cd and Ni-MH batteries, and as a result, they weigh less and take less space for a given energy delivery. However, the use of lithium-ion batteries in many large applications such as electric vehicles and storage devices for future power grids is hindered by the poor thermal stability, relatively high toxicity, and high cost of lithium cobalt oxide (LiCoO2) powders, which are currently used as the cathode material in commercial lithium-ion batteries. Recently, lithium iron phosphate (LiFePO 4) powders have become a favorable cathode material for lithium-ion batteries because of their low cost, high discharge potential (around 3.4 V versus Li/Li+), large specific capacity (170 mAh g -1), good thermal stability, and high abundance with the environmentally benign and safe nature. As a result, there is a huge demand for the production of high-performance LiFePO4. However, LiFePO4 also has its own limitation such as low conductivity (˜10-9 S cm -1), which results in poor rate capability. To address this problem, various approaches can be used such as decreasing particle size of LiFePO 4, doping LiFePO4 with metal ions or coating LiFePO 4 surface with carboneous materials. Formation of conductive layer on LiFePO4 and decreasing particle size are promising approaches due to their superior contribution to electrical conductivity and electrochemical performance of LiFePO4. Although different approaches can be used for surface coating and particle size decrement, electrospinning can be potentially considered as an efficient, simple and inexpensive way. In this study, LiFePO 4/carbon and carbon nanotube- and graphene-loaded electrospun LiFePO 4/carbon composite nanofibers were synthesized by using a combination of sol-gel and electrospinning. During the material preparation, polyacrylonitrile (PAN) was used as an electrospinning media and a carbon source. LiFePO 4 precursor materials and/or conductive materials (carbon nanotubes and graphene) and PAN were dissolved in N,N-dimethylformamide separately and they were mixed before electrospinning. LiFePO4 precursor/PAN fibers were heat treated, during which LiFePO4 precursor transformed to energy-storage LiFePO4 material and PAN was converted to carbon. The surface morphology, microstructure and electrochemical performance of the materials were analyzed. Compared with conventional powder based positive electrodes, the novel LiFePO4/C composite nanofiber cathodes possess better electrochemical performance. Furthermore, the newly developed LiFePO 4/C composite nanofibers are easy to fabricate, highly controllable, and can be used in practical Lithium-ion battery applications. In addition to LiFePO4, more recent efforts have been directed to mixed form of layered lithiummetal oxides (Li-Ni-Mn-Co). Nickel and manganese are of importance because of their lower cost, safety and higher abundance in nature. These new cathodes offer noticeable improvement in the capacity and cycling behavior. In these cathodes, LiNi1/3Co1/3Mn 1/3O2 attracted significant interest because of its good electrochemical properties such as high capacity, prolonged cycling life, and so on. On the other hand, it has some disadvantages such as instability at high voltages and high current densities. To overcome these problems, synthesis of layered Li-rich composite materials such as xLi2MnO3˙(1-x)LiCo 1/3Ni1/3Mn1/3O2 can be a promising approach. In this study, various xLi2MnO3˙(1-x)LiCo 1/3Ni1/3Mn1/3O2 (x=0.1, 0.2, 0.3, 0.4, 0.5) composite cathode materials were prepared by a one-step sol-gel route. Morphology, microstructure and electrochemical behavior of these cathode materials were evaluated. The resultant cathode material shows good electrochemical performance. Relatively low cost and simple preparation route make new xLi2MnO3˙(1-x)LiMn1/3Ni 1/3Co1/3O2 composite materials possible to use as potential cathode candidate for lithium-ion batteries.

Construction of high-energy-density supercapacitors from pine-cone-derived high-surface-area carbons.

PubMed

Karthikeyan, Kaliyappan; Amaresh, Samuthirapandiyan; Lee, Sol Nip; Sun, Xueliang; Aravindan, Vanchiappan; Lee, Young-Gi; Lee, Yun Sung

2014-05-01

Very high surface area activated carbons (AC) are synthesized from pine cone petals by a chemical activation process and subsequently evaluated as an electrode material for supercapacitor applications in a nonaqueous medium. The maximum specific surface area of ∼3950 m(2)  g(-1) is noted for the material treated with a 1:5 ratio of KOH to pine cone petals (PCC5), which is much higher than that reported for carbonaceous materials derived from various other biomass precursors. A symmetric supercapacitor is fabricated with PCC5 electrodes, and the results showed enhanced supercapacitive behavior with the highest energy density of ∼61 Wh kg(-1). Furthermore, outstanding cycling ability is evidenced for such a configuration, and ∼90 % of the initial specific capacitance after 20,000 cycles under harsh conditions was observed. This result revealed that the pine-cone-derived high-surface-area AC can be used effectively as a promising electrode material to construct high-energy-density supercapacitors. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

High Performance Materials Applications to Moon/Mars Missions and Bases

NASA Technical Reports Server (NTRS)

Noever, David A.; Smith, David D.; Sibille, Laurent; Brown, Scott C.; Cronise, Raymond J.; Lehoczky, Sandor L.

1998-01-01

Two classes of material processing scenarios will feature prominently in future interplanetary exploration: in situ production using locally available materials in lunar or planetary landings and high performance structural materials which carve out a set of properties for uniquely hostile space environments. To be competitive, high performance materials must typically offer orders of magnitude improvements in thermal conductivity or insulation, deliver high strength-to-weight ratios, or provide superior durability (low corrosion and/or ablative character, e.g., in heat shields). The space-related environmental parameters of high radiation flux, low weight, and superior reliability limits many typical aerospace materials to a short list comprising high performance alloys, nanocomposites and thin-layer metal laminates (Al-Cu, Al-Ag) with typical dimensions less than the Frank-Reed-type dislocation source. Extremely light weight carbon-carbon composites and carbon aerogels will be presented as novel examples which define broadened material parameters, particularly owing to their extreme thermal insulation (R-32-64) and low densities (<0.01 g/cu cm) approaching that of air itself. Even with these low-weight payload additions, rocket thrust limits and transport costs will always place a premium on assembling as much structural and life support resources upon interplanetary, lunar, or asteroid arrival. As an example, for in situ lunar glass manufacture, solar furnaces reaching 1700 C for pure silica glass manufacture in situ are compared with sol-gel technology and acid-leached ultrapure (<0.1% FeO) silica aerogel precursors.

Anodes for alkaline electrolysis

DOEpatents

Soloveichik, Grigorii Lev [Latham, NY

2011-02-01

A method of making an anode for alkaline electrolysis cells includes adsorption of precursor material on a carbonaceous material, conversion of the precursor material to hydroxide form and conversion of precursor material from hydroxide form to oxy-hydroxide form within the alkaline electrolysis cell.

Improved ablative materials for the ASRM nozzle

NASA Technical Reports Server (NTRS)

Canfield, A.; Clinton, R. G.; Armour, W.; Koenig, J.

1992-01-01

Rayon precursor carbon-cloth phenolic was developed more than 30 years ago and is used in most nozzles today including the Poseidon, Trident, Peacekeeper, Small ICBM, Space Shuttle, and numerous tactical and space systems. Specifications and manufacturing controls were placed on these materials and, once qualified, a no-change policy was instituted. The current material is acceptable; however, prepreg variability does not always accommodate the requirements of automation. The advanced solid rocket motor requires material with less variability for automated manufacturing. An advanced solid rocket motor materials team, composed of NASA, Thiokol, Aerojet, SRI, and Lockheed specialists, along with materials suppliers ICI Fiberite/Polycarbon, BP Chemicals/Hitco, and Amoco, embarked on a program to improve the current materials. The program consisted of heat treatment studies and standard and low-density material improvements evaluation. Improvements evaluated included fiber/fabric heat treatments, weave variations, resin application methods, process controls, and monitors.

Elemental Metals or Oxides Distributed on a Carbon Substrate or Self-Supported and the Manufacturing Process Using Graphite Oxide as Template

NASA Technical Reports Server (NTRS)

Hung, Ching-Cheh (Inventor)

1999-01-01

A process for providing elemental metals or metal oxides distributed on a carbon substrate or self-supported utilizing graphite oxide as a precursor. The graphite oxide is exposed to one or more metal chlorides to form an intermediary product comprising carbon, metal, chloride, and oxygen. This intermediary product can be further processed by direct exposure to carbonate-solutions to form a second intermediary product comprising carbon, metal carbonate, and oxygen. Either intermediary product may be further processed: a) in air to produce metal oxide; b) in an inert environment to produce metal oxide on carbon substrate; c) in a reducing environment to produce elemental metal distributed on carbon substrate. The product generally takes the shape of the carbon precursor.

Synthesis and Characterization of Solution and Melt Processible Poly(Acrylonitrile-Co-Methyl Acrylate) Statistical Copolymers

NASA Astrophysics Data System (ADS)

Pisipati, Padmapriya

Polyacrylonitrile (PAN) and its copolymers are used in a wide variety of applications ranging from textiles to purification membranes, packaging material and carbon fiber precursors. High performance polyacrylonitrile copolymer fiber is the most dominant precursor for carbon fibers. Synthesis of very high molecular weight poly(acrylonitrile-co-methyl acrylate) copolymers with weight average molecular weights of at least 1.7 million g/mole were synthesized on a laboratory scale using low temperature, emulsion copolymerization in a closed pressure reactor. Single filaments were spun via hybrid dry-jet gel solution spinning. These very high molecular weight copolymers produced precursor fibers with tensile strengths averaging 954 MPa with an elastic modulus of 15.9 GPa (N = 296). The small filament diameters were approximately 5 im. Results indicated that the low filament diameter that was achieved with a high draw ratio, combined with the hybrid dry-jet gel spinning process lead to an exponential enhancement of the tensile properties of these fibers. Carbon fibers for polymer matrix composites are currently derived from polyacrylonitrile copolymer fiber precursors where solution spinning accounts for ˜40 % of the total fiber production cost. To expand carbon fiber applications into the automotive industry, the cost of the carbon fiber needs to be reduced from 8 to ˜3-5. In order to develop an alternative melt processing route several benign plasticizers have been investigated. A low temperature, persulfate-metabisulfite initiated emulsion copolymerization was developed to synthesize poly(acrylonitrile-co-methyl acrylate) copolymers with acrylonitrile contents between 91-96 wt% with a molecular weight range of 100-200 kg/mol. This method was designed for a potential industrial scale up. Furthermore, water was investigated as a potential melting point depressant for these copolymers. Twenty-five wt% water lead to a decrease in the Tm of a 93/7 wt/wt % poly(acrylonitrile-co-methyl acrylate) of Mw = 200 kg/mol to 160 0C as measured via DSC. Glycerin, ethylene glycol and glycerin/water combinations were investigated as potential plasticizers for high molecular weight (˜200,000 g/mol), high acrylonitrile (93-96 mole:mole %) content poly(acrylonitrile-co-methyl acrylate) statistical copolymers. Pure glycerin (25 wt %) induced crystallization followed by a reduced "Tm" of about 213 0C via DSC. However this composition did not melt process well. A lower M W (˜35 kg/mol) copolymer did extrude with no apparent degradation. Our hypothesis is that the hydroxyl groups in glycerin (or water) disrupt the strong dipole-dipole interactions between the chains enabling the copolymer endothermic transition (Tm) to be reduced and enable melting before the onset of degradation. Additionally high molecular weight (Mw = 200-230 kg/mol) poly(acrylonitrile-co-methyl acrylate) copolymers with lower acrylonitrile content (82-85 wt %) were synthesized via emulsion copolymerization and successfully melt pressed. These materials will be further investigated for their utility in packaging applications.

Silsesquioxanes as precursors to ceramic composites

NASA Technical Reports Server (NTRS)

Hurwitz, Frances I.; Hyatt, Lizbeth H.; Gorecki, Joy; Damore, Lisa

1987-01-01

Silsesquioxanes having the general structure RSiO sub 1.5, where R = methyl, propyl, or phenyl, melt flow at 70 to 100 C. Above 100 C, free -OH groups condense. At 225 C further crosslinking occurs, and the materials form thermosets. Pyrolysis, with accompanying loss of volatiles, takes place at nominally 525 C. At higher temperatures, the R group serves as an internal carbon soruce for carbo-thermal reduction to SiC accompanied by the evolution of CO. By blending silsesquioxanes with varying R groups, both the melt rheology and composition of the fired ceramic can be controlled. Fibers can be spun from the melt which are stable in argon in 1400 C. The silsesquioxanes also were used as matrix precursors for Nicalon and alpha-SiC platelet reinforced composites.

High rate capacitive performance of single-walled carbon nanotube aerogels

DOE PAGES

Van Aken, Katherine L.; Pérez, Carlos R.; Oh, Youngseok; ...

2015-05-30

Single-walled carbon nanotube (SWCNT) aerogels produced by critical-point-drying of wet-gel precursors exhibit unique properties, such as high surface-area-to-volume and strength-to-weight ratios. They are free-standing, are binder-free, and can be scaled to thicknesses of more than 1 mm. In this paper, we examine the electric double layer capacitive behavior of these materials using a common room temperature ionic liquid electrolyte, 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide (EMI-TFSI). Electrochemical performance is assessed through galvanostatic cycling, cyclic voltammetry and impedance spectroscopy. Results indicate stable capacitive performance over 10,000 cycles as well as an impressive performance at high charge and discharge rates, due to accessible pore networks andmore » enhanced electronic and ionic conductivities of SWCNT aerogels. Finally, these materials can find applications in mechanically compressible and flexible supercapacitor devices with high power requirements.« less

Dissolved organic carbon concentrations and compositions, and trihalomethane formation potentials in waters from agricultural peat soils, Sacramento-San Joaquin Delta, California; implications for drinking-water quality

USGS Publications Warehouse

Fujii, Roger; Ranalli, Anthony J.; Aiken, George R.; Bergamaschi, Brian A.

1998-01-01

Water exported from the Sacramento-San Joaquin River delta (Delta) is an important drinking-water source for more than 20 million people in California. At times, this water contains elevated concentrations of dissolved organic carbon and bromide, and exceeds the U.S. Environmental Protection Agency's maximum contaminant level for trihalomethanes of 0.100 milligrams per liter if chlorinated for drinking water. About 20 to 50 percent of the trihalomethane precursors to Delta waters originates from drainage water from peat soils on Delta islands. This report elucidates some of the factors and processes controlling and affecting the concentration and quality of dissolved organic carbon released from peat soils and relates the propensity of dissolved organic carbon to form trihalomethanes to its chemical composition.Soil water was sampled from near-surface, oxidized, well-decomposed peat soil (upper soil zone) and deeper, reduced, fibrous peat soil (lower soil zone) from one agricultural field in the west central Delta over 1 year. Concentrations of dissolved organic carbon in the upper soil zone were highly variable, with median concentrations ranging from 46.4 to 83.2 milligrams per liter. Concentrations of dissolved organic carbon in samples from the lower soil zone were much less variable and generally slightly higher than samples from the upper soil zone, with median concentrations ranging from 49.3 to 82.3 milligrams per liter. The dissolved organic carbon from the lower soil zone had significantly higher aromaticity (as measured by specific ultraviolet absorbance) and contained significantly greater amounts of aromatic humic substances (as measured by XAD resin fractionation and carbon-13 nuclear magnetic resonance analysis of XAD isolates) than the dissolved organic carbon from the upper soil zone. These results support the conclusion that more aromatic forms of dissolved organic carbon are produced under anaerobic conditions compared to aerobic conditions. Dissolved organic carbon concentration, trihalomethane formation potential, and ultraviolet absorbance were all highly correlated, showing that trihalomethane precursors increased with increasing dissolved organic carbon and ultraviolet absorbance for whole water samples. Contrary to the generally accepted conceptual model for trihalomethane formation that assumes that aromatic forms of carbon are primary precursors to trihalomethanes, results from this study indicate that dissolved organic carbon aromaticity appears unrelated to trihalomethane formation on a carbon-normalized basis. Thus, dissolved organic carbon aromaticity alone cannot fully explain or predict trihalomethane precursor content, and further investigation of aromatic and nonaromatic forms of carbon will be needed to better identify trihalomethane precursors.

Hydrothermal replacement of biogenic and abiogenic aragonite by Mg-carbonates - Relation between textural control on effective element fluxes and resulting carbonate phase

NASA Astrophysics Data System (ADS)

Jonas, Laura; Müller, Thomas; Dohmen, Ralf; Immenhauser, Adrian; Putlitz, Benita

2017-01-01

Dolomitization, i.e., the secondary replacement of calcite or aragonite (CaCO3) by dolomite (CaMg[CO3]2), is one of the most volumetrically important carbonate diagenetic processes. It occurs under near surface and shallow burial conditions and can significantly modify rock properties through changes in porosity and permeability. Dolomitization fronts are directly coupled to fluid pathways, which may be related to the initial porosity/permeability of the precursor limestone, an existing fault network or secondary porosity/permeability created through the replacement reaction. In this study, the textural control on the replacement of biogenic and abiogenic aragonite by Mg-carbonates, that are typical precursor phases in the dolomitization process, was experimentally studied under hydrothermal conditions. Aragonite samples with different textural and microstructural properties exhibiting a compact (inorganic aragonite single crystal), an intermediate (bivalve shell of Arctica islandica) and open porous structure (skeleton of coral Porites sp.) were reacted with a solution of 0.9 M MgCl2 and 0.015 M SrCl2 at 200 °C. The replacement of aragonite by a Ca-bearing magnesite and a Mg-Ca carbonate of non-stoichiometric dolomitic composition takes place via a dissolution-precipitation process and leads to the formation of a porous reaction front that progressively replaces the aragonite precursor. The reaction leads to the development of porosity within the reaction front and distinctive microstructures such as gaps and cavities at the reaction interface. The newly formed reaction rim consists of chemically distinct phases separated by sharp boundaries. It was found that the number of phases and their chemical variation decreases with increasing initial porosity and reactive surface area. This observation is explained by variations in effective element fluxes that result in differential chemical gradients in the fluid within the pore space of the reaction rim. Observed reaction rates are highest for the replacement of the initially highly porous coral and lowest for the compact structure of a single aragonite crystal. Therefore, the reaction progress equally depends on effective element fluxes between the fluid at the reaction interface and the bulk solution surrounding the test material as well as the reactive surface area. This study demonstrates that the textural and microstructural properties of the parent material have a significant influence on the chemical composition of the product phase. Moreover, our data highlight the importance of effective fluid-mediated element exchange between the fluid at the reaction interface and the bulk solution controlled by the local microstructure.

Synthesis of SnO2 pillared carbon using long chain alkylamine grafted graphene oxide: an efficient anode material for lithium ion batteries.

PubMed

Reddy, M Jeevan Kumar; Ryu, Sung Hun; Shanmugharaj, A M

2016-01-07

With the objective of developing new advanced composite materials that can be used as anodes for lithium ion batteries (LIBs), herein we describe the synthesis of SnO2 pillared carbon using various alkylamine (hexylamine; dodecylamine and octadecylamine) grafted graphene oxides and butyl trichlorotin precursors followed by its calcination at 500 °C for 2 h. While the grafted alkylamine induces crystalline growth of SnO2 pillars, thermal annealing of alkylamine grafted graphene oxide results in the formation of amorphous carbon coated graphene. Field emission scanning electron microscopy (FE-SEM) results reveal the successful formation of SnO2 pillared carbon on the graphene surface. X-ray diffraction (XRD), transmission electron microscopy (TEM) and Raman spectroscopy characterization corroborates the formation of rutile SnO2 crystals on the graphene surface. A significant rise in the BET surface area is observed for SnO2 pillared carbon, when compared to pristine GO. Electrochemical characterization studies of SnO2 pillared carbon based anode materials showed an enhanced lithium storage capacity and fine cyclic performance in comparison with pristine GO. The initial specific capacities of SnO2 pillared carbon are observed to be 1379 mA h g(-1), 1255 mA h g(-1) and 1360 mA h g(-1) that decrease to 750 mA h g(-1), 643 mA h g(-1) and 560 mA h g(-1) depending upon the chain length of grafted alkylamine on the graphene surface respectively. Electrochemical impedance spectral analysis reveals that the exchange current density of SnO2 pillared carbon based electrodes is higher, corroborating its enhanced electrochemical activity in comparison with GO based electrodes.

Convenient and large-scale synthesis of nitrogen-rich hierarchical porous carbon spheres for supercapacitors and CO2 capture

NASA Astrophysics Data System (ADS)

Chang, Binbin; Zhang, Shouren; Yin, Hang; Yang, Baocheng

2017-08-01

Herein, considering the great potential of nitrogen-doped hierarchical porous carbons in energy storage and CO2 capture, we designed a convenient and easily large-scale production strategy for preparing nitrogen-doped hierarchical porous carbon sphere (NHPCS) materials. In this synthesis route, spherical resorcinol-formaldehyde (RF) resins were selected as carbon precursor, and then the ZnCl2-impregnated RF resin spheres were carbonized in a NH3 atmosphere at a temperature range of 600-800 °C. During the one-step heat-treatment process, nitrogen atom could be efficiently incorporated into the carbon skeleton, and the interconnected and hierarchical pore structure with different micro/mesopore proportion could be generated and tuned by adjusting the activating agent ZnCl2 dosage and carbonization temperature. The resultant nitrogen-doped hierarchical porous carbon sphere materials exhibited a satisfactory charge storage capacity, and the optimal sample of NHPCS-2-8 with a high mesopore proportion obtained at 800 °C with a ZnCl2/RF mass ratio of 2:1 presented a specific capacitance of 273.8 F g-1 at a current density of 0.5 A g-1. More importantly, the assembled NHPCS-2-8-based symmetric capacitor displayed a high energy density of 17.2 Wh kg-1 at a power density of 178.9 W kg-1 within a voltage window of 0 ∼ 1.8 V in 0.5 M Na2SO4 aqueous electrolyte. In addition, the CO2 capture application of these NHPCS materials was also explored, and the optimal sample of NHPCS-0-8 with a large micropore proportion prepared at 800 °C exhibited an exceptional CO2 uptake capacity at ambient pressures of up to 4.23 mmol g-1 at 0 °C.

Deposition of amorphous carbon thin films by aerosol-assisted CVD method

NASA Astrophysics Data System (ADS)

Fadzilah, A. N.; Dayana, K.; Rusop, M.

2018-05-01

This paper reports on the deposition of amorphous carbon (a-C) by Aerosol-assisted Chemical Vapor Deposition (AACVD) using natural source of camphor oil as the precursor material. 4 samples were deposited at 4 different deposition flow rate from 15 sccm to 20 sccm, with 5 sccm interval for each sample. The analysis includes the electrical, optical and structural analysis of the data. The a-C structure which came from the manipulation of synthesis parameter was characterized by the solar simulator system, UV-VIS-NIR, Raman spectroscope and AFM. The properties of a-C are highly dependent on the deposition techniques and deposition parameters; hence the influences of gas flow rate were studied.

Rapid synthesis of N, S co-doped carbon dots and their application for Fe3+ ion detection

NASA Astrophysics Data System (ADS)

Zhang, Jian; Wang, Junbin; Fu, Jinping; Fu, Xucheng; Gan, Wei; Hao, Hequn

2018-02-01

In this study, nitrogen and sulfur co-doped carbon dots (NSCDs) were fabricated by microwave-assisted one-pot synthesis using vitamin C and thiourea as precursors. The as-prepared NSCDs demonstrated excellent properties, including aqueous dispensability, strong fluorescence emission, excellent environmental stability, high selectivity, and sensitivity toward Fe3+ ions. The NSCD-based material can be used as a "turn off" fluorescent probe for detecting Fe3+ ions at a low detection limit (4.2 nM). In addition, the "turn off" and "turn on" of NSCD fluorescent probe could be modulated by adding Fe3+ and EDTA, indicating weak interaction between the Fe3+ ions and NSCDs.

Trihalomethane formation potential of aquatic and terrestrial fulvic and humic acids: Sorption on activated carbon.

PubMed

Abouleish, Mohamed Y Z; Wells, Martha J M

2015-07-15

Humic substances (HSs) are precursors for the formation of hazardous disinfection by-products (DBPs) during chlorination of water. Various surrogate parameters have been used to investigate the generation of DBPs by HS precursors and the removal of these precursors by activated carbon treatment. Dissolved organic carbon (DOC)- and ultraviolet absorbance (UVA254)-based isotherms are commonly reported and presumed to be good predictors of the trihalomethane formation potential (THMFP). However, THMFP-based isotherms are rarely published such that the three types of parameters have not been compared directly. Batch equilibrium experiments on activated carbon were used to generate constant-initial-concentration sorption isotherms for well-characterized samples obtained from the International Humic Substances Society (IHSS). HSs representing type (fulvic acid [FA], humic acid [HA]), origin (aquatic, terrestrial), and geographical source (Nordic, Suwannee, Peat, Soil) were examined at pH6 and pH9. THMFP-based isotherms were generated and compared to determine if DOC- and UVA254-based isotherms were good predictors of the THMFP. The sorption process depended on the composition of the HSs and the chemical nature of the activated carbon, both of which were influenced by pH. Activated carbon removal of THM-precursors was pH- and HS-dependent. In some instances, the THMFP existed after UVA254 was depleted. Copyright © 2015 Elsevier B.V. All rights reserved.

Adsorption of N-nitrosodimethylamine precursors by powdered and granular activated carbon.

PubMed

Hanigan, David; Zhang, Jinwei; Herckes, Pierre; Krasner, Stuart W; Chen, Chao; Westerhoff, Paul

2012-11-20

Activated carbon (AC) has been shown to remove precursors of halogenated disinfection byproducts. Granular and powdered activated carbon (GAC, PAC) were investigated for their potential to adsorb N-nitrosodimethylamine (NDMA) precursors from blends of river water and effluent from a wastewater treatment plant (WWTP). At bench scale, waters were exposed to lignite or bituminous AC, either as PAC in bottle point experiments or as GAC in rapid small-scale column tests (RSSCTs). NDMA formation potential (FP) was used as a surrogate for precursor removal. NDMA FP was reduced by 37, 59, and 91% with 3, 8, and 75 mg/L of one PAC, respectively, with a 4-h contact time. In RSSCTs and in full-scale GAC contactors, NDMA FP removal always exceeded that of the bulk dissolved organic carbon (DOC) and UV absorbance at 254 nm. For example, whereas DOC breakthrough exceeded 90% of its influent concentration after 10,000 bed volumes of operation in an RSSCT, NDMA FP was less than 40% of influent concentration after the same bed life of the GAC. At full or pilot scale, high NDMA FP reduction ranging from >60 to >90% was achieved across GAC contactors, dependent upon the GAC bed life and/or use of a preoxidant (chlorine or ozone). In all experiments, NDMA formation was not reduced to zero, which suggests that although some precursors are strongly sorbed, others are not. This is among the first studies to show that AC is capable of adsorbing NDMA precursors, but further research is needed to better understand NDMA precursor chemical properties (e.g., hydrophobicity, molecular size) and evaluate how best to incorporate this finding into full-scale designs and practice.

Synthesis of Dispersible Mesoporous Nitrogen-Doped Hollow Carbon Nanoplates with Uniform Hexagonal Morphologies for Supercapacitors.

PubMed

Cao, Jie; Jafta, Charl J; Gong, Jiang; Ran, Qidi; Lin, Xianzhong; Félix, Roberto; Wilks, Regan G; Bär, Marcus; Yuan, Jiayin; Ballauff, Matthias; Lu, Yan

2016-11-02

In this study, dispersible mesoporous nitrogen-doped hollow carbon nanoplates have been synthesized as a new anisotropic carbon nanostructure using gibbsite nanoplates as templates. The gibbsite-silica core-shell nanoplates were first prepared before the gibbsite core was etched away. Dopamine as carbon precursor was self-polymerized on the hollow silica nanoplates surface assisted by sonification, which not only favors a homogeneous polymer coating on the nanoplates but also prevents their aggregation during the polymerization. Individual silica-polydopamine core-shell nanoplates were immobilized in a silica gel in an insulated state via a silica nanocasting technique. After pyrolysis in a nanoconfine environment and elimination of silica, discrete and dispersible hollow carbon nanoplates are obtained. The resulted hollow carbon nanoplates bear uniform hexagonal morphology with specific surface area of 460 m 2 ·g -1 and fairly accessible small mesopores (∼3.8 nm). They show excellent colloidal stability in aqueous media and are applied as electrode materials for symmetric supercapacitors. When using polyvinylimidazolium-based nanoparticles as a binder in electrodes, the hollow carbon nanoplates present superior performance in parallel to polyvinylidene fluoride (PVDF) binder.

Application of the Taguchi analytical method for optimization of effective parameters of the chemical vapor deposition process controlling the production of nanotubes/nanobeads.

PubMed

Sharon, Maheshwar; Apte, P R; Purandare, S C; Zacharia, Renju

2005-02-01

Seven variable parameters of the chemical vapor deposition system have been optimized with the help of the Taguchi analytical method for getting a desired product, e.g., carbon nanotubes or carbon nanobeads. It is observed that almost all selected parameters influence the growth of carbon nanotubes. However, among them, the nature of precursor (racemic, R or Technical grade camphor) and the carrier gas (hydrogen, argon and mixture of argon/hydrogen) seem to be more important parameters affecting the growth of carbon nanotubes. Whereas, for the growth of nanobeads, out of seven parameters, only two, i.e., catalyst (powder of iron, cobalt, and nickel) and temperature (1023 K, 1123 K, and 1273 K), are the most influential parameters. Systematic defects or islands on the substrate surface enhance nucleation of novel carbon materials. Quantitative contributions of process parameters as well as optimum factor levels are obtained by performing analysis of variance (ANOVA) and analysis of mean (ANOM), respectively.

In situ formation of titanium carbide using titanium and carbon-nanotube powders by laser cladding

NASA Astrophysics Data System (ADS)

Savalani, M. M.; Ng, C. C.; Li, Q. H.; Man, H. C.

2012-01-01

Titanium metal matrix composite coatings are considered to be important candidates for high wear resistance applications. In this study, TiC reinforced Ti matrix composite layers were fabricated by laser cladding with 5, 10, 15 and 20 wt% carbon-nanotube. The effects of the carbon-nanotube content on phase composition, microstructure, micro-hardness and dry sliding wear resistance of the coating were studied. Microstructural observation using scanning electron microscopy showed that the coatings consisted of a matrix of alpha-titanium phases and the reinforcement phase of titanium carbide in the form of fine dendrites, indicating that titanium carbide was synthesized by the in situ reaction during laser irradiation. Additionally, measurements on the micro-hardness and dry sliding wear resistance of the coatings indicated that the mechanical properties were affected by the amount of carbon-nanotube in the starting precursor materials and were enhanced by increasing the carbon-nanotube content. Results indicated that the composite layers exhibit high hardness and excellent wear resistance.

Hierarchical Nanostructures of Nitrogen-Doped Porous Carbon Polyhedrons Confined in Carbon Nanosheets for High-Performance Supercapacitors.

PubMed

Zhao, Zhe; Liu, Siliang; Zhu, Jixin; Xu, Jingsan; Li, Le; Huang, Zhaoqi; Zhang, Chao; Liu, Tianxi

2018-05-31

Interconnected close-packed nitrogen-doped porous carbon polyhedrons (NCPs) confined in two-dimensional carbon nanosheets (CNSs) have been prepared through a sustainable one-pot pyrolysis of a simple solid mixture of zeolitic imidazolate framework-8 (ZIF-8) crystals and with organic potassium as the precursors. The hierarchically organized framework of the NCP-CNS composites enables NCPs and CNSs to act as well-defined electrolyte reservoirs and mechanical buffers accommodating large volume expansions of NCPs, respectively. Among the unique composite nanostructures, the NCPs with vast micropores provide electric double-layer capacitances, while the CNSs bridge the individual NCPs to form a conductive pathway with a hierarchical porosity. As a result, the NCP-CNS composites with high electrical integrity and structural stability are used as electrode materials for high-performance supercapacitors, which exhibit excellent electrochemical capacitive characteristics in terms of an outstanding capacitance of 300 F g -1 at 1 A g -1 , large energy density of 20.9 W h kg -1 , and great cycling performance of 100% retention after 6000 cycles. This work therefore presents a one-pot and efficient strategy to prepare an ordered arrangement of ZIF-8-derived porous carbons toward new electrode materials in promising energy storage systems.

Recent Progress in Producing Lignin-Based Carbon Fibers for Functional Applications

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

Paul, Ryan; Burwell, Deanna; Dai, Xuliang

Lignin, a biopolymer, has been investigated as a renewable and low-cost carbon fiber precursor since the 1960s. Although successful lab-scale production of lignin-based carbon fibers has been reported, there are currently not any commercial producers. This paper will highlight some of the known challenges with converting lignin-based precursors into carbon fiber, and the reported methods for purifying and modifying lignin to improve it as a precursor. Several of the challenges with lignin are related to its diversity in chemical structure and purity, depending on its biomass source (e.g. hardwood, softwood, grasses) and extraction method (e.g. organosolv, kraft). In order tomore » make progress in this field, GrafTech and Oak Ridge National Laboratory are collaborating to develop lignin-based carbon fiber technology and to demonstrate it in functional applications, as part of a cooperative agreement with the DOE Advanced Manufacturing Office. The progress made to date with producing lignin-based carbon fiber for functional applications, as well as developing and qualifying a supply chain and value proposition, are also highlighted.« less

Electrical conductivity of activated carbon-metal oxide nanocomposites under compression: a comparison study.

PubMed

Barroso-Bogeat, A; Alexandre-Franco, M; Fernández-González, C; Macías-García, A; Gómez-Serrano, V

2014-12-07

From a granular commercial activated carbon (AC) and six metal oxide (Al2O3, Fe2O3, SnO2, TiO2, WO3 and ZnO) precursors, two series of AC-metal oxide nanocomposites were prepared by wet impregnation, oven-drying at 120 °C, and subsequent heat treatment at 200 or 850 °C in an inert atmosphere. Here, the electrical conductivity of the resulting products was studied under moderate compression. The influence of the applied pressure, sample volume, mechanical work, and density of the hybrid materials was thoroughly investigated. The DC electrical conductivity of the compressed samples was measured at room temperature by the four-probe method. Compaction assays suggest that the mechanical properties of the nanocomposites are largely determined by the carbon matrix. Both the decrease in volume and the increase in density were relatively small and only significant at pressures lower than 100 kPa for AC and most nanocomposites. In contrast, the bulk electrical conductivity of the hybrid materials was strongly influenced by the intrinsic conductivity, mean crystallite size, content and chemical nature of the supported phases, which ultimately depend on the metal oxide precursor and heat treatment temperature. The supported nanoparticles may be considered to act as electrical switches either hindering or favouring the effective electron transport between the AC cores of neighbouring composite particles in contact under compression. Conductivity values as a rule were lower for the nanocomposites than for the raw AC, all of them falling in the range of semiconductor materials. With the increase in heat treatment temperature, the trend is toward the improvement of conductivity due to the increase in the crystallite size and, in some cases, to the formation of metals in the elemental state and even metal carbides. The patterns of variation of the electrical conductivity with pressure and mechanical work were slightly similar, thus suggesting the predominance of the pressure effects rather than the volume ones.

Molecular aspects of aromatic C additions to soils: Implications of char quality for ecosystem functionality

NASA Astrophysics Data System (ADS)

Keiluweit, M.; Nico, P. S.; Johnson, M. G.; Kleber, M.

2009-12-01

Solid residues of incomplete combustion (biochar or char) are continuously being added to soils due to natural vegetation fires in many ecosystems. However, new strategies for carbon sequestration in soils are likely to include the active addition of biochar to soils. Since biochar is a highly aromatic organic material such additions will modify the native molecular structure of soil organic matter and thus alter interactions with the global atmosphere and hydrosphere. Here we present a molecular level assessment of the physical organization and chemical complexity of biomass-derived chars and, specifically, that of aromatic carbon in char structures. Differences among wood and grass charred at temperatures from 100 to 700°C are investigated. BET-N2 surface area, X-ray diffraction (XRD), synchrotron-based Near-edge X-ray Absorption Fine Structure (NEXAFS) and Fourier transform infrared (FT-IR) spectroscopy results demonstrate how the two plant precursor materials undergo analogous, but quantitatively different physical-chemical transitions as charring intensity increases. These changes suggest the existence of four distinct physical and chemical categories of char. We find that each category of char consists of a unique mixture of chemical phases and physical states: (i) in transition chars the crystalline character of the precursor materials is preserved, (ii) in amorphous chars the heat-altered molecules and incipient aromatic polycondensates are randomly mixed, (iii) composite chars consist of poorly ordered graphene stacks embedded in amorphous phases, and (iv) turbostratic chars are dominated by turbostratic (disordered) graphitic crystallites. There is wide variation in both the chemical and the physical nature of aromatic carbon among these char categories. In this presentation we will point out how molecular variations among the aromatic components of the different char categories translate into differences in their ability to: (i) persist in the environment, (ii) function as environmental sorbents, and (iii) to enable the soil to provide environmental services.

Facile Synthesis of Highly Aligned Multiwalled Carbon Nanotubes from Polymer Precursors

DOE PAGES

Han, Catherine Y.; Xiao, Zhi-Li; Wang, H. Hau; ...

2009-01-01

We report a facile one-step approach which involves no flammable gas, no catalyst, and no in situ polymerization for the preparation of well-aligned carbon nanotube array. A polymer precursor is placed on top of an anodized aluminum oxide (AAO) membrane containing regular nanopore arrays, and slow heating under Ar flow allows the molten polymer to wet the template through adhesive force. The polymer spread into the nanopores of the template to form polymer nanotubes. Upon carbonization the resulting multi-walled carbon nanotubes duplicate the nanopores morphology precisely. The process is demonstrated for 230, 50, and 20 nm pore membranes. The synthesized carbonmore » nanotubes are characterized with scanning/transmission electron microscopies, Raman spectroscopy, and resistive measurements. Convenient functionalization of the nanotubes with this method is demonstrated through premixing CoPt nanoparticles in the polymer precursors.« less

Gas-Flow Tailoring Fabrication of Graphene-like Co-Nx-C Nanosheet Supported Sub-10 nm PtCo Nanoalloys as Synergistic Catalyst for Air-Cathode Microbial Fuel Cells.

PubMed

Cao, Chun; Wei, Liling; Zhai, Qiran; Ci, Jiliang; Li, Weiwei; Wang, Gang; Shen, Jianquan

2017-07-12

In this work, we presented a novel, facile, and template-free strategy for fabricating graphene-like N-doped carbon as oxygen reduction catalyst in sustainable microbial fuel cells (MFCs) by using an ion-inducing and spontaneous gas-flow tailoring effect from a unique nitrogen-rich polymer gel precursor which has not been reported in materials science. Remarkably, by introduction of trace platinum- and cobalt- precursor in polymer gel, highly dispersed sub-10 nm PtCo nanoalloys can be in situ grown and anchored on graphene-like carbon. The as-prepared catalysts were investigated by a series of physical characterizations, electrochemical measurements, and microbial fuel cell tests. Interestingly, even with a low Pt content (5.13 wt %), the most active Co/N codoped carbon supported PtCo nanoalloys (Co-N-C/Pt) exhibited dramatically improved catalytic activity toward oxygen reduction reaction coupled with superior output power density (1008 ± 43 mW m -2 ) in MFCs, which was 29.40% higher than the state of the art Pt/C (20 wt %). Notability, the distinct catalytic activity of Co-N-C/Pt was attributed to the highly efficient synergistic catalytic effect of Co-Nx-C and PtCo nanoalloys. Therefore, Co-N-C/Pt should be a promising oxygen reduction catalyst for application in MFCs. Further, the novel strategy for graphene-like carbon also can be widely used in many other energy conversion and storage devices.

Chitin based heteroatom-doped porous carbon as electrode materials for supercapacitors.

PubMed

Zhou, Jie; Bao, Li; Wu, Shengji; Yang, Wei; Wang, Hui

2017-10-01

Chitin biomass has received much attention as an amino-functional polysaccharide precursor for synthesis of carbon materials. Rich nitrogen and oxygen dual-doped porous carbon derived from cicada slough (CS), a renewable biomass mainly composed of chitin, was synthesized and employed as electrode materials for electrochemical capacitors, for the first time ever. The cicada slough-derived carbon (CSC) was prepared by a facile process via pre-carbonization in air, followed by KOH activation. The weight ratio of KOH and char plays an important role in fabricating the microporous structure and tuning the surface chemistry of CSC. The obtained CSC had a large specific surface area (1243-2217m 2 g -1 ), fairly high oxygen content (28.95-33.78 at%) and moderate nitrogen content (1.47-4.35 at%). The electrochemical performance of the CS char and CSC as electrodes for capacitors was evaluated in a three-electrode cell configuration with 6M KOH as the electrolyte. Electrochemical studies showed that the as-prepared CSC activated at the KOH-to-char weight ratio of 2 exhibited the highest specific capacitance (266.5Fg -1 at a current density of 0.5Ag -1 ) and excellent rate capability (196.2Fg -1 remained at 20Ag -1 ) and cycle durability. In addition, the CSC-2-based symmetrical device possessed the desirable energy density and power density of about 15.97Whkg -1 and 5000Wkg -1 at 5Ag -1 , respectively. Copyright © 2017 Elsevier Ltd. All rights reserved.

The enhancement in electrical analysis of the nitrogen doped amorphous carbon thin films (a-C:N) prepared by aerosol-assisted CVD

NASA Astrophysics Data System (ADS)

Fadzilah, A. N.; Dayana, K.; Rusop, M.

2018-05-01

This paper reports on the deposition of Nitrogen doped amorphous carbon (a-C:N) by Aerosol-assisted Chemical Vapor Deposition (AACVD) using natural source of camphor oil as the precursor material. 5 samples were deposited at 5 different deposition times from 15 min to 90 min, with 15 min interval for each sample. The highest slope of linear graph was noted at the sample with 45 min deposition time, showing the lowest electrical resistance of the sample. From I-V characteristic, the sample deposited at 45 min has the highest electrical conductivity due to high sp2 carbon bonding ratio. Nanostructured behavior of N doped a-C:N was also investigated by FESEM micrograph resulting with the particle size less than 100nm.

From Carbon-Based Nanotubes to Nanocages for Advanced Energy Conversion and Storage.

PubMed

Wu, Qiang; Yang, Lijun; Wang, Xizhang; Hu, Zheng

2017-02-21

Carbon-based nanomaterials have been the focus of research interests in the past 30 years due to their abundant microstructures and morphologies, excellent properties, and wide potential applications, as landmarked by 0D fullerene, 1D nanotubes, and 2D graphene. With the availability of high specific surface area (SSA), well-balanced pore distribution, high conductivity, and tunable wettability, carbon-based nanomaterials are highly expected as advanced materials for energy conversion and storage to meet the increasing demands for clean and renewable energies. In this context, attention is usually attracted by the star material of graphene in recent years. In this Account, we overview our studies on carbon-based nanotubes to nanocages for energy conversion and storage, including their synthesis, performances, and related mechanisms. The two carbon nanostructures have the common features of interior cavity, high conductivity, and easy doping but much different SSAs and pore distributions, leading to different performances. We demonstrated a six-membered-ring-based growth mechanism of carbon nanotubes (CNTs) with benzene precursor based on the structural similarity of the benzene ring to the building unit of CNTs. By this mechanism, nitrogen-doped CNTs (NCNTs) with homogeneous N distribution and predominant pyridinic N were obtained with pyridine precursor, providing a new kind of support for convenient surface functionalization via N-participation. Accordingly, various transition-metal nanoparticles were directly immobilized onto NCNTs without premodification. The so-constructed catalysts featured high dispersion, narrow size distribution and tunable composition, which presented superior catalytic performances for energy conversions, for example, the oxygen reduction reaction (ORR) and methanol oxidation in fuel cells. With the advent of the new field of carbon-based metal-free electrocatalysts, we first extended ORR catalysts from the electron-rich N-doped to the electron-deficient B-doped sp 2 carbon. The combined experimental and theoretical study indicated the ORR activity originated from the activation of carbon π electrons by breaking the integrity of π conjugation, despite the electron-rich or electron-deficient nature of the dopants. With this understanding, metal-free electrocatalysts were further extended to the dopant-free defective carbon nanomaterials. Moreover, we developed novel 3D hierarchical carbon-based nanocages by the in situ MgO template method, which featured coexisting micro-meso-macropores and much larger SSA than the nanotubes. The unique 3D architecture avoids the restacking generally faced by 2D graphene due to the intrinsic π-π interaction. Consequently, the hierarchical nanocages presented superior performances not only as new catalyst supports and metal-free electrocatalysts but also as electrode materials for energy storage. State-of-the-art supercapacitive performances were achieved with high energy density and power density, as well as excellent rate capability and cycling stability. The large interior space of the nanocages enabled the encapsulation of high-loading sulfur to alleviate polysulfide dissolution while greatly enhancing the electron conduction and Li-ion diffusion, leading to top level performance of lithium-sulfur battery. These results not only provide unique carbon-based nanomaterials but also lead to in-depth understanding of growth mechanisms, material design, and structure-performance relationships, which is significant to promote their energy applications and also to enrich the exciting field of carbon-based nanomaterials.

From Bench Top to Market: Growth of Multi-Walled Carbon Nanotubes by Injection CVD Using Fe Organometallics - Production of a Commercial Reactor

NASA Technical Reports Server (NTRS)

Rowsell, J.; Hepp, A. F.; Harris, J. D.; Raffaelle, R. P.; Cowen, J. C.; Scheiman, D. A.; Flood, D. M.; Flood, D. J.

2009-01-01

Preferential oriented multiwalled carbon nanotubes were prepared by the injection chemical vapor deposition (CVD) method using either cyclopentadienyliron dicarbonyl dimer or cyclooctatetraene iron tricarbonyl as the iron catalyst source. The catalyst precursors were dissolved in toluene as the carrier solvent for the injections. The concentration of the catalyst was found to influence both the growth (i.e., MWNT orientation) of the nanotubes, as well as the amount of iron in the deposited material. As deposited, the multiwalled carbon nanotubes contained as little as 2.8% iron by weight. The material was deposited onto tantalum foil and fused silica substrates. The nanotubes were characterized by scanning electron microscopy, transmission electron microscopy, Raman spectroscopy and thermogravimetric analysis. This synthetic route provides a simple and scalable method to deposit MWNTs with a low defect density, low metal content and a preferred orientation. Subsequently, a small start-up was founded to commercialize the deposition equipment. The contrast between the research and entrepreneurial environments will be discussed.

Cellular control over spicule formation in sea urchin embryos: A structural approach.

PubMed

Beniash, E; Addadi, L; Weiner, S

1999-03-01

The spicules of the sea urchin embryo form in intracellular membrane-delineated compartments. Each spicule is composed of a single crystal of calcite and amorphous calcium carbonate. The latter transforms with time into calcite by overgrowth of the preexisting crystal. Relationships between the membrane surrounding the spiculogenic compartment and the spicule mineral phase were studied in the transmission electron microscope (TEM) using freeze-fracture. In all the replicas observed the spicules were tightly surrounded by the membrane. Furthermore, a variety of structures that are related to the material exchange process across the membrane were observed. The spiculogenic cells were separated from other cell types of the embryo, frozen, and freeze-dried on the TEM grids. The contents of electron-dense granules in the spiculogenic cells were shown by electron diffraction to be composed of amorphous calcium carbonate. These observations are consistent with the notion that the amorphous calcium carbonate-containing granules contain the precursor mineral phase for spicule formation and that the membrane surrounding the forming spicule is involved both in transport of material and in controlling spicule mineralization. Copyright 1999 Academic Press.

Preparation of porous carbon spheres from 2-keto-l-gulonic acid mother liquor by oxidation and activation for electric double-layer capacitor application.

PubMed

Hao, Zhi-Qiang; Cao, Jing-Pei; Zhao, Xiao-Yan; Wu, Yan; Zhu, Jun-Sheng; Dang, Ya-Li; Zhuang, Qi-Qi; Wei, Xian-Yong

2018-03-01

A novel strategy is proposed for the increase of specific surface area (SSA) of porous carbon sphere (PCS) by oxidation and activation. 2-keto-l-gulonic acid mother liquor (GAML) as a high-pollution waste has a relatively high value of reutilization. For its high value-added utilization, GAML is used as the precursor for preparation of PCS as carbon-based electrode materials for electric double-layer capacitor. PCS is prepared by hydrothermal carbonization, carbonization and KOH activation, and Fe(NO 3 ) 3 9H 2 O is used as an oxidizing agent during carbonization. The as-prepared PCS has excellent porosity and high SSA of 2478 m 2  g -1 . Meanwhile, the pore structure of PCS can be controlled by the adjustment of carbonization parameters (carbonization temperature and the loading of Fe(NO 3 ) 3 9H 2 O). Besides, the SSA and specific capacitance of PCS can be increased remarkably when Fe(NO 3 ) 3 9H 2 O is added in carbonization. The specific capacitance of PCS can reach 303.7 F g -1 at 40 mA g -1 . PCSs as electrode material have superior electrochemical stability. After 8000 cycles, the capacitance retention is 98.3% at 2 A g -1 . The electric double-layer capacitance of PCS is improved when CS is carbonized with Fe(NO 3 ) 3 9H 2 O, and the economic and environmental benefits are achieved by the effective recycle of GAML. Copyright © 2017 Elsevier Inc. All rights reserved.

An efficient synthesis of graphenated carbon nanotubes over the tailored mesoporous molecular sieves by chemical vapor deposition

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

Atchudan, R.; Department of Chemistry, CEG Campus, Anna University, Chennai 600025; Joo, Jin., E-mail: joojin@knu.ac.kr

2013-06-01

Highlights: ► Tailored 3D cubic Ni/KIT-6 with large pores was synthesized successfully. ► The new hybrid g-CNTs in large scale were synthesized using Ni/KIT-6 by CVD method. ► The use of mesoporous material by CVD method would be an ideal choice to prepare g-CNTs at reasonable cost. ► This type of g-CNTs might be a new avenue for nano-electronic applications. - Abstract: The new hybrid of graphenated carbon nanotubes (g-CNTs) was superior to either CNTs or graphene. Mesoporous 3D cubic Ni/KIT-6 were synthesized hydrothermally through organic template route and then were used as catalytic template for the production of g-CNTsmore » using acetylene as a carbon precursor by chemical vapor deposition (CVD) method. The deposited new hybrid carbon materials were purified and analyzed by various physico-chemical techniques such as XRD, TGA, SEM, TEM and Raman spectroscopy techniques. The graphitization of CNTs was confirmed by TGA and HRTEM studies. Thermal stability, surface morphology, and structural morphology of these materials were revealed by TGA, SEM and TEM analysis, respectively. Moreover, the tailored mesoporous Ni/KIT-6 molecular sieves were found to possess better quality and massive quantity of g-CNTs produced compared to other catalytic template route.« less

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

Faraby, H.; DiBattista, M.; Bandaru, P. R., E-mail: pbandaru@ucsd.edu

Metal deposition through focused ion beam (FIB) based systems is thought to result in material composed of the primary metal from the metallo-organic precursor in addition to carbon, oxygen, and gallium. We determined, through electrical resistance and chemical composition measurements on a wide range of FIB deposited platinum and tungsten lines, that the gallium ion (Ga{sup +}) concentration in the metal lines plays the dominant role in controlling the electrical resistivity. Effective medium theory, based on McLachlan's formalisms, was used to describe the relationship between the Ga{sup +} concentration and the corresponding resistivity.

Growth of High Quality Carbon Nanotubes on Free Standing Diamond Substrates

DTIC Science & Technology

2010-01-01

CNTs forming a mat of ~5 µm thickness and consisting of ~20 nm diameter tubes were observed to grow in a thermal CVD system using C2H2 as precursor...with CNT microfin architectures have been recently proposed by Kordas et al. [5]. CNT films as thermal interface materials were also discussed by Zhu...using a 1 inch diameter quartz tube in a horizontal furnace. Initially, the tube furnace was evacuated by using a rough pump and then purged with Ar

Adsorption Properties of Lignin-derived Activated Carbon Fibers (LACF)

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

Contescu, Cristian I.; Gallego, Nidia C.; Thibaud-Erkey, Catherine

The object of this CRADA project between Oak Ridge National Laboratory (ORNL) and United Technologies Research Center (UTRC) is the characterization of lignin-derived activated carbon fibers (LACF) and determination of their adsorption properties for volatile organic compounds (VOC). Carbon fibers from lignin raw materials were manufactured at Oak Ridge National Laboratory (ORNL) using the technology previously developed at ORNL. These fibers were physically activated at ORNL using various activation conditions, and their surface area and pore-size distribution were characterized by gas adsorption. Based on these properties, ORNL did down-select five differently activated LACF materials that were delivered to UTRC formore » measurement of VOC adsorption properties. UTRC used standard techniques based on breakthrough curves to measure and determine the adsorption properties of indoor air pollutants (IAP) - namely formaldehyde and carbon dioxide - and to verify the extent of saturated fiber regenerability by thermal treatments. The results are summarized as follows: (1) ORNL demonstrated that physical activation of lignin-derived carbon fibers can be tailored to obtain LACF with surface areas and pore size distributions matching the properties of activated carbon fibers obtained from more expensive, fossil-fuel precursors; (2) UTRC investigated the LACF potential for use in air cleaning applications currently pursued by UTRC, such as building ventilation, and demonstrated their regenerability for CO2 and formaldehyde, (3) Both partners agree that LACF have potential for possible use in air cleaning applications.« less

Non-PGM cathode catalysts for fuel cell application derived from heat treated heteroatomic amines precursors

DOEpatents

Serov, Alexey; Halevi, Barr; Artyushkova, Kateryna; Atanassov, Plamen B; Martinez, Ulises A

2017-04-25

A method of preparing M-N--C catalysts utilizing a sacrificial support approach and inexpensive and readily available polymer precursors as the source of nitrogen and carbon is disclosed. Exemplary polymer precursors include non-porphyrin precursors with no initial catalytic activity. Examples of suitable non-catalytic non-porphyrin precursors include, but are not necessarily limited to low molecular weight precursors that form complexes with iron such as 4-aminoantipirine, phenylenediamine, hydroxysuccinimide, ethanolamine, and the like.

Simultaneous removal of ammonia and N-nitrosamine precursors from high ammonia water by zeolite and powdered activated carbon.

PubMed

Xue, Runmiao; Donovan, Ariel; Zhang, Haiting; Ma, Yinfa; Adams, Craig; Yang, John; Hua, Bin; Inniss, Enos; Eichholz, Todd; Shi, Honglan

2018-02-01

When adding sufficient chlorine to achieve breakpoint chlorination to source water containing high concentration of ammonia during drinking water treatment, high concentrations of disinfection by-products (DBPs) may form. If N-nitrosamine precursors are present, highly toxic N-nitrosamines, primarily N-nitrosodimethylamine (NDMA), may also form. Removing their precursors before disinfection should be a more effective way to minimize these DBPs formation. In this study, zeolites and activated carbon were examined for ammonia and N-nitrosamine precursor removal when incorporated into drinking water treatment processes. The test results indicate that Mordenite zeolite can remove ammonia and five of seven N-nitrosamine precursors efficiently by single step adsorption test. The practical applicability was evaluated by simulation of typical drinking water treatment processes using six-gang stirring system. The Mordenite zeolite was applied at the steps of lime softening, alum coagulation, and alum coagulation with powdered activated carbon (PAC) sorption. While the lime softening process resulted in poor zeolite performance, alum coagulation did not impact ammonia and N-nitrosamine precursor removal. During alum coagulation, more than 67% ammonia and 70%-100% N-nitrosamine precursors were removed by Mordenite zeolite (except 3-(dimethylaminomethyl)indole (DMAI) and 4-dimethylaminoantipyrine (DMAP)). PAC effectively removed DMAI and DMAP when added during alum coagulation. A combination of the zeolite and PAC selected efficiently removed ammonia and all tested seven N-nitrosamine precursors (dimethylamine (DMA), ethylmethylamine (EMA), diethylamine (DEA), dipropylamine (DPA), trimethylamine (TMA), DMAP, and DMAI) during the alum coagulation process. Copyright © 2017. Published by Elsevier B.V.

Synthesis of SnO2 pillared carbon using long chain alkylamine grafted graphene oxide: an efficient anode material for lithium ion batteries

NASA Astrophysics Data System (ADS)

Reddy, M. Jeevan Kumar; Ryu, Sung Hun; Shanmugharaj, A. M.

2015-12-01

With the objective of developing new advanced composite materials that can be used as anodes for lithium ion batteries (LIBs), herein we describe the synthesis of SnO2 pillared carbon using various alkylamine (hexylamine; dodecylamine and octadecylamine) grafted graphene oxides and butyl trichlorotin precursors followed by its calcination at 500 °C for 2 h. While the grafted alkylamine induces crystalline growth of SnO2 pillars, thermal annealing of alkylamine grafted graphene oxide results in the formation of amorphous carbon coated graphene. Field emission scanning electron microscopy (FE-SEM) results reveal the successful formation of SnO2 pillared carbon on the graphene surface. X-ray diffraction (XRD), transmission electron microscopy (TEM) and Raman spectroscopy characterization corroborates the formation of rutile SnO2 crystals on the graphene surface. A significant rise in the BET surface area is observed for SnO2 pillared carbon, when compared to pristine GO. Electrochemical characterization studies of SnO2 pillared carbon based anode materials showed an enhanced lithium storage capacity and fine cyclic performance in comparison with pristine GO. The initial specific capacities of SnO2 pillared carbon are observed to be 1379 mA h g-1, 1255 mA h g-1 and 1360 mA h g-1 that decrease to 750 mA h g-1, 643 mA h g-1 and 560 mA h g-1 depending upon the chain length of grafted alkylamine on the graphene surface respectively. Electrochemical impedance spectral analysis reveals that the exchange current density of SnO2 pillared carbon based electrodes is higher, corroborating its enhanced electrochemical activity in comparison with GO based electrodes.With the objective of developing new advanced composite materials that can be used as anodes for lithium ion batteries (LIBs), herein we describe the synthesis of SnO2 pillared carbon using various alkylamine (hexylamine; dodecylamine and octadecylamine) grafted graphene oxides and butyl trichlorotin precursors followed by its calcination at 500 °C for 2 h. While the grafted alkylamine induces crystalline growth of SnO2 pillars, thermal annealing of alkylamine grafted graphene oxide results in the formation of amorphous carbon coated graphene. Field emission scanning electron microscopy (FE-SEM) results reveal the successful formation of SnO2 pillared carbon on the graphene surface. X-ray diffraction (XRD), transmission electron microscopy (TEM) and Raman spectroscopy characterization corroborates the formation of rutile SnO2 crystals on the graphene surface. A significant rise in the BET surface area is observed for SnO2 pillared carbon, when compared to pristine GO. Electrochemical characterization studies of SnO2 pillared carbon based anode materials showed an enhanced lithium storage capacity and fine cyclic performance in comparison with pristine GO. The initial specific capacities of SnO2 pillared carbon are observed to be 1379 mA h g-1, 1255 mA h g-1 and 1360 mA h g-1 that decrease to 750 mA h g-1, 643 mA h g-1 and 560 mA h g-1 depending upon the chain length of grafted alkylamine on the graphene surface respectively. Electrochemical impedance spectral analysis reveals that the exchange current density of SnO2 pillared carbon based electrodes is higher, corroborating its enhanced electrochemical activity in comparison with GO based electrodes. Electronic supplementary information (ESI) available: XPS, FE-SEM, FE-TEM, TGA FT-IR, EIS, CV of and charge discharge profiles of RGO-SnO2 composites. See DOI: 10.1039/c5nr06680h

Novel sorbent materials for environmental remediation via Pyrolysis of biomass

NASA Astrophysics Data System (ADS)

Zabaniotou, Anastasia

2013-04-01

One of the major challenges facing society at this moment is the transition from a non-sustainable, fossil resources-based economy to a sustainable bio-based economy. By producing multiple products, a biorefinery can take advantage of the differences in biomass components and intermediates and maximize the value derived from the biomass feedstock. The high-value products enhance profitability, the high-volume fuel helps meet national energy needs, and the power production reduces costs and avoids greenhouse-gas emissions From pyrolysis, besides gas and liquid products a solid product - char, is derived as well. This char contains the non converted carbon and can be used for activated carbon production and/or as additive in composite material production. Commercially available activated carbons are still considered expensive due to the use of non-renewable and relatively expensive starting material such as coal. The present study describes pyrolysis as a method to produce high added value carbon materials such as activated carbons (AC) from agricultural residues pyrolysis. Olive kernel has been investigated as the precursor of the above materials. The produced activated carbon was characterized by proximate and ultimate analyses, BET method and porosity estimation. Furthermore, its adsorption of pesticide compound in aqueous solution by was studied. Pyrolysis of olive kernel was conducted at 800 oC for 45min in a fixed reactor. For the production of the activated carbon the pyrolytic char was physically activated under steam in the presence of CO2 at 970oC for 3 h in a bench scale reactor. The active carbons obtained from both scales were characterized by N2 adsorption at 77 K, methyl-blue adsorption (MB adsorption) at room temperature and SEM analysis. Surface area and MB adsorption were found to increase with the degree of burn-off. The surface area of the activated carbons was found to increase up to 1500 m2/g at a burn-off level of 60-65wt.%, while SEM analysis showed the appearance of micropores to mesopores in the produced tire active carbons. Activated carbon prepared from olive kernel is a super active carbon and used as an adsorbent for the removal of pesticide from aqueous solutions (Bromopropylate). The higher removal achieved was 100% in 60 min. The produced activated carbon from agricultural residue was proved to be very effective for gas and water stream purification. Biomass can give a wide spectrum of fuels and materials in the integrated concept of biorefinery

Production of Prebiotic Molecule Precursors from Hypervelocity Impact Simulation Experiments on Carbonate Sediments

NASA Astrophysics Data System (ADS)

Farcy, B. J.; Grubisic, A.; Li, X.; Pinnick, V. T.; Sutton, M.; Pavlov, A.; Brinckerhoff, W. B.

2017-12-01

Organic molecules, including amino acids and other biotic precursors, have been shown to form in the cooling and expanding plasma plume generated from hypervelocity impacts through the processes of atomization, ionization, and molecular recombination of impactor and impact surface. Various sources of carbon, such as atmospheric methane and carbonaceous material from meteorites, are known to yield cyano-bearing molecules and simple amino acids from impact plasmas. However, the role of mineralogical carbon has not yet been investigated in this process. We have performed experiments using laser ablation mass spectrometry (LA-MS) to study the negative ion yield of plasma-produced prebiotic molecules. A mixture of 10% NH4Cl and 90% CaCO3 was pressed into a pellet and ablated with a 1064 nm Nd:YAG laser, and the resultant negative ions were measured by a plasma analyzer quadrupole MS. Mass spectra show characteristic peaks at m/z = 26 and m/z = 42, indicating the presence of CN- and CNO- ions. When isotopically labeled 15NH4Cl and Ca13CO3 were used in the sample ablation pellet, the purported CN- and CNO- peaks shifted according to their added isotopic mass. Indeed, comparison of resulting ion formation from momentum-based techniques, such as massive cluster secondary ion mass spectrometry, show comparable fragmentation and recombination of CN- and CNO- ions. These findings show that CN- ions, as well as CN radicals and thus HCN, can be formed during meteoritic bombardment of carbonate minerals. During the late heavy bombardment of the earth from 4.1-3.8 Ga, impact-driven chemistry could have played a dominant role in shaping the earth's early prebiotic inventory and sources of chemical energy. As carbonate sediments are common in the Archean, carbonate deposits are most likely an important contributor of carbon for this process, along with atmospheric and meteoritic carbon sources.

Multi-wall carbon nanotube@zeolite imidazolate framework composite from a nanoscale zinc oxide precursor

DOE PAGES

Yue, Yanfeng; Guo, Bingkun; Qiao, Zhenan; ...

2014-07-24

Nanocomposite of multi-walled carbon nanotube@zeolite imidazolate frameworks (MWNT@ZIF) was prepared through a nanotube-facilitated growth based on a nanosized ZnO precursor. The electrically conductive nanocomposite displays a capacity of 380 mAh/g at 0.1 °C in Li–sulfur battery, transforming electrically inactive ZIF into the active one for battery applications.

Green synthesis of boron doped graphene and its application as high performance anode material in Li ion battery

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

Sahoo, Madhumita; Sreena, K.P.; Vinayan, B.P.

2015-01-15

Graphical abstract: Boron doped graphene (B-G), synthesized by simple hydrogen induced reduction technique using boric acid as boron precursor, have more uneven surface as a result of smaller bonding distance of boron compared to carbon, showed high capacity and high rate capability compared to pristine graphene as an anode material for Li ion battery application. - Abstract: The present work demonstrates a facile route for the large-scale, catalyst free, and green synthesis approach of boron doped graphene (B-G) and its use as high performance anode material for Li ion battery (LIB) application. Boron atoms were doped into graphene framework withmore » an atomic percentage of 5.93% via hydrogen induced thermal reduction technique using graphite oxide and boric acid as precursors. Various characterization techniques were used to confirm the boron doping in graphene sheets. B-G as anode material shows a discharge capacity of 548 mAh g{sup −1} at 100 mA g{sup −1} after 30th cycles. At high current density value of 1 A g{sup −1}, B-G as anode material enhances the specific capacity by about 1.7 times compared to pristine graphene. The present study shows a simplistic way of boron doping in graphene leading to an enhanced Li ion adsorption due to the change in electronic states.« less

Enhancement of binding characteristics for production of an agglomerated product

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

Taulbee, Darrell; Hodgen, Robert

A method is provided for preparing a product from a precursor material. The method includes the steps of (a) mixing a particulate material and a binder to form a precursor material and (b) irradiating that precursor material with microwave radiation so as to activate the binder and form the product.

Technical Note: Methionine, a precursor of methane in living plants

NASA Astrophysics Data System (ADS)

Lenhart, K.; Althoff, F.; Greule, M.; Keppler, F.

2015-03-01

When terrestrial plants were identified as producers of the greenhouse gas methane, much discussion and debate ensued not only about their contribution to the global methane budget but also with regard to the validity of the observation itself. Although the phenomenon has now become more accepted for both living and dead plants, the mechanism of methane formation in living plants remains to be elucidated and its precursor compounds to be identified. We made use of stable isotope techniques to verify the in vivo formation of methane, and, in order to identify the carbon precursor, 13C positionally labeled organic compounds were employed. Here we show that the amino acid L-methionine acts as a methane precursor in living plants. Employing 13C-labeled methionine clearly identified the sulfur-bound methyl group of methionine as a carbon precursor of methane released from lavender (Lavandula angustifolia). Furthermore, when lavender plants were stressed physically, methane release rates and the stable carbon isotope values of the emitted methane greatly increased. Our results provide additional support that plants possess a mechanism for methane production and suggest that methionine might play an important role in the formation of methane in living plants, particularly under stress conditions.

Technical note: Methionine, a precursor of methane in living plants

NASA Astrophysics Data System (ADS)

Lenhart, K.; Althoff, F.; Greule, M.; Keppler, F.

2014-11-01

When terrestrial plants were identified as producers of the greenhouse gas methane, much discussion and debate ensued, not only about their contribution to the global methane budget, but also with regard to the validity of the observation itself. Although the phenomenon has now become more accepted for both living and dead plants, the mechanism of methane formation in living plants remains to be elucidated and its precursor compounds identified. We made use of stable isotope techniques to verify in vivo formation of methane and, in order to identify the carbon precursor, 13C-positionally labelled organic compounds were employed. Here we show that the amino acid L-methionine acts as a methane precursor in living plants. Employing 13C-labelled methionine clearly identified the sulphur-bound methyl group of methionine as a carbon precursor of methane released from lavender (Lavandula angustifolia). Furthermore, when lavender plants were stressed physically, methane release rates and the stable carbon isotope values of the emitted methane greatly increased. Our results provide additional support that plants possess a mechanism for methane production and suggest that methionine might play an important role in the formation of methane in living plants, particularly under stress conditions.

Ab initio molecular dynamics of atomic-scale surface reactions: insights into metal organic chemical vapor deposition of AlN on graphene.

PubMed

Sangiovanni, D G; Gueorguiev, G K; Kakanakova-Georgieva, A

2018-06-19

Metal organic chemical vapor deposition (MOCVD) of group III nitrides on graphene heterostructures offers new opportunities for the development of flexible optoelectronic devices and for the stabilization of conceptually-new two-dimensional materials. However, the MOCVD of group III nitrides is regulated by an intricate interplay of gas-phase and surface reactions that are beyond the resolution of experimental techniques. We use density-functional ab initio molecular dynamics (AIMD) with van der Waals corrections to identify atomistic pathways and associated electronic mechanisms driving precursor/surface reactions during metal organic vapor phase epitaxy at elevated temperatures of aluminum nitride on graphene, considered here as model case study. The results presented provide plausible interpretations of atomistic and electronic processes responsible for delivery of Al, C adatoms, and C-Al, CHx, AlNH2 admolecules on pristine graphene via precursor/surface reactions. In addition, the simulations reveal C adatom permeation across defect-free graphene, as well as exchange of C monomers with graphene carbon atoms, for which we obtain rates of ∼0.3 THz at typical experimental temperatures (1500 K), and extract activation energies Eexca = 0.28 ± 0.13 eV and attempt frequencies Aexc = 2.1 (×1.7±1) THz via Arrhenius linear regression. The results demonstrate that AIMD simulations enable understanding complex precursor/surface reaction mechanisms, and thus propose AIMD to become an indispensable routine prediction-tool toward more effective exploitation of chemical precursors and better control of MOCVD processes during synthesis of functional materials.

Carbonization-dependent nitrogen-doped hollow porous carbon nanospheres synthesis and electrochemical study for supercapacitors

NASA Astrophysics Data System (ADS)

Zhou, Lingyun; Xie, Guohong; Chen, Xiling

2018-05-01

In this paper, a nitrogen-doped hollow microporous carbon nanospheres was synthesized via the combination of hyper-crosslinking mediated self-assembly and further pyrolysis using polylactide-b-polystyrene (PLA-b-PS) copolymers and aniline monomers as precursor. The pore structure and the correlative electrochemical performance of nitrogen-doped hollow microporous carbon nanospheres were affected by the molar mass ratio of aniline and PS in block copolymers and the carbonization conditions. The electrochemical measurements results showed that the obtained PLA150-PS250-N4-900-10H sample with nitrogen content of 3.57% and the BET surface area of 945 m2 g-1 displays the best capacitance performance. At a current density of 1.0 Ag-1, the resultant specific capacitance is 250 Fg-1. In addition, it also exhibits high capacitance retention of 98% after charging-discharging 1500 times at 25 Ag-1. The results demonstrate the nitrogen-doped hollow microporous carbon nanospheres can be used as promising supercapacitor electrode materials for high performance energy storage devices.

Gas-solid carbonation as a possible source of carbonates in cold planetary environments

NASA Astrophysics Data System (ADS)

Garenne, A.; Montes-Hernandez, G.; Beck, P.; Schmitt, B.; Brissaud, O.; Pommerol, A.

2013-02-01

Carbonates are abundant sedimentary minerals at the surface and sub-surface of the Earth and they have been proposed as tracers of liquid water in extraterrestrial environments. Their formation mechanism is since generally associated with aqueous alteration processes. Recently, carbonate minerals have been discovered on Mars' surface by different orbitals or rover missions. In particular, the phoenix mission has measured from 1% to 5% of calcium carbonate (calcite type) within the soil (Smith et al., 2009). These occurrences have been reported in area where the relative humidity is significantly high (Boynton et al., 2009). The small concentration of carbonates suggests an alternative process on mineral grain surfaces (as suggested by Shaheen et al., 2010) than carbonation in aqueous conditions. Such an observation could rather point toward a possible formation mechanism by dust-gas reaction under current Martian conditions. To understand the mechanism of carbonate formation under conditions relevant to current Martian atmosphere and surface, we designed an experimental setup consisting of an infrared microscope coupled to a cryogenic reaction cell (IR-CryoCell setup). Three different mineral precursors of carbonates (Ca and Mg hydroxides, and a hydrated Ca silicate formed from Ca2SiO4), low temperature (from -10 to +30 °C), and reduced CO2 pressure (from 100 to 2000 mbar) were utilized to investigate the mechanism of gas-solid carbonation at mineral surfaces. These mineral materials are crucial precursors to form Ca and Mg carbonates in humid environments (0%

Facile synthesis of thermal- and photostable titania with paramagnetic oxygen vacancies for visible-light photocatalysis.

PubMed

Zou, Xiaoxin; Liu, Jikai; Su, Juan; Zuo, Fan; Chen, Jiesheng; Feng, Pingyun

2013-02-18

A novel dopant-free TiO(2) photocatalyst (V(o)(.)-TiO(2)), which is self-modified by a large number of paramagnetic (single-electron-trapped) oxygen vacancies, was prepared by calcining a mixture of a porous amorphous TiO(2) precursor, imidazole, and hydrochloric acid at elevated temperature (450 °C) in air. Control experiments demonstrate that the porous TiO(2) precursor, imidazole, and hydrochloric acid are all necessary for the formation of V(o)(.)-TiO(2). Although the synthesis of V(o)(.)-TiO(2) originates from such a multicomponent system, this synthetic approach is facile, controllable, and reproducible. X-ray diffraction, XPS, and EPR spectroscopy reveal that the V(o)(.)-TiO(2) material with a high crystallinity embodies a mass of paramagnetic oxygen vacancies, and is free of other dopant species such as nitrogen and carbon. UV/Vis diffuse-reflectance spectroscopy and photoelectrochemical measurement demonstrate that V(o)(.)-TiO(2) is a stable visible-light-responsive material with photogenerated charge separation efficiency higher than N-TiO(2) and P25 under visible-light irradiation. The V(o)(.)-TiO(2) material exhibits not only satisfactory thermal- and photostability, but also superior photocatalytic activity for H(2) evolution (115 μmol h(-1) g(-1)) from water with methanol as sacrificial reagent under visible light (λ>400 nm) irradiation. Furthermore, the effects of reaction temperature, ratio of starting materials (imidazole:TiO(2) precursor) and calcination time on the photocatalytic activity and the microstructure of V(o)(.)-TiO(2) were elucidated. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Harmful impact on presynaptic glutamate and GABA transport by carbon dots synthesized from sulfur-containing carbohydrate precursor.

PubMed

Borisova, Tatiana; Dekaliuk, Mariia; Pozdnyakova, Natalia; Pastukhov, Artem; Dudarenko, Marina; Borysov, Arsenii; Vari, Sandor G; Demchenko, Alexander P

2017-07-01

Carbon nanoparticles that may be potent air pollutants with adverse effects on human health often contain heteroatoms including sulfur. In order to study in detail their effects on different physiological and biochemical processes, artificially produced carbon dots (CDs) with well-controlled composition that allows fluorescence detection may be of great use. Having been prepared from different types of organic precursors, CDs expose different atoms at their surface suggesting a broad variation of functional groups. Recently, we demonstrated neurotoxic properties of CDs synthesized from the amino acid β-alanine, and it is of importance to analyze whether CDs obtained from different precursors and particularly those exposing sulfur atoms induce similar neurotoxic effects. This study focused on synthesis of CDs from the sulfur-containing precursor thiourea-CDs (TU-CDs) with a size less than 10 nm, their characterization, and neuroactivity assessment. Neuroactive properties of TU-CDs were analyzed based on their effects on the key characteristics of glutamatergic and γ-aminobutyric acid (GABA) neurotransmission in isolated rat brain nerve terminals. It was observed that TU-CDs (0.5-1.0 mg/ml) attenuated the initial velocity of Na + -dependent transporter-mediated uptake and accumulation of L-[ 14 C]glutamate and [ 3 H]GABA by nerve terminals in a dose-dependent manner and increased the ambient level of the neurotransmitters. Starting from the concentration of 0.2 mg/ml, TU-CDs evoked a gradual dose-dependent depolarization of the plasma membrane of nerve terminals measured with the cationic potentiometric dye rhodamine 6G. Within the concentration range of 0.1-0.5 mg/ml, TU-CDs caused an "unphysiological" step-like increase in fluorescence intensity of the рН-sensitive fluorescent dye acridine orange accumulated by synaptic vesicles. Therefore, despite different surface properties and fluorescent features of CDs prepared from different starting materials (thiourea and β-alanine), their principal neurotoxic effects are analogous but displayed at a different level of efficiency. Sulfur-containing TU-CDs exhibit lower effects (by ~30%) on glutamate and GABA transport in the nerve terminals in comparison with sulfur-free β-alanine CDs. Our results suggest considering that an uncontrolled presence of carbon-containing particulate matter in the human environment may pose a toxicity risk for the central nervous system.

ZnO@C (core@shell) microspheres derived from spent coffee grounds as applicable non-precious electrode material for DMFCs.

PubMed

Ghouri, Zafar Khan; Al-Meer, Saeed; Barakat, Nasser A M; Kim, Hak Yong

2017-05-11

Although numerous reports have introduced non precious electrocatalysts for methanol oxidation, most of those studies did not consider the corresponding high onset potential which restricts utilization in real fuel cells. In this study, an -90 mV [vs. Ag/AgCl] onset potential non-precious electrocatalyst is introduced as an applicable anode material for the direct methanol fuel cells. Moreover, the proposed material was prepared from a cheap and abundantly existing resource; the spent coffee grounds. Typically, the spent coffee grounds were facilely converted to core@shell (ZnO@C) microspheres through a two-step approach, involving chemical activation and a subsequent calcination at temperature of 700 °C. Activation of the carbon derived from the spent coffee grounds was performed with ZnCl 2 which acts as pore-forming agent as well as a precursor for the ZnO. The structure and morphology were characterized by (XRD), (SEM), and (TEM) analyses while the electrochemical characterizations was evaluated by cyclic voltammetry (CV) technique. Besides the comparatively very low onset potential, the introduced microspheres exhibited relatively high current density; 17 mA/cm 2 . Overall, based on the advantages of the green source of carbon and the good electrocatalytic activity, the spent coffee grounds-derived carbon can be considered a promise anode material for the DMFCs.

Tailoring the properties of a zero-valent iron-based composite by mechanochemistry for nitrophenols degradation in wastewaters.

PubMed

Cagnetta, Giovanni; Huang, Jun; Lomovskiy, Igor O; Yu, Gang

2017-11-01

Zero-valent iron (ZVI) is a valuable material for environmental remediation, because of its safeness, large availability, and inexpensiveness. Moreover, its reactivity can be improved by addition of (nano-) particles of other elements such as noble metals. However, common preparation methods for this kind of iron-based composites involve wet precipitation of noble metal salt precursors, so they are often expensive and not green. Mechanochemical procedures can provide a solvent-free alternative, even at a large scale. The present study demonstrates that it is possible to tailor functional properties of ZVI-based materials, utilizing high-energy ball milling. All main preparation parameters are investigated and discussed. Specifically, a copper-carbon-iron ternary composite was prepared for fast degradation of 4-nitrophenol (utilized as model pollutant) to 4-aminophenol and other phenolic compounds. Copper and carbon are purposely chosen to insert specific properties to the composite: Copper acts as efficient nano-cathode that enhances electron transfer from iron to 4-nitrophenol, while carbon protects the iron surface from fast oxidation in open air. In this way, the reactive material can rapidly reduce high concentration of nitrophenols in water, it does not require acid washing to be activated, and can be stored in open air for one week without any significant activity loss.

Fabrication of 3D lawn-shaped N-doped porous carbon matrix/polyaniline nanocomposite as the electrode material for supercapacitors

NASA Astrophysics Data System (ADS)

Zhang, Xiuling; Ma, Li; Gan, Mengyu; Fu, Gang; Jin, Meng; Lei, Yao; Yang, Peishu; Yan, Maofa

2017-02-01

A facile approach to acquire electrode materials with prominent electrochemical property is pivotal to the progress of supercapacitors. 3D nitrogen-doped porous carbon matrix (PCM), with high specific surface area (SSA) up to 2720 m2 g-1, was obtained from the carbonization and activation of the nitrogen-enriched composite precursor (graphene/polyaniline). Then 3D lawn-shaped PCM/PANI composite was obtained by the simple in-situ polymerization. The morphology and structure of these resulting composites were characterized by combining SEM and TEM measurements, Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD) spectroscopy analyses and Raman spectroscope. The element content of all samples was evaluated using CHN analysis. The results of electrochemical testing indicated that the PCM/PANI composite displays a higher capacitance value of 527 F g-1 at 1 A g-1 compared to 338 F g-1 for pure PANI, and exhibits appreciable rate capability with a retention of 76% at 20 A g-1 as well as fine long-term cycling performance (with 88% retention of specific capacitance after 1000 cycles at 10 A g-1). Simultaneously, the excellent capacitance performance coupled with the facile synthesis of PCM/PANI indicates it is a promising electrode material for supercapacitors.

Controlled preparation of carbon nanotube-iron oxide nanoparticle hybrid materials by a modified wet impregnation method

NASA Astrophysics Data System (ADS)

Tsoufis, Τheodoros; Douvalis, Alexios P.; Lekka, Christina E.; Trikalitis, Pantelis N.; Bakas, Thomas; Gournis, Dimitrios

2013-09-01

We report a novel, simple, versatile, and reproducible approach for the in situ synthesis of iron oxide nanoparticles (NP) on the surface of carbon nanotubes (CNT). Chemically functionalized single- or multi-wall CNT were used as nanotemplates for the synthesis of a range of very small (<10 nm) ferrimagnetic and/or anti-ferromagnetic iron oxide NP on their surface. For the synthesis of the hybrid materials, we employed for the first time a modified wet impregnation method involving the adsorption of ferric cations (as nanoparticle's precursor) on the functionalized nanotube surface and the subsequent interaction with acetic acid vapors followed by calcination at 400 °C under different atmospheres (air, argon, and oxygen). X-ray diffraction, transmission electron microscopy, Mössbauer spectroscopy, and magnetization measurements were used to study in-detail the morphology, size, and type of crystalline phases in the resulting hybrid materials. In addition, Raman measurements were used to monitor possible structural changes of the nanotubes during the synthetic approach. The experimental results were further supported by density functional theory calculations. These calculations were also used to disclose, how the type of the carbon nanotube template affects the nature and the size of the resulting NP in the final hybrids.

The Ca-looping process for CO2 capture and energy storage: role of nanoparticle technology

NASA Astrophysics Data System (ADS)

Valverde, Jose Manuel

2018-02-01

The calcium looping (CaL) process, based on the cyclic carbonation/calcination of CaO, has come into scene in the last years with a high potential to be used in large-scale technologies aimed at mitigating global warming. In the CaL process for CO2 capture, the CO2-loaded flue gas is used to fluidize a bed of CaO particles at temperatures around 650 °C. The carbonated particles are then circulated into a calciner reactor wherein the CaO solids are regenerated at temperatures near 950 °C under high CO2 concentration. Calcination at such harsh conditions causes a marked sintering and loss of reactivity of the regenerated CaO. This main drawback could be however compensated from the very low cost of natural CaO precursors such as limestone or dolomite. Another emerging application of the CaL process is thermochemical energy storage (TCES) in concentrated solar power (CSP) plants. Importantly, carbonation/calcination conditions to maximize the global CaL-CSP plant efficiency could differ radically from those used for CO2 capture. Thus, carbonation could be carried out at high temperatures under high CO2 partial pressure for maximum efficiency, whereas the solids could be calcined at relatively low temperatures in the absence of CO2 to promote calcination. Our work highlights the critical role of carbonation/calcination conditions on the performance of CaO derived from natural precursors. While conditions in the CaL process for CO2 capture lead to a severe CaO deactivation with the number of cycles, the same material may exhibit a high and stable conversion at optimum CaL-CSP conditions. Moreover, the type of CaL conditions influences critically the reaction kinetics, which plays a main role on the optimization of relevant operation parameters such as the residence time in the reactors. This paper is devoted to a brief review on the latest research activity in our group concerning these issues as well as the possible role of nanoparticle technology to enhance the activity of Ca-based materials at CaL conditions for CO2 capture and energy storage.

Nanocomposites with embedded structures for lithium-ion batteries

NASA Astrophysics Data System (ADS)

Yang, Zichao

Lithium-ion batteries (LIBs) have been widely employed in portable electronics and are rapidly expanding into emerging markets such as hybrid and electric vehicles and potentially electric grid storage. These new opportunities create new challenges for LIBs and further improvement of specific energy, cycling performance and rate capability are required. A major strategy in performance enhancement for the electrode materials involves the creation of carbon composites to provide mechanical buffering of active material and to improve electrical conductivity. In the current work, a platform is developed for creating functional hybrid materials by copolymerization of organic molecules and inorganic compounds followed by thermal pyrolysis, and the approach yields nanostructured composites in which nanoparticles are uniformly embedded in a porous, partially graphitic carbon matrix. Depending upon the chemistry of the starting materials, nanocomposites with embedded structures created using the approach are attractive as anode or cathode materials for next-generation rechargeable lithium battery systems. The platform is very versatile and through ex situ conversion or utilization of multiple precursors, can be applied to various classes of materials including metal oxides (single or mixed), metals, metal sulfides, alloys, metalloids, phosphates, etc. The approach also lends itself to the development of scalable processes for production of nanostructured battery materials. Mechanistic analysis was performed and reveals that the performance enhancement of the embedded nanocomposite configuration is mainly brought about by the mechanical buffering effect offered by the carbon matrix. The active material loading was shown to be an important factor in the design of the composites as electrode materials. In addition to the polymerization-based approach, other in situ methods such as one based on spray pyrolysis are also explored and demonstrate the versatility of the in situ synthesis concept.

Physical Properties of 3D Interconnected Graphite Networks - Aerographite

DTIC Science & Technology

2015-10-30

Figure 1.2: Influence of toluene injection rate per time on Aerographite density...................... 6 Figure 1.3: Influence of toluene injection ...densities ........................... 20 Figure 3.15: Capacitance as a function of carbon precursor injection rate .............................. 20...At a constant temperature profile of 200° C in the injection zone and 760° C in main zone, a carbon precursor (toluene) is injected with a